#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/91/7009168.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_7009168
loop_
_publ_author_name
'Deacon, Glen B.'
'Delbridge, Ewan E.'
'Forsyth, Craig M.'
'Skelton, Brian W.'
'White, Allan H.'
_publ_section_title
;
 Novel pyrazolate coordination modes and unusual
 Tl  · · ·  Tl
 or Tl-π-(phenyl) interactions in the crystal structures of
 [{Tl3(Ph2pz)3}n], [{Tl4(Ph2pz)4}n], [{Tl4(Ph2pz)3(OH)}2] and
 [{Tl4(MePhpz)3(OH)}n] (Ph2pz = 3,5-diphenylpyrazolate;
 MePhpz = 3-methyl-5-phenylpyrazolate)
;
_journal_issue                   5
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              745
_journal_paper_doi               10.1039/a909048g
_journal_year                    2000
_chemical_formula_sum            'C92 H72 Cl4 N12 O2 Tl8'
_chemical_formula_weight         3154.55
_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'
_cell_angle_alpha                90.00000
_cell_angle_beta                 92.160(3)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            2
_cell_length_a                   13.851(2)
_cell_length_b                   21.533(4)
_cell_length_c                   14.721(3)
_cell_measurement_reflns_used    5806
_cell_measurement_temperature    153
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     4387.5(14)
_computing_cell_refinement       'Siemens SAINT (Siemens, 1995)'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        'xtal ADDREF SORTRF'
_computing_molecular_graphics    xtal
_computing_publication_material  'xtal BONDLA CIFIO'
_computing_structure_refinement  'xtal CRYLSQ'
_computing_structure_solution    xtal
_diffrn_ambient_temperature      153
_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer
;
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_detector       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .082
_diffrn_reflns_av_sigmaI/netI    .1
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            50455
_diffrn_reflns_theta_max         29.23
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    14.811
_exptl_absorpt_correction_T_max  .432
_exptl_absorpt_correction_T_min  .096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.388
_exptl_crystal_description       prism
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .39
_exptl_crystal_size_min          .22
_refine_diff_density_max         2.533
_refine_diff_density_min         -1.714
_refine_ls_abs_structure_details none
_refine_ls_extinction_coef       1768(109)
_refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970'
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_all   .95
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           atomblock
_refine_ls_number_constraints    0
_refine_ls_number_parameters     534
_refine_ls_number_reflns         7654
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .066
_refine_ls_R_factor_gt           .038
_refine_ls_shift/su_max          .049
_refine_ls_shift/su_mean         .004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .047
_refine_ls_wR_factor_ref         .042
_reflns_d_resolution_high        .728
_reflns_d_resolution_low         13.803
_reflns_Friedel_coverage         0
_reflns_limit_h_max              18
_reflns_limit_h_min              0
_reflns_limit_k_max              29
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              -20
_reflns_number_gt                7654
_reflns_number_total             11124
_reflns_threshold_expression     'F    > 4.00 sig(F   )'
_cod_data_source_file            a909048g.txt
_cod_data_source_block           gbdtll
_cod_original_sg_symbol_Hall     -p_2ybc
_cod_original_sg_symbol_H-M      P_1_21/c_1
_cod_database_code               7009168
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
-x,1/2+y,1/2-z
-x,-y,-z
+x,1/2-y,1/2+z
loop_
_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_calc_attached_atom
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tl1 .55529(2) .040031(16) .59284(2) .02243(17) Uani ? ? 1.00000 ? ?
Tl2 .40878(2) -.024038(15) .80914(2) .02182(17) Uani ? ? 1.00000 ? ?
Tl3 .38131(2) .171195(15) .73201(2) .02192(17) Uani ? ? 1.00000 ? ?
Tl4 .25246(3) .050784(17) .56326(3) .0289(2) Uani ? ? 1.00000 ? ?
O0 .4068(4) .0995(3) .6028(4) .023(3) Uani ? ? 1.00000 ? ?
N11 .5716(5) .0664(3) .7660(4) .018(3) Uani ? ? 1.00000 ? ?
N12 .4949(5) .0904(3) .8131(4) .023(4) Uani ? ? 1.00000 ? ?
C13 .5249(6) .0956(4) .9020(5) .021(4) Uani ? ? 1.00000 ? ?
C131 .4596(6) .1191(4) .9699(5) .018(4) Uani ? ? 1.00000 ? ?
C132 .3596(6) .1150(4) .9599(6) .022(4) Uani ? ? 1.00000 ? ?
C133 .3012(6) .1376(4) 1.0266(6) .025(5) Uani ? ? 1.00000 ? ?
C134 .3402(6) .1644(4) 1.1038(6) .026(5) Uani ? ? 1.00000 ? ?
C135 .4389(7) .1698(4) 1.1159(6) .030(5) Uani ? ? 1.00000 ? ?
C136 .4980(6) .1482(4) 1.0491(6) .024(5) Uani ? ? 1.00000 ? ?
C14 .6192(6) .0735(4) .9132(6) .023(4) Uani ? ? 1.00000 ? ?
C15 .6448(6) .0561(4) .8248(5) .018(4) Uani ? ? 1.00000 ? ?
C151 .7383(6) .0312(4) .7968(6) .020(4) Uani ? ? 1.00000 ? ?
C152 .7887(6) -.0112(4) .8524(6) .024(5) Uani ? ? 1.00000 ? ?
C153 .8794(7) -.0341(4) .8297(6) .029(5) Uani ? ? 1.00000 ? ?
C154 .9193(6) -.0150(4) .7515(6) .029(5) Uani ? ? 1.00000 ? ?
C155 .8707(7) .0280(4) .6946(6) .031(5) Uani ? ? 1.00000 ? ?
C156 .7808(6) .0506(4) .7183(6) .025(5) Uani ? ? 1.00000 ? ?
N21 .4227(5) -.0616(3) .6335(5) .024(4) Uani ? ? 1.00000 ? ?
N22 .3259(5) -.0552(3) .6125(5) .022(4) Uani ? ? 1.00000 ? ?
C23 .2938(6) -.1085(4) .5745(5) .018(4) Uani ? ? 1.00000 ? ?
C231 .1916(6) -.1170(4) .5425(5) .021(4) Uani ? ? 1.00000 ? ?
C232 .1165(7) -.0828(4) .5792(6) .027(5) Uani ? ? 1.00000 ? ?
C233 .0227(6) -.0897(5) .5456(6) .032(5) Uani ? ? 1.00000 ? ?
C234 .0007(7) -.1324(5) .4785(7) .036(6) Uani ? ? 1.00000 ? ?
C235 .0727(6) -.1677(4) .4426(7) .031(5) Uani ? ? 1.00000 ? ?
C236 .1678(6) -.1600(4) .4744(6) .026(5) Uani ? ? 1.00000 ? ?
C24 .3700(6) -.1512(4) .5695(5) .022(4) Uani ? ? 1.00000 ? ?
C25 .4503(6) -.1197(4) .6076(5) .022(4) Uani ? ? 1.00000 ? ?
C251 .5496(6) -.1402(4) .6163(5) .020(4) Uani ? ? 1.00000 ? ?
C252 .6209(7) -.1076(4) .6681(5) .024(4) Uani ? ? 1.00000 ? ?
C253 .7170(6) -.1241(4) .6705(6) .025(5) Uani ? ? 1.00000 ? ?
C254 .7444(7) -.1756(5) .6244(7) .035(5) Uani ? ? 1.00000 ? ?
C255 .6763(7) -.2117(4) .5773(6) .032(5) Uani ? ? 1.00000 ? ?
C256 .5793(7) -.1932(4) .5722(6) .027(5) Uani ? ? 1.00000 ? ?
N31 .2309(5) .0965(3) .7470(5) .024(4) Uani ? ? 1.00000 ? ?
N32 .2451(5) .0358(3) .7744(5) .021(4) Uani ? ? 1.00000 ? ?
C33 .1713(6) .0209(3) .8280(5) .017(4) Uani ? ? 1.00000 ? ?
C331 .1649(6) -.0421(4) .8696(5) .019(4) Uani ? ? 1.00000 ? ?
C332 .2012(6) -.0947(4) .8279(6) .025(5) Uani ? ? 1.00000 ? ?
C333 .1979(7) -.1527(4) .8688(6) .030(5) Uani ? ? 1.00000 ? ?
C334 .1603(7) -.1572(4) .9535(7) .037(6) Uani ? ? 1.00000 ? ?
C335 .1217(7) -.1062(4) .9943(6) .032(5) Uani ? ? 1.00000 ? ?
C336 .1232(6) -.0494(4) .9542(6) .022(4) Uani ? ? 1.00000 ? ?
C34 .1112(6) .0718(4) .8378(6) .023(4) Uani ? ? 1.00000 ? ?
C35 .1500(6) .1180(4) .7857(5) .019(4) Uani ? ? 1.00000 ? ?
C351 .1128(6) .1812(4) .7678(7) .027(5) Uani ? ? 1.00000 ? ?
C352 .1363(6) .2151(4) .6904(7) .030(5) Uani ? ? 1.00000 ? ?
C353 .0976(6) .2743(4) .6748(8) .040(6) Uani ? ? 1.00000 ? ?
C354 .0331(7) .2990(4) .7333(9) .050(7) Uani ? ? 1.00000 ? ?
C355 .0073(7) .2664(4) .8090(8) .043(6) Uani ? ? 1.00000 ? ?
C356 .0482(6) .2081(4) .8264(7) .033(5) Uani ? ? 1.00000 ? ?
Cl1 .62130(17) .20834(12) .66119(16) .0368(13) Uani ? ? 1.00000 ? ?
Cl2 .7716(2) .21813(15) .8044(2) .0572(18) Uani ? ? 1.00000 ? ?
C0 .6478(7) .2166(5) .7796(6) .036(6) Uani ? ? 1.00000 ? ?
H0 .41315 .11560 .55065 .02800 Uiso ? ? 1.00000 ? ?
H132 .33075 .09678 .90521 .03000 Uiso ? ? 1.00000 ? ?
H133 .23156 .13410 1.01934 .03300 Uiso ? ? 1.00000 ? ?
H134 .29843 .17928 1.14941 .03400 Uiso ? ? 1.00000 ? ?
H135 .46570 .18864 1.17030 .03700 Uiso ? ? 1.00000 ? ?
H136 .56742 .15258 1.05713 .03100 Uiso ? ? 1.00000 ? ?
H14 .65734 .07012 .96909 .02700 Uiso ? ? 1.00000 ? ?
H152 .76002 -.02474 .90743 .03000 Uiso ? ? 1.00000 ? ?
H153 .91377 -.06287 .86947 .03600 Uiso ? ? 1.00000 ? ?
H154 .98085 -.03079 .73576 .03700 Uiso ? ? 1.00000 ? ?
H155 .89946 .04132 .63943 .03900 Uiso ? ? 1.00000 ? ?
H156 .74780 .08053 .67954 .03200 Uiso ? ? 1.00000 ? ?
H232 .13062 -.05398 .62787 .03500 Uiso ? ? 1.00000 ? ?
H233 -.02766 -.06447 .56997 .03800 Uiso ? ? 1.00000 ? ?
H234 -.06598 -.13842 .45705 .04600 Uiso ? ? 1.00000 ? ?
H235 .05850 -.19785 .39498 .03800 Uiso ? ? 1.00000 ? ?
H236 .21814 -.18470 .44897 .03200 Uiso ? ? 1.00000 ? ?
H24 .36816 -.19288 .54539 .02700 Uiso ? ? 1.00000 ? ?
H252 .60102 -.07246 .70295 .03000 Uiso ? ? 1.00000 ? ?
H253 .76406 -.09939 .70482 .03100 Uiso ? ? 1.00000 ? ?
H254 .81254 -.18614 .62376 .04500 Uiso ? ? 1.00000 ? ?
H255 .69518 -.25019 .54861 .04200 Uiso ? ? 1.00000 ? ?
H256 .53221 -.21754 .53739 .03300 Uiso ? ? 1.00000 ? ?
H332 .22956 -.09066 .76913 .03100 Uiso ? ? 1.00000 ? ?
H333 .22112 -.18860 .83781 .03700 Uiso ? ? 1.00000 ? ?
H334 .16245 -.19695 .98509 .04600 Uiso ? ? 1.00000 ? ?
H335 .09311 -.11053 1.05335 .04100 Uiso ? ? 1.00000 ? ?
H336 .09654 -.01365 .98403 .02800 Uiso ? ? 1.00000 ? ?
H34 .05461 .07434 .87371 .02800 Uiso ? ? 1.00000 ? ?
H352 .17941 .19757 .64783 .03800 Uiso ? ? 1.00000 ? ?
H353 .11614 .29748 .62156 .05100 Uiso ? ? 1.00000 ? ?
H354 .00637 .33933 .72260 .06200 Uiso ? ? 1.00000 ? ?
H355 -.03887 .28339 .84994 .05500 Uiso ? ? 1.00000 ? ?
H356 .03269 .18606 .88114 .04200 Uiso ? ? 1.00000 ? ?
H0a .61931 .18261 .81144 .04500 Uiso ? ? 1.00000 ? ?
H0b .61900 .25428 .80068 .04500 Uiso ? ? 1.00000 ? ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C ? 0 184 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1'
N ? 0 24 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1'
O ? 0 4 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1'
H ? 0 144 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1'
Tl ? 0 16 -3.556 9.659 'Int Tables Vol IV Tables 2.2B and 2.3.1'
Cl ? 0 8 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1'
loop_
_diffrn_attenuator_code
_diffrn_attenuator_scale
? ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
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_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Tl2 Tl1 O0 . . . 71.58(13) ?
Tl2 Tl1 N11 . . . 48.66(14) ?
Tl2 Tl1 N21 . . . 41.81(14) ?
Tl2 Tl1 Tl1 . . '3 656' 103.003(17) ?
Tl2 Tl1 Tl4 . . '3 656' 129.172(14) ?
O0 Tl1 N11 . . . 82.44(19) ?
O0 Tl1 N21 . . . 81.0(2) ?
O0 Tl1 Tl1 . . '3 656' 87.75(13) ?
O0 Tl1 Tl4 . . '3 656' 149.05(12) ?
N11 Tl1 N21 . . . 89.7(2) ?
N11 Tl1 Tl1 . . '3 656' 151.66(14) ?
N11 Tl1 Tl4 . . '3 656' 128.27(14) ?
N21 Tl1 Tl1 . . '3 656' 62.44(14) ?
N21 Tl1 Tl4 . . '3 656' 100.63(14) ?
Tl1 Tl1 Tl4 '3 656' . '3 656' 66.638(14) ?
Tl1 Tl2 N11 . . . 39.81(12) ?
Tl1 Tl2 N12 . . . 58.87(14) ?
Tl1 Tl2 N21 . . . 45.91(15) ?
Tl1 Tl2 N32 . . . 97.61(15) ?
N11 Tl2 N12 . . . 26.9(2) ?
N11 Tl2 N21 . . . 85.0(2) ?
N11 Tl2 N32 . . . 106.4(2) ?
N12 Tl2 N21 . . . 103.9(2) ?
N12 Tl2 N32 . . . 86.3(2) ?
N21 Tl2 N32 . . . 93.0(2) ?
Tl4 Tl3 O0 . . . 35.74(13) ?
Tl4 Tl3 N12 . . . 95.73(15) ?
Tl4 Tl3 N31 . . . 47.04(15) ?
O0 Tl3 N12 . . . 80.5(2) ?
O0 Tl3 N31 . . . 79.7(2) ?
N12 Tl3 N31 . . . 91.1(2) ?
Tl3 Tl4 O0 . . . 36.65(13) ?
Tl3 Tl4 N22 . . . 103.76(15) ?
Tl3 Tl4 N31 . . . 41.85(14) ?
Tl3 Tl4 Tl1 . . '3 656' 112.209(15) ?
O0 Tl4 N22 . . . 88.9(2) ?
O0 Tl4 N31 . . . 75.58(19) ?
O0 Tl4 Tl1 . . '3 656' 75.83(13) ?
N22 Tl4 N31 . . . 95.2(2) ?
N22 Tl4 Tl1 . . '3 656' 58.53(15) ?
N31 Tl4 Tl1 . . '3 656' 141.18(14) ?
Tl1 O0 Tl3 . . . 121.2(2) ?
Tl1 O0 Tl4 . . . 119.8(2) ?
Tl1 O0 H0 . . . 92.5(4) ?
Tl3 O0 Tl4 . . . 107.6(2) ?
Tl3 O0 H0 . . . 117.4(5) ?
Tl4 O0 H0 . . . 94.6(4) ?
Tl1 N11 Tl2 . . . 91.52(19) ?
Tl1 N11 N12 . . . 121.9(4) ?
Tl1 N11 C15 . . . 129.4(5) ?
Tl2 N11 N12 . . . 63.3(4) ?
Tl2 N11 C15 . . . 108.0(5) ?
N12 N11 C15 . . . 108.5(6) ?
Tl2 N12 Tl3 . . . 109.7(2) ?
Tl2 N12 N11 . . . 89.8(4) ?
Tl2 N12 C13 . . . 102.2(5) ?
Tl3 N12 N11 . . . 118.6(5) ?
Tl3 N12 C13 . . . 122.8(5) ?
N11 N12 C13 . . . 107.4(6) ?
N12 C13 C131 . . . 120.7(7) ?
N12 C13 C14 . . . 109.7(7) ?
C131 C13 C14 . . . 129.6(7) ?
C13 C131 C132 . . . 123.0(7) ?
C13 C131 C136 . . . 119.6(7) ?
C132 C131 C136 . . . 117.4(7) ?
C131 C132 C133 . . . 120.6(8) ?
C131 C132 H132 . . . 119.5(8) ?
C133 C132 H132 . . . 119.9(8) ?
C132 C133 C134 . . . 121.0(8) ?
C132 C133 H133 . . . 120.0(8) ?
C134 C133 H133 . . . 119.0(9) ?
C133 C134 C135 . . . 120.2(8) ?
C133 C134 H134 . . . 119.6(9) ?
C135 C134 H134 . . . 120.2(8) ?
C134 C135 C136 . . . 119.4(8) ?
C134 C135 H135 . . . 119.7(9) ?
C136 C135 H135 . . . 120.9(9) ?
C131 C136 C135 . . . 121.5(8) ?
C131 C136 H136 . . . 119.1(8) ?
C135 C136 H136 . . . 119.4(8) ?
C13 C14 C15 . . . 104.3(7) ?
C13 C14 H14 . . . 127.5(8) ?
C15 C14 H14 . . . 128.2(8) ?
N11 C15 C14 . . . 110.1(7) ?
N11 C15 C151 . . . 122.5(7) ?
C14 C15 C151 . . . 127.4(7) ?
C15 C151 C152 . . . 119.9(7) ?
C15 C151 C156 . . . 122.0(7) ?
C152 C151 C156 . . . 118.0(8) ?
C151 C152 C153 . . . 121.5(8) ?
C151 C152 H152 . . . 118.7(8) ?
C153 C152 H152 . . . 119.8(8) ?
C152 C153 C154 . . . 119.5(8) ?
C152 C153 H153 . . . 120.5(9) ?
C154 C153 H153 . . . 120.0(9) ?
C153 C154 C155 . . . 120.2(8) ?
C153 C154 H154 . . . 119.6(9) ?
C155 C154 H154 . . . 120.2(9) ?
C154 C155 C156 . . . 119.6(8) ?
C154 C155 H155 . . . 119.7(9) ?
C156 C155 H155 . . . 120.7(9) ?
C151 C156 C155 . . . 121.2(8) ?
C151 C156 H156 . . . 119.3(8) ?
C155 C156 H156 . . . 119.5(9) ?
Tl1 N21 Tl2 . . . 92.3(2) ?
Tl1 N21 N22 . . . 119.6(5) ?
Tl1 N21 C25 . . . 116.2(5) ?
Tl2 N21 N22 . . . 94.6(4) ?
Tl2 N21 C25 . . . 124.6(5) ?
N22 N21 C25 . . . 108.0(7) ?
Tl4 N22 N21 . . . 121.4(5) ?
Tl4 N22 C23 . . . 121.0(5) ?
N21 N22 C23 . . . 108.3(6) ?
N22 C23 C231 . . . 122.2(7) ?
N22 C23 C24 . . . 110.0(7) ?
C231 C23 C24 . . . 127.7(7) ?
C23 C231 C232 . . . 121.7(7) ?
C23 C231 C236 . . . 120.5(7) ?
C232 C231 C236 . . . 117.9(8) ?
C231 C232 C233 . . . 120.5(8) ?
C231 C232 H232 . . . 119.6(8) ?
C233 C232 H232 . . . 119.9(9) ?
C232 C233 C234 . . . 120.6(9) ?
C232 C233 H233 . . . 119.4(9) ?
C234 C233 H233 . . . 120.0(9) ?
C233 C234 C235 . . . 120.1(8) ?
C233 C234 H234 . . . 120.3(9) ?
C235 C234 H234 . . . 119.6(10) ?
C234 C235 C236 . . . 119.8(9) ?
C234 C235 H235 . . . 121.2(9) ?
C236 C235 H235 . . . 119.1(9) ?
C231 C236 C235 . . . 121.1(8) ?
C231 C236 H236 . . . 119.3(8) ?
C235 C236 H236 . . . 119.6(9) ?
C23 C24 C25 . . . 104.5(7) ?
C23 C24 H24 . . . 128.2(8) ?
C25 C24 H24 . . . 127.4(8) ?
N21 C25 C24 . . . 109.2(7) ?
N21 C25 C251 . . . 122.0(7) ?
C24 C25 C251 . . . 128.8(8) ?
C25 C251 C252 . . . 122.7(7) ?
C25 C251 C256 . . . 120.6(7) ?
C252 C251 C256 . . . 116.7(8) ?
C251 C252 C253 . . . 122.9(8) ?
C251 C252 H252 . . . 118.1(8) ?
C253 C252 H252 . . . 119.0(8) ?
C252 C253 C254 . . . 118.9(8) ?
C252 C253 H253 . . . 120.3(8) ?
C254 C253 H253 . . . 120.8(9) ?
C253 C254 C255 . . . 120.5(9) ?
C253 C254 H254 . . . 119.0(9) ?
C255 C254 H254 . . . 120.5(9) ?
C254 C255 C256 . . . 120.0(9) ?
C254 C255 H255 . . . 120.4(9) ?
C256 C255 H255 . . . 119.7(9) ?
C251 C256 C255 . . . 120.8(8) ?
C251 C256 H256 . . . 119.3(8) ?
C255 C256 H256 . . . 120.0(9) ?
Tl3 N31 Tl4 . . . 91.1(2) ?
Tl3 N31 N32 . . . 119.7(5) ?
Tl3 N31 C35 . . . 119.5(5) ?
Tl4 N31 N32 . . . 86.1(4) ?
Tl4 N31 C35 . . . 128.5(5) ?
N32 N31 C35 . . . 108.1(7) ?
Tl2 N32 N31 . . . 129.1(5) ?
Tl2 N32 C33 . . . 115.7(5) ?
N31 N32 C33 . . . 107.0(6) ?
N32 C33 C331 . . . 120.9(7) ?
N32 C33 C34 . . . 110.0(7) ?
C331 C33 C34 . . . 129.1(7) ?
C33 C331 C332 . . . 122.0(7) ?
C33 C331 C336 . . . 120.0(7) ?
C332 C331 C336 . . . 118.0(7) ?
C331 C332 C333 . . . 121.5(8) ?
C331 C332 H332 . . . 119.2(8) ?
C333 C332 H332 . . . 119.3(9) ?
C332 C333 C334 . . . 118.5(8) ?
C332 C333 H333 . . . 120.1(9) ?
C334 C333 H333 . . . 121.4(9) ?
C333 C334 C335 . . . 120.6(9) ?
C333 C334 H334 . . . 119.4(9) ?
C335 C334 H334 . . . 120.0(10) ?
C334 C335 C336 . . . 121.2(9) ?
C334 C335 H335 . . . 119.6(9) ?
C336 C335 H335 . . . 119.2(9) ?
C331 C336 C335 . . . 120.1(8) ?
C331 C336 H336 . . . 119.4(8) ?
C335 C336 H336 . . . 120.5(9) ?
C33 C34 C35 . . . 105.4(7) ?
C33 C34 H34 . . . 127.3(8) ?
C35 C34 H34 . . . 127.3(8) ?
N31 C35 C34 . . . 109.4(7) ?
N31 C35 C351 . . . 121.9(7) ?
C34 C35 C351 . . . 128.6(8) ?
C35 C351 C352 . . . 122.4(8) ?
C35 C351 C356 . . . 120.2(8) ?
C352 C351 C356 . . . 117.4(8) ?
C351 C352 C353 . . . 120.7(9) ?
C351 C352 H352 . . . 119.7(9) ?
C353 C352 H352 . . . 119.7(10) ?
C352 C353 C354 . . . 120.3(10) ?
C352 C353 H353 . . . 119.4(10) ?
C354 C353 H353 . . . 120.3(9) ?
C353 C354 C355 . . . 120.4(9) ?
C353 C354 H354 . . . 120.4(12) ?
C355 C354 H354 . . . 119.1(11) ?
C354 C355 C356 . . . 119.4(10) ?
C354 C355 H355 . . . 120.7(9) ?
C356 C355 H355 . . . 119.9(11) ?
C351 C356 C355 . . . 121.7(9) ?
C351 C356 H356 . . . 118.6(9) ?
C355 C356 H356 . . . 119.6(10) ?
Cl1 C0 Cl2 . . . 111.9(5) ?
Cl1 C0 H0a . . . 109.2(7) ?
Cl1 C0 H0b . . . 109.2(7) ?
Cl2 C0 H0a . . . 109.4(8) ?
Cl2 C0 H0b . . . 109.5(8) ?
H0a C0 H0b . . . 107.6(9) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Tl1 Tl2 . . 4.0801(7) ?
Tl1 O0 . . 2.432(6) ?
Tl1 N11 . . 2.613(6) ?
Tl1 N21 . . 2.933(7) ?
Tl1 Tl1 . '3 656' 3.5317(6) ?
Tl1 Tl4 . '3 656' 4.0813(6) ?
Tl2 N11 . . 3.065(7) ?
Tl2 N12 . . 2.737(7) ?
Tl2 N21 . . 2.722(7) ?
Tl2 N32 . . 2.642(7) ?
Tl3 Tl4 . . 3.9679(7) ?
Tl3 O0 . . 2.485(6) ?
Tl3 N12 . . 2.606(7) ?
Tl3 N31 . . 2.648(7) ?
Tl4 O0 . . 2.432(6) ?
Tl4 N22 . . 2.591(7) ?
Tl4 N31 . . 2.905(7) ?
O0 H0 . . .851(5) ?
N11 N12 . . 1.389(10) ?
N11 C15 . . 1.327(10) ?
N12 C13 . . 1.363(10) ?
C13 C131 . . 1.465(12) ?
C13 C14 . . 1.393(12) ?
C131 C132 . . 1.389(12) ?
C131 C136 . . 1.409(11) ?
C132 C133 . . 1.384(12) ?
C132 H132 . . .969(8) ?
C133 C134 . . 1.367(12) ?
C133 H133 . . .969(9) ?
C134 C135 . . 1.377(13) ?
C134 H134 . . .957(9) ?
C135 C136 . . 1.384(13) ?
C135 H135 . . .960(9) ?
C136 H136 . . .969(9) ?
C14 C15 . . 1.413(12) ?
C14 H14 . . .963(8) ?
C15 C151 . . 1.474(11) ?
C151 C152 . . 1.396(12) ?
C151 C156 . . 1.381(12) ?
C152 C153 . . 1.401(13) ?
C152 H152 . . .961(8) ?
C153 C154 . . 1.359(13) ?
C153 H153 . . .966(9) ?
C154 C155 . . 1.404(13) ?
C154 H154 . . .955(9) ?
C155 C156 . . 1.393(13) ?
C155 H155 . . .961(9) ?
C156 H156 . . .965(9) ?
N21 N22 . . 1.372(10) ?
N21 C25 . . 1.367(11) ?
N22 C23 . . 1.345(10) ?
C23 C231 . . 1.486(11) ?
C23 C24 . . 1.404(12) ?
C231 C232 . . 1.401(12) ?
C231 C236 . . 1.394(12) ?
C232 C233 . . 1.381(12) ?
C232 H232 . . .962(9) ?
C233 C234 . . 1.376(14) ?
C233 H233 . . .963(9) ?
C234 C235 . . 1.375(14) ?
C234 H234 . . .973(9) ?
C235 C236 . . 1.391(12) ?
C235 H235 . . .971(10) ?
C236 H236 . . .964(9) ?
C24 C25 . . 1.401(12) ?
C24 H24 . . .966(8) ?
C25 C251 . . 1.446(12) ?
C251 C252 . . 1.410(12) ?
C251 C256 . . 1.383(12) ?
C252 C253 . . 1.377(12) ?
C252 H252 . . .961(8) ?
C253 C254 . . 1.363(13) ?
C253 H253 . . .968(8) ?
C254 C255 . . 1.389(13) ?
C254 H254 . . .971(10) ?
C255 C256 . . 1.400(13) ?
C255 H255 . . .970(9) ?
C256 H256 . . .969(9) ?
N31 N32 . . 1.380(10) ?
N31 C35 . . 1.357(11) ?
N32 C33 . . 1.353(11) ?
C33 C331 . . 1.493(11) ?
C33 C34 . . 1.386(11) ?
C331 C332 . . 1.391(12) ?
C331 C336 . . 1.401(12) ?
C332 C333 . . 1.388(12) ?
C332 H332 . . .968(9) ?
C333 C334 . . 1.371(14) ?
C333 H333 . . .960(9) ?
C334 C335 . . 1.371(14) ?
C334 H334 . . .974(10) ?
C335 C336 . . 1.358(13) ?
C335 H335 . . .973(10) ?
C336 H336 . . .966(8) ?
C34 C35 . . 1.378(12) ?
C34 H34 . . .964(8) ?
C35 C351 . . 1.475(11) ?
C351 C352 . . 1.402(13) ?
C351 C356 . . 1.393(13) ?
C352 C353 . . 1.397(13) ?
C352 H352 . . .960(9) ?
C353 C354 . . 1.372(16) ?
C353 H353 . . .972(11) ?
C354 C355 . . 1.375(17) ?
C354 H354 . . .955(10) ?
C355 C356 . . 1.396(13) ?
C355 H355 . . .967(11) ?
C356 H356 . . .966(10) ?
Cl1 C0 . . 1.777(9) ?
Cl2 C0 . . 1.739(10) ?
C0 H0a . . .962(10) ?
C0 H0b . . .961(10) ?
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Tl1 Tl3 4.2841(7) . . ?
Tl1 Tl4 4.2070(8) . . ?
Tl1 N12 3.548(7) . . ?
Tl1 C15 3.605(8) . . ?
Tl1 C151 3.861(8) . . ?
Tl1 C156 3.576(8) . . ?
Tl1 N21 3.390(7) . '3 656' ?
Tl1 N22 3.511(7) . '3 656' ?
Tl1 N22 3.802(7) . . ?
Tl1 C23 3.606(8) . '3 656' ?
Tl1 C24 3.562(8) . '3 656' ?
Tl1 C25 3.743(9) . . ?
Tl1 C25 3.411(8) . '3 656' ?
Tl1 C251 3.896(8) . . ?
Tl1 C251 3.987(8) . '3 656' ?
Tl1 C252 3.477(8) . . ?
Tl1 Cl1 3.862(3) . . ?
Tl1 H0 2.6110(4) . . ?
Tl1 H156 3.0403(5) . . ?
Tl1 H252 2.9696(5) . . ?
Tl2 Tl3 4.3674(9) . . ?
Tl2 Tl4 4.4490(8) . . ?
Tl2 O0 4.036(6) . . ?
Tl2 C13 3.305(8) . . ?
Tl2 C131 3.934(8) . . ?
Tl2 C132 3.804(8) . . ?
Tl2 C135 3.918(9) . '3 657' ?
Tl2 C136 3.601(8) . '3 657' ?
Tl2 C14 3.862(8) . . ?
Tl2 C15 3.696(8) . . ?
Tl2 N22 3.146(7) . . ?
Tl2 C23 4.167(8) . . ?
Tl2 C25 3.675(8) . . ?
Tl2 C252 4.080(9) . . ?
Tl2 N31 3.671(7) . . ?
Tl2 C33 3.450(8) . . ?
Tl2 C331 3.548(8) . . ?
Tl2 C332 3.274(9) . . ?
Tl2 C333 4.144(9) . . ?
Tl2 H132 3.1704(5) . . ?
Tl2 H136 3.4054(6) . '3 657' ?
Tl2 H14 3.5647(7) . '3 657' ?
Tl2 H252 3.3068(5) . . ?
Tl2 H332 2.9081(5) . . ?
Tl3 N11 3.491(7) . . ?
Tl3 C13 3.535(8) . . ?
Tl3 C131 3.796(8) . . ?
Tl3 C132 3.590(9) . . ?
Tl3 C134 4.041(9) . '4 554' ?
Tl3 C135 3.921(9) . '4 554' ?
Tl3 C255 3.878(9) . '2 656' ?
Tl3 C256 4.125(9) . '2 656' ?
Tl3 N32 3.541(7) . . ?
Tl3 C35 3.520(8) . . ?
Tl3 C351 3.783(8) . . ?
Tl3 C352 3.554(9) . . ?
Tl3 Cl1 3.611(2) . . ?
Tl3 C0 3.857(10) . . ?
Tl3 H0 2.9739(6) . . ?
Tl3 H132 3.1134(6) . . ?
Tl3 H134 3.6136(6) . '4 554' ?
Tl3 H135 3.3736(6) . '4 554' ?
Tl3 H352 3.0688(5) . . ?
Tl3 H0a 3.4647(6) . . ?
Tl4 N21 3.507(7) . . ?
Tl4 C23 3.481(8) . . ?
Tl4 C231 3.720(8) . . ?
Tl4 C232 3.450(9) . . ?
Tl4 C233 4.163(9) . '3 556' ?
Tl4 C234 3.950(9) . '3 556' ?
Tl4 C252 4.077(8) . '3 656' ?
Tl4 C253 3.824(8) . '3 656' ?
Tl4 C254 3.855(10) . '3 656' ?
Tl4 C255 4.174(9) . '3 656' ?
Tl4 N32 3.130(7) . . ?
Tl4 C33 4.146(8) . . ?
Tl4 C35 3.896(8) . . ?
Tl4 H0 2.6395(5) . . ?
Tl4 H232 2.9938(5) . . ?
Tl4 H233 3.6289(6) . '3 556' ?
Tl4 H234 3.2038(5) . '3 556' ?
Tl4 H352 3.5579(6) . . ?
O0 Cl1 3.856(6) . . ?
N11 C13 2.217(10) . . ?
N11 C14 2.247(10) . . ?
N11 C151 2.457(10) . . ?
N11 Cl1 3.503(7) . . ?
N12 C131 2.458(10) . . ?
N12 C132 2.962(11) . . ?
N12 C14 2.253(11) . . ?
N12 C15 2.204(11) . . ?
N12 Cl1 3.849(7) . . ?
C13 C132 2.509(12) . . ?
C13 C136 2.484(12) . . ?
C13 C15 2.217(12) . . ?
C13 H14 2.122(8) . . ?
C131 C133 2.410(12) . . ?
C131 C134 2.796(12) . . ?
C131 C135 2.437(12) . . ?
C131 C14 2.587(12) . . ?
C131 H132 2.048(8) . . ?
C131 H136 2.062(8) . . ?
C132 C134 2.394(12) . . ?
C132 C135 2.771(12) . . ?
C132 C136 2.391(12) . . ?
C132 H133 2.049(9) . . ?
C133 C135 2.378(13) . . ?
C133 C136 2.743(12) . . ?
C133 H132 2.047(9) . . ?
C133 H134 2.019(9) . . ?
C134 C136 2.384(13) . . ?
C134 H133 2.023(9) . . ?
C134 H135 2.031(9) . . ?
C135 Cl1 3.686(10) . 4 ?
C135 H134 2.035(10) . . ?
C135 H136 2.043(10) . . ?
C136 Cl1 3.870(9) . 4 ?
C136 H135 2.050(8) . . ?
C14 C151 2.589(12) . . ?
C15 C152 2.485(12) . . ?
C15 C156 2.498(12) . . ?
C15 Cl2 3.923(8) . . ?
C15 H14 2.146(8) . . ?
C151 C153 2.440(12) . . ?
C151 C154 2.801(12) . . ?
C151 C155 2.416(13) . . ?
C151 H152 2.039(8) . . ?
C151 H156 2.035(8) . . ?
C152 C154 2.385(13) . . ?
C152 C155 2.757(13) . . ?
C152 C156 2.380(12) . . ?
C152 H153 2.066(9) . . ?
C153 C155 2.396(13) . . ?
C153 C156 2.776(12) . . ?
C153 H152 2.056(9) . . ?
C153 H154 2.010(9) . . ?
C154 C156 2.417(12) . . ?
C154 H153 2.024(9) . . ?
C154 H155 2.057(9) . . ?
C155 H154 2.057(9) . . ?
C155 H156 2.048(9) . . ?
C156 Cl2 3.827(9) . . ?
C156 H155 2.058(9) . . ?
N21 C23 2.202(11) . . ?
N21 C24 2.256(11) . . ?
N21 C251 2.460(11) . . ?
N21 C252 2.945(11) . . ?
N22 C231 2.479(10) . . ?
N22 C232 2.983(11) . . ?
N22 C24 2.253(11) . . ?
N22 C25 2.216(11) . . ?
C23 C232 2.521(12) . . ?
C23 C236 2.500(12) . . ?
C23 C25 2.217(12) . . ?
C23 H24 2.139(8) . . ?
C231 C233 2.416(12) . . ?
C231 C234 2.794(12) . . ?
C231 C235 2.425(12) . . ?
C231 C24 2.594(12) . . ?
C231 H232 2.054(8) . . ?
C231 H236 2.047(8) . . ?
C232 C234 2.395(13) . . ?
C232 C235 2.768(13) . . ?
C232 C236 2.394(13) . . ?
C232 H233 2.035(9) . . ?
C233 C235 2.383(14) . . ?
C233 C236 2.755(13) . . ?
C233 H232 2.039(9) . . ?
C233 H234 2.047(9) . . ?
C234 C236 2.392(13) . . ?
C234 H233 2.036(10) . . ?
C234 H235 2.053(10) . . ?
C235 H234 2.040(9) . . ?
C235 H236 2.047(9) . . ?
C236 Cl1 3.747(9) . '3 656' ?
C236 H235 2.047(9) . . ?
C24 C251 2.567(12) . . ?
C24 Cl1 3.618(9) . '3 656' ?
C24 Cl2 3.936(9) . '2 646' ?
C25 C252 2.507(12) . . ?
C25 C256 2.458(12) . . ?
C25 H24 2.130(8) . . ?
C251 C253 2.448(12) . . ?
C251 C254 2.802(13) . . ?
C251 C255 2.420(12) . . ?
C251 H252 2.047(8) . . ?
C251 H256 2.040(8) . . ?
C252 C254 2.359(13) . . ?
C252 C255 2.734(13) . . ?
C252 C256 2.378(12) . . ?
C252 H253 2.043(9) . . ?
C253 C255 2.389(13) . . ?
C253 C256 2.782(12) . . ?
C253 H252 2.025(9) . . ?
C253 H254 2.020(9) . . ?
C254 C256 2.415(13) . . ?
C254 H253 2.036(10) . . ?
C254 H255 2.057(10) . . ?
C255 H254 2.059(9) . . ?
C255 H256 2.062(9) . . ?
C256 H0 2.467(9) . '3 656' ?
C256 H255 2.060(9) . . ?
N31 C33 2.197(10) . . ?
N31 C34 2.233(11) . . ?
N31 C351 2.476(11) . . ?
N31 C352 2.975(11) . . ?
N32 C331 2.476(11) . . ?
N32 C332 2.987(11) . . ?
N32 C34 2.244(11) . . ?
N32 C35 2.216(10) . . ?
C33 C332 2.523(12) . . ?
C33 C336 2.507(11) . . ?
C33 C35 2.198(11) . . ?
C33 H34 2.114(8) . . ?
C331 C333 2.425(12) . . ?
C331 C334 2.770(12) . . ?
C331 C335 2.390(12) . . ?
C331 C34 2.599(11) . . ?
C331 H332 2.046(8) . . ?
C331 H336 2.056(8) . . ?
C332 C334 2.372(13) . . ?
C332 C335 2.734(13) . . ?
C332 C336 2.393(12) . . ?
C332 H333 2.046(9) . . ?
C333 C335 2.382(13) . . ?
C333 C336 2.774(12) . . ?
C333 Cl1 3.938(9) . '2 646' ?
C333 Cl2 3.808(10) . '2 646' ?
C333 H332 2.045(9) . . ?
C333 H334 2.035(9) . . ?
C334 C336 2.378(13) . . ?
C334 Cl2 3.881(11) . '3 657' ?
C334 H333 2.043(10) . . ?
C334 H335 2.035(10) . . ?
C335 H334 2.040(10) . . ?
C335 H336 2.027(10) . . ?
C336 H335 2.020(8) . . ?
C34 C351 2.571(12) . . ?
C35 C352 2.521(12) . . ?
C35 C356 2.486(12) . . ?
C35 H34 2.107(8) . . ?
C351 C353 2.432(13) . . ?
C351 C354 2.805(13) . . ?
C351 C355 2.437(13) . . ?
C351 H352 2.054(9) . . ?
C351 H356 2.041(9) . . ?
C352 C354 2.402(13) . . ?
C352 C355 2.773(14) . . ?
C352 C356 2.388(14) . . ?
C352 H353 2.057(9) . . ?
C353 C355 2.384(16) . . ?
C353 C356 2.756(15) . . ?
C353 H352 2.049(9) . . ?
C353 H354 2.031(10) . . ?
C354 C356 2.393(15) . . ?
C354 H353 2.043(13) . . ?
C354 H355 2.045(13) . . ?
C355 Cl2 3.425(10) . '1 455' ?
C355 H354 2.021(11) . . ?
C355 H356 2.053(10) . . ?
C356 Cl2 3.839(9) . '1 455' ?
C356 H355 2.057(9) . . ?
Cl1 Cl2 2.914(4) . . ?
Cl1 H135 3.099(3) . '4 554' ?
Cl1 H136 3.433(3) . '4 554' ?
Cl1 H156 3.268(3) . . ?
Cl1 H236 2.847(2) . '3 656' ?
Cl1 H24 3.068(2) . '3 656' ?
Cl1 H333 3.112(3) . '2 656' ?
Cl1 H0a 2.281(2) . . ?
Cl1 H0b 2.281(2) . . ?
Cl2 H333 2.906(3) . '2 656' ?
Cl2 H334 3.230(3) . '3 657' ?
Cl2 H355 3.031(3) . '1 655' ?
Cl2 H0a 2.249(3) . . ?
Cl2 H0b 2.251(3) . . ?
H0a H0b 1.5514(3) . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
? ? ? ? ? ? ? ? ? ? ?
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
? ? ? ? ? ? ? ? ? ?
