#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/93/2019350.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_2019350
loop_
_publ_author_name
'Zahn, G.'
'Franke, A.'
'Dietzsch, W.'
_publ_section_title
;
 Bis(tetra-n-butylammonium)
 Bis(μ-1,1-dicyanoethene-2,2-diselenolato)dithallate(I) Acetone Solvate,
 [(C4H9)4N]2[Tl2{Se2C=C(CN)2}2].2(CH3)2CO
;
_journal_issue                   5
_journal_name_full
'Acta Crystallographica Section C Crystal Structure Communications'
_journal_page_first              854
_journal_paper_doi               10.1107/S0108270194003562
_journal_volume                  51
_journal_year                    1995
_chemical_formula_sum            'C46 H84 N6 O2 Se4 Tl2'
_chemical_formula_weight         1477.82
_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_type_scat_source           IntTabIV
_cell_angle_alpha                90
_cell_angle_beta                 107.980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.973(2)
_cell_length_b                   12.572(2)
_cell_length_c                   18.993(2)
_cell_measurement_reflns_used    70
_cell_measurement_temperature    296
_cell_measurement_theta_max      14.4
_cell_measurement_theta_min      10.2
_cell_volume                     2946.4(7)
_diffrn_measurement_device       'Stoe Stadi 4'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7449
_diffrn_reflns_theta_max         27.5
_diffrn_standards_decay_%        <2
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9
_exptl_absorpt_correction_T_max  0.259
_exptl_absorpt_correction_T_min  0.118
_exptl_absorpt_correction_type   'empirical \y scan (Flack, 1974)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_description       '{011} prism and {101} pinacoid'
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.73
_refine_diff_density_min         -0.59
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.52
_refine_ls_hydrogen_treatment
' refall with restraints, except for those of solvent'
_refine_ls_number_parameters     282
_refine_ls_number_reflns         2263
_refine_ls_R_factor_obs          0.0504
_refine_ls_shift/esd_max         <0.01
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w=1/[σ~(F²)~ + 0.000349F²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0474
_reflns_number_observed          2263
_reflns_number_total             6764
_reflns_observed_criterion       I>=2\s~I~
_cod_data_source_file            sh1009sup1.cif
_cod_data_source_block           sh1009a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w=1/[\s~(F^2^)~ + 0.000349F^2^]'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w=1/[\s~(F^2^)~ +
0.000349F^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2946.4
_cod_database_code               2019350
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2+x,1/2-y,1/2+z
-x,-y,-z
1/2-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
Tl .01077(5) .14150(5) -.00132(4) .0917(3)
Se(1) .05863(10) .00812(15) .14503(7) .0869(6)
Se(2) -.18093(10) .01855(13) .02938(7) .0775(6)
N(1) -.3387(9) .0203(10) .1644(7) .083(5)
N(2) -.0240(9) .0165(11) .3234(6) .085(5)
C(1) -.0890(8) .0152(9) .1291(6) .053(4)
C(2) -.1344(9) .0170(10) .1854(6) .054(4)
C(3) -.2503(12) .0189(10) .1736(6) .062(5)
C(4) -.0695(10) .0161(12) .2618(8) .072(6)
N(3) -.0265(7) .2488(8) .4999(6) .058(4)
C(5) -.0674(9) .3123(10) .5541(6) .056(5)
C(6) -.1161(10) .2479(11) .6029(7) .070(5)
C(7) -.1572(11) .3227(12) .6498(8) .089(6)
C(8) -.2075(12) .2651(15) .7020(9) .124(8)
C(9) .0630(9) .1716(10) .5408(7) .062(5)
C(10) .1626(10) .2203(10) .5940(7) .067(6)
C(11) .2446(10) .1356(12) .6250(9) .090(6)
C(12) .3460(12) .1753(13) .6790(10) .118(8)
C(13) .0167(9) .3311(9) .4573(6) .056(5)
C(14) .0687(10) .2902(11) .4030(7) .073(6)
C(15) .0969(11) .3833(13) .3619(7) .090(6)
C(16) .1594(13) .3484(15) .3105(9) .132(8)
C(17) -.1160(10) .1848(10) .4475(7) .062(5)
C(18) -.2119(10) .2435(11) .4009(8) .078(6)
C(19) -.2930(11) .1683(12) .3536(9) .094(7)
C(20) -.3945(14) .2188(15) .3050(11) .151(9)
O(1A) .1512(5) .4270(17) .0309(11) .151(8)
C(21A) .252(2) .542(3) .1273(16) .162(12)
C(22A) .1497(15) .488(2) .0805(13) .110(9)
C(23A) .056(2) .488(3) .113(2) .194(14)
O(1B) .192(4) .612(3) .101(3) .245(14)
C(21B) .235(6) .489(5) .018(4) .245(14)
C(22B) .178(5) .524(4) .073(3) .245(14)
C(23B) .091(6) .450(5) .082(5) .245(14)
H5A -.1285(9) .3670(10) .5226(6) .075(16)
H5B .0002(9) .3566(10) .5896(6) .075(16)
H6A -.0552(10) .1962(11) .6380(7) .097(18)
H6B -.1823(10) .2006(11) .5689(7) .097(18)
H7A -.0903(11) .3705(12) .6825(8) .16(2)
H7B -.2179(11) .3738(12) .6138(8) .16(2)
H8A -.2354(12) .3228(15) .7341(9) .27(2)
H8B -.1475(12) .2143(15) .7388(9) .27(2)
H8C -.2751(12) .2176(15) .6701(9) .27(2)
H9A .0879(9) .1280(10) .4997(7) .065(16)
H9B .0289(9) .1171(10) .5716(7) .065(16)
H10A .1413(10) .2587(10) .6384(7) .074(17)
H10B .1962(10) .2784(10) .5653(7) .074(17)
H11A .2649(10) .0983(12) .5798(9) .126(19)
H11B .2090(10) .0775(12) .6524(9) .126(19)
H12A .4009(12) .1096(13) .6989(10) .22(2)
H12B .3274(12) .2122(13) .7251(10) .22(2)
H12C .3833(12) .2330(13) .6525(10) .22(2)
H13A .0760(9) .3786(9) .4973(6) .0466(15)
H13B -.0506(9) .3807(9) .4275(6) .0466(15)
H14A .1416(10) .2472(11) .4317(7) .052(15)
H14B .0134(10) .2378(11) .3642(7) .052(15)
H15A .0228(11) .4217(13) .3297(7) .17(2)
H15B .1456(11) .4390(13) .4017(7) .17(2)
H16A .1779(13) .4170(15) .2823(9) .26(2)
H16B .1111(13) .2930(15) .2703(9) .26(2)
H16C .2339(13) .3104(15) .3422(9) .26(2)
H17A -.1443(10) .1283(10) .4802(7) .053(15)
H17B -.0813(10) .1427(10) .4107(7) .053(15)
H18A -.2485(10) .2867(11) .4362(8) .107(18)
H18B -.1866(10) .2989(11) .3660(8) .107(18)
H19A -.2549(11) .1264(12) .3186(9) .129(19)
H19B -.3153(11) .1123(12) .3895(9) .129(19)
H20A -.4476(14) .1581(15) .2732(11) .34(2)
H20B -.3743(14) .2744(15) .2679(11) .34(2)
H20C -.4347(14) .2604(15) .3388(11) .34(2)
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
Se(1) Tl Se(2) . . . 61.50(10) yes
Se(1) Tl Se(2) . 3_555 . 60.60(10) yes
Se(1) Tl Se(2) . . 3_555 81.50(10) yes
Se(1) Tl Se(2) . 3_555 3_555 80.70(10) yes
Se(1) Tl Se(1) . . 3_555 111.50(10) yes
Se(2) Tl Se(2) . . 3_555 110.80(10) yes
Se(1) Se(2) Se(1) . . 3_555 90.90(10) yes
Se(2) Se(1) Se(2) . . 3_555 89.10(10) yes
Se(1) C(1) Se(2) . . . 117.7(5) yes
Se(1) C(1) C(2) . . . 123.1(7) yes
Se(2) C(1) C(2) . . . 119.2(7) yes
C(1) C(2) C(3) . . . 124.0(10) yes
C(1) C(2) C(4) . . . 122.0(10) yes
C(3) C(2) C(4) . . . 114.0(10) yes
C(2) C(3) N(1) . . . 180.0(10) yes
C(2) C(4) N(2) . . . 176.0(10) yes
Se(2) H(15B) C(15) . 2_454 2_454 150.0(10) yes
Se(2) H(5A) C(5) . 4_445 4_445 165.0(10) yes
Se(2) H(10B) C(10) . 2_454 2_454 163.0(10) yes
N(1) H(13B) C(13) . 4_445 4_445 160.0(10) yes
N(1) H(5B) C(5) . 2_454 2_454 174.0(10) yes
N(2) H(17B) C(17) . . . 170.0(10) yes
N(2) H(9B) C(9) . 3_556 3_556 158.0(10) yes
Tl O(1A) C(22A) . . . 125(2) yes
Tl Tl O(1A) 3_555 . . 158.0(10) yes
Tl O(1B) C(22B) . 3_565 3_565 120(3) yes
Tl Tl O(1B) 3_555 . 3_565 135.0(10) yes
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
Tl Tl 3_555 3.5700(10) yes
Tl Se(1) . 3.140(2) yes
Tl Se(1) 3_555 3.207(2) yes
Tl Se(2) . 3.132(2) yes
Tl Se(2) 3_555 3.151(2) yes
Se(1) Se(2) . 3.207(2) yes
Se(1) Se(2) 3_555 4.104(2) yes
Se(1) C(1) . 1.850(10) yes
Se(2) C(1) . 1.900(10) yes
C(1) C(2) . 1.37(2) yes
C(2) C(3) . 1.45(2) yes
C(2) C(4) . 1.44(2) yes
C(3) N(1) . 1.11(2) yes
C(4) N(2) . 1.14(2) yes
Se(2) H(15B) 2_454 2.800(10) yes
Se(2) H(5A) 4_445 3.040(10) yes
Se(2) H(10B) 2_454 3.190(10) yes
N(1) H(13B) 4_445 2.58(2) yes
N(1) H(5B) 2_454 2.64(2) yes
N(2) H(17B) . 2.56(2) yes
N(2) H(9B) 3_556 2.62(2) yes
Tl O(1A) . 3.99(2) yes
Tl O(1B) 3_565 4.13(5) yes
