#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/63/2006360.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# 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_2006360
loop_
_publ_author_name
'James, Sian C.'
'Norman, Nicholas C.'
'Orpen, A. Guy'
'Quayle, Michael J.'
_publ_section_title
;
 Tetrahydrofuran Adducts of a Chlorobismuthate(III) Anion and Antimony
 Triiodide
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1024
_journal_page_last               1027
_journal_paper_doi               10.1107/S0108270197004009
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          '[Li (C4 H8 O)4][Bi2 Cl8 (C4 H8 O)]'
_chemical_formula_structural     '[Bi2 (\m-Cl)2 (Cl)8 (thf)] [Li(thf)4]'
_chemical_formula_sum            'C20 H40 Bi Cl4 Li O5'
_chemical_formula_weight         718.24
_chemical_name_systematic
;
Bis(Tetra(thf))lithium(I) Tetrachloro di(μ-chloro) bis(thf)dibismuthate(III)
;
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 104.24(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.598(2)
_cell_length_b                   24.577(3)
_cell_length_c                   11.378(4)
_cell_measurement_reflns_used    72
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      50
_cell_measurement_theta_min      5
_cell_volume                     2872.5(12)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXTL-Plus
_computing_structure_refinement  SHELXTL-Plus
_computing_structure_solution    'SHELXTL-Plus (Sheldrick, 1995)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 60
_diffrn_measured_fraction_theta_max 97
_diffrn_measurement_device       'Siemens SMART area detector'
_diffrn_measurement_method       'ω rotation with narrow frame'
_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  0.1286
_diffrn_reflns_av_sigmaI/netI    0.1756
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13321
_diffrn_reflns_theta_full        49.91
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    6.535
_exptl_absorpt_correction_T_max  0.0955
_exptl_absorpt_correction_T_min  0.0441
_exptl_absorpt_correction_type   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         '1.79  (0.91 \%A from Bi1)'
_refine_diff_density_min         '-2.07  (0.36 \%A from Bi1)'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.854
_refine_ls_goodness_of_fit_obs   0.994
_refine_ls_hydrogen_treatment    'H atoms: see text'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.854
_refine_ls_restrained_S_obs      0.994
_refine_ls_R_factor_all          0.1236
_refine_ls_R_factor_obs          .0498
_refine_ls_shift/esd_max         -0.015
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.021P)²] where P=[max(Fo²,0)+2Fc²]/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0863
_refine_ls_wR_factor_obs         .0716
_reflns_number_observed          2685
_reflns_number_total             5039
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            bm1150.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.021P)^2^] where P=[max(Fo^2^,0)+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^)+(0.021P)^2^] where P=[max(Fo^2^,0)+2Fc^2^]/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2872.7(12)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C20 H40 Bi1 Cl4 Li O5'
_cod_database_code               2006360
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_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_group
_atom_site_type_symbol
Bi1 .84344(4) .938365(14) .46489(4) .03731(13) Uani d . 1 . Bi
Cl1 .9818(3) .85929(11) .4205(3) .0597(8) Uani d . 1 . Cl
Cl2 1.0468(3) .97858(11) .6650(2) .0628(9) Uani d . 1 . Cl
Cl3 .7437(3) .87861(10) .6035(3) .0557(8) Uani d . 1 . Cl
Cl4 .6527(3) .92008(10) .2797(2) .0535(8) Uani d . 1 . Cl
Li1 .1679(19) .8303(7) .0091(17) .060(6) Uani d . 1 . Li
O1 .1399(7) .7915(3) -.1436(6) .055(2) Uani d . 1 . O
O2 .3184(8) .8753(3) .0255(7) .061(2) Uani d . 1 . O
O3 .1837(8) .7816(3) .1420(7) .052(2) Uani d . 1 . O
O4 .0200(7) .8765(3) .0055(7) .067(2) Uani d . 1 . O
O5 .6937(8) 1.0131(3) .5165(7) .076(3) Uani d . 1 . O
C11 .1318(11) .8168(4) -.2573(9) .050(3) Uani d . 1 . C
H11A .1750(11) .8528(4) -.2457(9) .060 Uiso calc R 1 . H
H11B .0396(11) .8220(4) -.3012(9) .060 Uiso calc R 1 . H
C12 .1978(16) .7804(5) -.3259(12) .120(6) Uani d . 1 . C
H12A .1443(16) .7759(5) -.4098(12) .144 Uiso calc R 1 . H
H12B .2832(16) .7958(5) -.3292(12) .144 Uiso calc R 1 . H
C13 .2151(13) .7296(5) -.2655(12) .082(4) Uani d . 1 . C
H13A .3066(13) .7176(5) -.2530(12) .098 Uiso calc R 1 . H
H13B .1583(13) .7019(5) -.3155(12) .098 Uiso calc R 1 . H
C14 .1818(11) .7352(4) -.1461(10) .057(3) Uani d . 1 . C
H14A .1110(11) .7098(4) -.1403(10) .069 Uiso calc R 1 . H
H14B .2587(11) .7278(4) -.0785(10) .069 Uiso calc R 1 . H
C21 .3165(13) .9348(5) .0210(14) .086(4) Uani d . 1 . C
H21A .2269(13) .9489(5) .0102(14) .103 Uiso calc R 1 . H
H21B .3726(13) .9505(5) .0960(14) .103 Uiso calc R 1 . H
C22 .3662(13) .9475(5) -.0821(14) .098(5) Uani d . 1 . C
H22A .4104(13) .9832(5) -.0707(14) .117 Uiso calc R 1 . H
H22B .2940(13) .9491(5) -.1562(14) .117 Uiso calc R 1 . H
C23 .4609(13) .9036(6) -.0945(13) .095(5) Uani d . 1 . C
H23A .5518(13) .9168(6) -.0685(13) .114 Uiso calc R 1 . H
H23B .4439(13) .8904(6) -.1791(13) .114 Uiso calc R 1 . H
C24 .4345(11) .8593(4) -.0098(11) .064(4) Uani d . 1 . C
H24A .4213(11) .8237(4) -.0521(11) .077 Uiso calc R 1 . H
H24B .5086(11) .8560(4) .0623(11) .077 Uiso calc R 1 . H
C31 .3013(11) .7674(4) .2239(11) .064(4) Uani d . 1 . C
H31A .3626(11) .7985(4) .2380(11) .077 Uiso calc R 1 . H
H31B .3427(11) .7362(4) .1930(11) .077 Uiso calc R 1 . H
C32 .2630(15) .7522(5) .3396(12) .099(5) Uani d . 1 . C
H32A .2613(15) .7847(5) .3907(12) .119 Uiso calc R 1 . H
H32B .3243(15) .7252(5) .3870(12) .119 Uiso calc R 1 . H
C33 .1285(14) .7282(5) .2959(13) .083(4) Uani d . 1 . C
H33A .0708(14) .7404(5) .3471(13) .100 Uiso calc R 1 . H
H33B .1321(14) .6879(5) .2967(13) .100 Uiso calc R 1 . H
C34 .0804(12) .7499(5) .1650(13) .083(5) Uani d . 1 . C
H34A .0594(12) .7193(5) .1068(13) .100 Uiso calc R 1 . H
H34B .0014(12) .7724(5) .1573(13) .100 Uiso calc R 1 . H
C41 -.0220(14) .8997(5) .1048(11) .083(4) Uani d . 1 . C
H41A -.0331(14) .8710(5) .1625(11) .099 Uiso calc R 1 . H
H41B .0425(14) .9265(5) .1485(11) .099 Uiso calc R 1 . H
C42 -.1429(15) .9256(7) .0534(13) .144(8) Uani d . 1 . C
H42A -.1444(15) .9618(7) .0912(13) .173 Uiso calc R 1 . H
H42B -.2146(15) .9036(7) .0705(13) .173 Uiso calc R 1 . H
C43 -.1620(12) .9317(6) -.0733(11) .087(5) Uani d . 1 . C
H43A -.1490(12) .9700(6) -.0947(11) .105 Uiso calc R 1 . H
H43B -.2507(12) .9200(6) -.1166(11) .105 Uiso calc R 1 . H
C44 -.0627(12) .8960(5) -.1034(10) .079(4) Uani d . 1 . C
H44A -.1052(12) .8651(5) -.1536(10) .095 Uiso calc R 1 . H
H44B -.0113(12) .9166(5) -.1503(10) .095 Uiso calc R 1 . H
C51 .7002(13) 1.0308(5) .6398(11) .081(4) Uani d . 1 . C
H51A .7854(13) 1.0211(5) .6941(11) .098 Uiso calc R 1 . H
H51B .6305(13) 1.0134(5) .6706(11) .098 Uiso calc R 1 . H
C52 .6831(13) 1.0905(5) .6350(12) .077(4) Uani d . 1 . C
H52A .6246(13) 1.1022(5) .6859(12) .092 Uiso calc R 1 . H
H52B .7679(13) 1.1092(5) .6632(12) .092 Uiso calc R 1 . H
C53 .6266(14) 1.1018(5) .5097(14) .107(6) Uani d . 1 . C
H53A .5329(14) 1.1102(5) .4976(14) .128 Uiso calc R 1 . H
H53B .6698(14) 1.1338(5) .4839(14) .128 Uiso calc R 1 . H
C54 .6418(13) 1.0565(5) .4403(11) .089(4) Uani d . 1 . C
H54A .7007(13) 1.0657(5) .3879(11) .106 Uiso calc R 1 . H
H54B .5564(13) 1.0460(5) .3875(11) .106 Uiso calc R 1 . H
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'
P P 0.1023 0.0942 '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'
Rh Rh -1.1178 0.9187 '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_3
_geom_angle
_geom_angle_publ_flag
Cl1 Bi1 Cl3 . 91.67(9) yes
Cl1 Bi1 Cl4 . 94.52(9) yes
Cl3 Bi1 Cl4 . 92.51(9) yes
Cl1 Bi1 O5 . 175.7(2) yes
Cl3 Bi1 O5 . 84.2(2) yes
Cl4 Bi1 O5 . 84.7(2) yes
Cl1 Bi1 Cl2 . 93.59(9) yes
Cl3 Bi1 Cl2 . 92.96(9) yes
Cl4 Bi1 Cl2 . 170.08(8) yes
O5 Bi1 Cl2 . 87.6(2) yes
Cl1 Bi1 Cl2 3_776 96.42(9) yes
Cl3 Bi1 Cl2 3_776 170.29(9) yes
Cl4 Bi1 Cl2 3_776 92.20(8) yes
O5 Bi1 Cl2 3_776 87.8(2) yes
Cl2 Bi1 Cl2 3_776 81.22(9) yes
Bi1 Cl2 Bi1 3_776 98.78(9) yes
O3 Li1 O4 . 107.4(10) ?
O3 Li1 O2 . 112.2(10) ?
O4 Li1 O2 . 108.4(9) ?
O3 Li1 O1 . 111.5(9) ?
O4 Li1 O1 . 109.1(10) ?
O2 Li1 O1 . 108.2(10) ?
C11 O1 C14 . 110.5(8) ?
C11 O1 Li1 . 124.2(8) ?
C14 O1 Li1 . 120.3(8) ?
C24 O2 C21 . 105.6(8) ?
C24 O2 Li1 . 124.3(8) ?
C21 O2 Li1 . 124.8(9) ?
C31 O3 C34 . 109.9(8) ?
C31 O3 Li1 . 125.0(9) ?
C34 O3 Li1 . 124.8(10) ?
C44 O4 C41 . 108.1(8) ?
C44 O4 Li1 . 122.9(9) ?
C41 O4 Li1 . 128.9(9) ?
C54 O5 C51 . 106.7(9) ?
C54 O5 Bi1 . 124.7(7) ?
C51 O5 Bi1 . 123.1(6) ?
O1 C11 C12 . 106.6(9) ?
C13 C12 C11 . 107.5(11) ?
C12 C13 C14 . 109.2(10) ?
O1 C14 C13 . 104.3(8) ?
C22 C21 O2 . 103.9(11) ?
C21 C22 C23 . 108.1(12) ?
C22 C23 C24 . 102.9(11) ?
O2 C24 C23 . 106.4(9) ?
O3 C31 C32 . 104.7(10) ?
C31 C32 C33 . 104.0(10) ?
C32 C33 C34 . 104.1(11) ?
O3 C34 C33 . 106.3(10) ?
C42 C41 O4 . 106.1(10) ?
C41 C42 C43 . 110.8(12) ?
C42 C43 C44 . 104.0(11) ?
O4 C44 C43 . 108.8(10) ?
O5 C51 C52 . 106.6(11) ?
C53 C52 C51 . 104.3(12) ?
C53 C54 O5 . 109.8(10) ?
C54 C53 C52 . 109.3(11) ?
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
Bi1 Cl1 . 2.558(3) yes
Bi1 Cl3 . 2.565(3) yes
Bi1 Cl4 . 2.576(3) yes
Bi1 O5 . 2.588(7) yes
Bi1 Cl2 . 2.896(3) yes
Bi1 Cl2 3_776 2.924(3) yes
Cl2 Bi1 3_776 2.924(3) ?
Li1 O3 . 1.90(2) yes
Li1 O4 . 1.93(2) yes
Li1 O2 . 1.91(2) yes
Li1 O1 . 1.94(2) yes
O1 C11 . 1.419(10) ?
O1 C14 . 1.456(10) ?
O2 C24 . 1.440(11) ?
O2 C21 . 1.463(12) ?
O3 C31 . 1.404(11) ?
O3 C34 . 1.420(12) ?
O4 C44 . 1.415(11) ?
O4 C41 . 1.430(11) ?
O5 C54 . 1.400(11) ?
O5 C51 . 1.454(12) ?
C11 C12 . 1.473(13) ?
C12 C13 . 1.414(15) ?
C13 C14 . 1.491(14) ?
C21 C22 . 1.433(15) ?
C22 C23 . 1.50(2) ?
C23 C24 . 1.526(14) ?
C31 C32 . 1.517(15) ?
C32 C33 . 1.51(2) ?
C33 C34 . 1.54(2) ?
C41 C42 . 1.421(15) ?
C42 C43 . 1.41(2) ?
C43 C44 . 1.473(14) ?
C51 C52 . 1.476(14) ?
C52 C53 . 1.431(15) ?
C54 C53 . 1.396(15) ?
