#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:33:36 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179976 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/70/7027092.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_7027092
loop_
_publ_author_name
'Hodge, Philip'
'James, Siân C.'
'Norman, Nicholas C.'
'Orpen, A. Guy'
_publ_section_title
;
 Neutral and anionic aryloxy halides of bismuth(III)
;
_journal_issue                   23
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4049
_journal_paper_doi               10.1039/a806647g
_journal_year                    1998
_chemical_formula_structural     '[Bi2 Cl4 (thf)2 (O -2,4,6-Me3 C6 H2)2]'
_chemical_formula_sum            'C13 H19 Bi Cl2 O2'
_chemical_formula_weight         487.16
_chemical_name_systematic
; 
 Tetrachloro bis-2,4,6-trimethylphenoxy bis tetrahydrofuran dibismuthate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 95.58(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.769(3)
_cell_length_b                   13.743(3)
_cell_length_c                   14.405(3)
_cell_measurement_reflns_used    235
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.550
_cell_measurement_theta_min      14.450
_cell_volume                     3107.0(11)
_computing_cell_refinement       'SAINT (Siemens, 1995b)'
_computing_data_collection       'SMART (Siemens, 1995b)'
_computing_data_reduction        'SAINT (Siemens, 1995b)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1995a)'
_computing_publication_material  'SHELXTL (Siemens, 1995a)'
_computing_structure_refinement  'SHELXTL (Siemens, 1995a)'
_computing_structure_solution    'SHELXTL (Siemens, 1995a)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens SMART Area Detector'
_diffrn_measurement_method       'ω rotation with narrow frames'
_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  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9560
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    11.685
_exptl_absorpt_correction_T_max  0.491504
_exptl_absorpt_correction_T_min  0.293096
_exptl_absorpt_correction_type   Sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.083
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.370
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       0.00018(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.035
_refine_ls_goodness_of_fit_obs   1.086
_refine_ls_hydrogen_treatment    'see text'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         3549
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_restrained_S_obs      1.086
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_obs          0.0241
_refine_ls_shift/esd_max         -0.008
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0201P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0496
_refine_ls_wR_factor_obs         0.0466
_reflns_number_observed          2874
_reflns_number_total             3549
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            806647Gsup1.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0201P)^2^+0.0000P] 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^)+(0.0201P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7027092
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Bi1 Bi 0.039840(9) 0.605366(13) 0.125886(10) 0.02268(6) Uani 1 d .
Cl1 Cl 0.05564(7) 0.78319(9) 0.12736(8) 0.0369(3) Uani 1 d .
Cl2 Cl -0.05004(7) 0.61559(10) -0.03244(8) 0.0369(3) Uani 1 d .
O1 O -0.0741(2) 0.6075(2) 0.2012(2) 0.0240(6) Uani 1 d .
O2 O 0.2002(2) 0.6155(3) 0.0796(3) 0.0496(10) Uani 1 d .
C1 C -0.1595(2) 0.5948(3) 0.1711(3) 0.0222(9) Uani 1 d .
C2 C -0.1940(3) 0.5019(4) 0.1783(3) 0.0276(10) Uani 1 d .
C3 C -0.2824(3) 0.4916(4) 0.1589(3) 0.0355(12) Uani 1 d .
H3A H -0.3072(3) 0.4291(4) 0.1644(3) 0.043 Uiso 1 calc R
C4 C -0.3351(3) 0.5697(4) 0.1319(3) 0.0374(13) Uani 1 d .
C5 C -0.2977(3) 0.6589(4) 0.1211(3) 0.0332(12) Uani 1 d .
H5A H -0.3328(3) 0.7120(4) 0.0994(3) 0.040 Uiso 1 calc R
C6 C -0.2100(3) 0.6750(4) 0.1407(3) 0.0280(10) Uani 1 d .
C7 C -0.1728(3) 0.7738(4) 0.1302(3) 0.0349(12) Uani 1 d .
H7A H -0.1110(3) 0.7713(4) 0.1468(3) 0.052 Uiso 1 calc R
H7B H -0.1984(3) 0.8196(4) 0.1716(3) 0.052 Uiso 1 calc R
H7C H -0.1844(3) 0.7955(4) 0.0654(3) 0.052 Uiso 1 calc R
C8 C -0.4313(3) 0.5571(5) 0.1151(4) 0.052(2) Uani 1 d .
H8A H -0.4462(3) 0.4891(5) 0.1261(4) 0.077 Uiso 1 calc R
H8B H -0.4506(3) 0.5749(5) 0.0506(4) 0.077 Uiso 1 calc R
H8C H -0.4592(3) 0.5992(5) 0.1579(4) 0.077 Uiso 1 calc R
C9 C -0.1392(3) 0.4153(3) 0.2047(3) 0.0374(12) Uani 1 d .
H9A H -0.1751(3) 0.3571(3) 0.2061(3) 0.056 Uiso 1 calc R
H9B H -0.1088(3) 0.4257(3) 0.2665(3) 0.056 Uiso 1 calc R
H9C H -0.0980(3) 0.4063(3) 0.1588(3) 0.056 Uiso 1 calc R
C10 C 0.2442(3) 0.5237(5) 0.0814(4) 0.0471(15) Uani 1 d .
H10A H 0.2319(3) 0.4897(5) 0.0210(4) 0.057 Uiso 1 calc R
H10B H 0.2254(3) 0.4817(5) 0.1314(4) 0.057 Uiso 1 calc R
C11 C 0.3388(3) 0.5446(6) 0.0995(5) 0.076(2) Uani 1 d .
H11A H 0.3625(3) 0.5153(6) 0.1592(5) 0.091 Uiso 1 calc R
H11B H 0.3699(3) 0.5182(6) 0.0486(5) 0.091 Uiso 1 calc R
C12 C 0.3454(3) 0.6505(5) 0.1031(5) 0.068(2) Uani 1 d .
H12A H 0.3652(3) 0.6758(5) 0.0446(5) 0.082 Uiso 1 calc R
H12B H 0.3866(3) 0.6708(5) 0.1559(5) 0.082 Uiso 1 calc R
C13 C 0.2583(3) 0.6892(5) 0.1158(4) 0.0443(14) Uani 1 d .
H13A H 0.2522(3) 0.7011(5) 0.1826(4) 0.053 Uiso 1 calc R
H13B H 0.2477(3) 0.7509(5) 0.0810(4) 0.053 Uiso 1 calc R
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'
Bi Bi -4.1077 10.2566 '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
O1 Bi1 Cl1 93.99(9) . .
O1 Bi1 O1 67.25(11) . 2
Cl1 Bi1 O1 88.14(8) . 2
O1 Bi1 Cl2 91.77(8) . .
Cl1 Bi1 Cl2 90.00(4) . .
O1 Bi1 Cl2 158.73(7) 2 .
O1 Bi1 O2 164.30(11) . .
Cl1 Bi1 O2 81.55(9) . .
O1 Bi1 O2 97.45(10) 2 .
Cl2 Bi1 O2 103.22(9) . .
O1 Bi1 Cl2 106.69(8) . 5_565
Cl1 Bi1 Cl2 154.34(4) . 5_565
O1 Bi1 Cl2 113.56(7) 2 5_565
Cl2 Bi1 Cl2 74.65(4) . 5_565
O2 Bi1 Cl2 82.14(9) . 5_565
C1 O1 Bi1 131.6(2) . .
C1 O1 Bi1 114.8(2) . 2
Bi1 O1 Bi1 112.73(11) . 2
C13 O2 C10 108.9(4) . .
C13 O2 Bi1 122.2(3) . .
C10 O2 Bi1 114.5(3) . .
O1 C1 C2 117.8(4) . .
O1 C1 C6 120.2(4) . .
C2 C1 C6 121.9(4) . .
C1 C2 C3 117.7(4) . .
C1 C2 C9 121.8(4) . .
C3 C2 C9 120.5(4) . .
C4 C3 C2 122.2(5) . .
C5 C4 C3 118.0(4) . .
C5 C4 C8 121.0(5) . .
C3 C4 C8 121.0(5) . .
C4 C5 C6 122.9(5) . .
C5 C6 C1 117.2(5) . .
C5 C6 C7 120.8(4) . .
C1 C6 C7 121.9(4) . .
O2 C10 C11 107.6(5) . .
C12 C11 C10 105.1(5) . .
C11 C12 C13 107.1(5) . .
O2 C13 C12 105.5(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Bi1 O1 2.187(3) .
Bi1 Cl1 2.4563(13) .
Bi1 O1 2.497(3) 2
Bi1 Cl2 2.5695(13) .
Bi1 O2 2.680(3) .
Bi1 Cl2 3.3317(14) 5_565
O1 C1 1.386(4) .
O1 Bi1 2.497(3) 2
O2 C13 1.429(6) .
O2 C10 1.439(6) .
C1 C2 1.396(6) .
C1 C6 1.404(6) .
C2 C3 1.402(6) .
C2 C9 1.497(6) .
C3 C4 1.390(7) .
C4 C5 1.375(7) .
C4 C8 1.524(6) .
C5 C6 1.402(6) .
C6 C7 1.494(7) .
C10 C11 1.516(7) .
C11 C12 1.460(9) .
C12 C13 1.501(7) .
