#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/92/7009298.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_7009298
loop_
_publ_author_name
'Barton, Andrew J.'
'Genge, Anthony R. J.'
'Levason, William'
'Reid, Gillian'
_publ_section_title
;
 Synthesis and structures of bismuth(III) complexes involving thio- and
 seleno-ether ligands
;
_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              859
_journal_paper_doi               10.1039/a909803h
_journal_year                    2000
_chemical_compound_source        'recrystallisation from MeCN'
_chemical_formula_moiety         'C8 H18 Bi I3 Se3 '
_chemical_formula_structural     '[Bi2I6{MeC(CH2SeMe)3}2]'
_chemical_formula_sum            'C8 H18 Bi I3 Se3'
_chemical_formula_weight         940.80
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             19100-01-25
_audit_creation_method           'by teXsan v1.8'
_cell_angle_alpha                90
_cell_angle_beta                 97.93(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.59(1)
_cell_length_b                   8.717(4)
_cell_length_c                   21.40(1)
_cell_measurement_reflns_used    14
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      11.7
_cell_measurement_theta_min      7.1
_cell_volume                     1957(2)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution
;
DIRDIF92 PATTY (Beurskens, 1992)
;
_diffrn_ambient_temperature      150.0(1)
_diffrn_measurement_device_type  'Rigaku AFC7S'
_diffrn_measurement_method       ω-2θ
_diffrn_orient_matrix_UB_11      -0.06456
_diffrn_orient_matrix_UB_12      0.08319
_diffrn_orient_matrix_UB_13      0.00188
_diffrn_orient_matrix_UB_21      -0.06138
_diffrn_orient_matrix_UB_22      -0.05661
_diffrn_orient_matrix_UB_23      -0.03152
_diffrn_orient_matrix_UB_31      -0.03401
_diffrn_orient_matrix_UB_32      -0.05508
_diffrn_orient_matrix_UB_33      0.03507
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.12563
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            3029
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        -1.00
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    19.295
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.352
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
DIFABS (Walker & Stuart, 1983)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.194
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1640.00
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.20
_refine_diff_density_min         -2.33
_refine_ls_abs_structure_details -
_refine_ls_abs_structure_Flack   -
_refine_ls_extinction_coef       -
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.471
_refine_ls_goodness_of_fit_ref   2.471
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     96
_refine_ls_number_reflns         700
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0838
_refine_ls_shift/su_max          0.0238
_refine_ls_shift/su_mean         0.0049
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(Fo) + 0.00000|Fo|²]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0742
_refine_ls_wR_factor_ref         0.0742
_reflns_number_gt                700
_reflns_number_total             2961
_reflns_threshold_expression     I>2.00σ(I)
_cod_data_source_file            a909803h.txt
_cod_data_source_block           bii3se3_BiI3_+_MeC(CH2SeMe)3
_cod_original_cell_volume        1956(2)
_cod_original_sg_symbol_H-M      'P 21/c     '
_cod_original_formula_sum        'C8 H18 Bi I3 Se3 '
_cod_database_code               7009298
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_occupancy
_atom_site_refinement_flags
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
Bi(1) 0.0587(4) 0.5244(4) 0.1006(2) 0.022(1) 1.000 . Uani d ?
I(1) 0.2003(8) 0.3408(7) 0.2011(3) 0.034(3) 1.000 . Uani d ?
I(2) 0.0394(8) 0.2356(6) 0.0125(3) 0.039(3) 1.000 . Uani d ?
I(3) -0.1878(8) 0.5184(8) 0.1469(3) 0.046(3) 1.000 . Uani d ?
Se(1) 0.132(1) 0.797(1) 0.1802(4) 0.028(4) 1.000 . Uani d ?
Se(2) 0.324(1) 0.606(1) 0.0538(5) 0.040(4) 1.000 . Uani d ?
Se(3) 0.624(1) 0.925(1) 0.0892(6) 0.062(5) 1.000 . Uani d ?
C(1) 0.42(1) 0.91(1) 0.205(4) 0.05(3) 1.000 . Uiso d ?
C(2) 0.381(9) 0.864(8) 0.136(4) 0.01(2) 1.000 . Uiso d ?
C(3) 0.22(1) 0.90(1) 0.121(4) 0.05(3) 1.000 . Uiso d ?
C(4) 0.412(9) 0.694(9) 0.130(4) 0.03(3) 1.000 . Uiso d ?
C(5) 0.44(1) 0.966(9) 0.088(4) 0.03(3) 1.000 . Uiso d ?
C(6) 0.00(1) 0.93(1) 0.158(4) 0.05(3) 1.000 . Uiso d ?
C(7) 0.43(1) 0.40(1) 0.065(5) 0.09(4) 1.000 . Uiso d ?
C(8) 0.69(1) 1.13(1) 0.128(6) 0.11(5) 1.000 . Uiso d ?
H(1) 0.3852 0.8474 0.2331 0.046 1.000 . Uiso c ?
H(2) 0.5168 0.8932 0.2149 0.046 1.000 . Uiso c ?
H(3) 0.4094 1.0149 0.2136 0.046 1.000 . Uiso c ?
H(4) 0.1890 0.8767 0.0768 0.031 1.000 . Uiso c ?
H(5) 0.2066 1.0164 0.1221 0.031 1.000 . Uiso c ?
H(6) 0.3934 0.6358 0.1646 0.026 1.000 . Uiso c ?
H(7) 0.5044 0.6807 0.1280 0.026 1.000 . Uiso c ?
H(8) 0.4125 1.0779 0.0962 0.038 1.000 . Uiso c ?
H(9) 0.3814 0.9514 0.0453 0.038 1.000 . Uiso c ?
H(10) 0.0222 1.0312 0.1638 0.031 1.000 . Uiso c ?
H(11) -0.0311 0.9160 0.1114 0.031 1.000 . Uiso c ?
H(12) -0.0722 0.9044 0.1781 0.031 1.000 . Uiso c ?
H(13) 0.4160 0.3465 0.1086 0.077 1.000 . Uiso c ?
H(14) 0.4024 0.3195 0.0363 0.077 1.000 . Uiso c ?
H(15) 0.5189 0.4085 0.0702 0.077 1.000 . Uiso c ?
H(16) 0.7854 1.1237 0.1325 0.084 1.000 . Uiso c ?
H(17) 0.6642 1.2088 0.1010 0.084 1.000 . Uiso c ?
H(18) 0.6679 1.1399 0.1681 0.084 1.000 . Uiso c ?
loop_
_atom_type_symbol
_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 32 0.002 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H 0 72 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
Se 0 12 -0.178 2.223
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
I 0 12 -0.726 1.812
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Bi 0 4 -4.861 10.559
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-2 0 12
-3 0 6
-2 1 11
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I(1) Bi(1) I(2) 89.3(2) . . . yes
I(1) Bi(1) I(2) 167.5(3) . . 3_565 yes
I(1) Bi(1) I(3) 97.5(2) . . . yes
I(1) Bi(1) Se(1) 87.0(2) . . . yes
I(1) Bi(1) Se(2) 88.3(3) . . . yes
I(2) Bi(1) I(2) 94.6(2) . . 3_565 yes
I(2) Bi(1) I(3) 101.6(3) . . . yes
I(2) Bi(1) Se(1) 168.3(3) . . . yes
I(2) Bi(1) Se(2) 88.7(3) . . . yes
I(2) Bi(1) I(3) 93.3(3) 3_565 . . yes
I(2) Bi(1) Se(1) 86.8(2) 3_565 . . yes
I(2) Bi(1) Se(2) 80.0(3) 3_565 . . yes
I(3) Bi(1) Se(1) 89.9(3) . . . yes
I(3) Bi(1) Se(2) 168.2(3) . . . yes
Se(1) Bi(1) Se(2) 80.1(3) . . . yes
Bi(1) I(2) Bi(1) 85.4(2) . . 3_565 yes
Bi(1) Se(1) C(3) 97(3) . . . yes
Bi(1) Se(1) C(6) 103(3) . . . yes
C(3) Se(1) C(6) 88(4) . . . yes
Bi(1) Se(2) C(4) 100(3) . . . yes
Bi(1) Se(2) C(7) 103(3) . . . yes
C(4) Se(2) C(7) 94(4) . . . yes
C(5) Se(3) C(8) 97(4) . . . yes
C(2) C(1) H(1) 112.5 . . . no
C(2) C(1) H(2) 109.4 . . . no
C(2) C(1) H(3) 111.8 . . . no
H(1) C(1) H(2) 108.8 . . . no
H(1) C(1) H(3) 108.6 . . . no
H(2) C(1) H(3) 105.4 . . . no
C(1) C(2) C(3) 107(7) . . . yes
C(1) C(2) C(4) 106(7) . . . yes
C(1) C(2) C(5) 115(7) . . . yes
C(3) C(2) C(4) 113(7) . . . yes
C(3) C(2) C(5) 103(7) . . . yes
C(4) C(2) C(5) 113(7) . . . yes
Se(1) C(3) C(2) 111(6) . . . yes
Se(1) C(3) H(4) 111.5 . . . no
Se(1) C(3) H(5) 110.6 . . . no
C(2) C(3) H(4) 111.1 . . . no
C(2) C(3) H(5) 111.1 . . . no
H(4) C(3) H(5) 101.0 . . . no
Se(2) C(4) C(2) 112(6) . . . yes
Se(2) C(4) H(6) 108.8 . . . no
Se(2) C(4) H(7) 106.7 . . . no
C(2) C(4) H(6) 112.8 . . . no
C(2) C(4) H(7) 109.6 . . . no
H(6) C(4) H(7) 106.7 . . . no
Se(3) C(5) C(2) 111(6) . . . yes
Se(3) C(5) H(8) 116.4 . . . no
Se(3) C(5) H(9) 116.8 . . . no
C(2) C(5) H(8) 106.8 . . . no
C(2) C(5) H(9) 106.5 . . . no
H(8) C(5) H(9) 98.0 . . . no
Se(1) C(6) H(10) 114.8 . . . no
Se(1) C(6) H(11) 109.7 . . . no
Se(1) C(6) H(12) 112.7 . . . no
H(10) C(6) H(11) 105.5 . . . no
H(10) C(6) H(12) 110.1 . . . no
H(11) C(6) H(12) 103.2 . . . no
Se(2) C(7) H(13) 110.1 . . . no
Se(2) C(7) H(14) 117.8 . . . no
Se(2) C(7) H(15) 114.4 . . . no
H(13) C(7) H(14) 103.4 . . . no
H(13) C(7) H(15) 99.3 . . . no
H(14) C(7) H(15) 109.6 . . . no
Se(3) C(8) H(16) 108.1 . . . no
Se(3) C(8) H(17) 112.1 . . . no
Se(3) C(8) H(18) 113.4 . . . no
H(16) C(8) H(17) 104.2 . . . no
H(16) C(8) H(18) 105.8 . . . no
H(17) C(8) H(18) 112.5 . . . no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Bi(1) I(1) 2.923(7) . . yes
Bi(1) I(2) 3.133(7) . . yes
Bi(1) I(2) 3.260(7) . 3_565 yes
Bi(1) I(3) 2.917(9) . . yes
Bi(1) Se(1) 2.96(1) . . yes
Bi(1) Se(2) 3.19(1) . . yes
Se(1) C(3) 1.93(9) . . yes
Se(1) C(6) 1.8(1) . . yes
Se(2) C(4) 1.92(9) . . yes
Se(2) C(7) 2.1(1) . . yes
Se(3) C(5) 2.0(1) . . yes
Se(3) C(8) 2.0(1) . . yes
C(1) C(2) 1.5(1) . . yes
C(1) H(1) 0.93 . . no
C(1) H(2) 0.97 . . no
C(1) H(3) 0.98 . . no
C(2) C(3) 1.7(1) . . yes
C(2) C(4) 1.53(9) . . yes
C(2) C(5) 1.5(1) . . yes
C(3) H(4) 1.00 . . no
C(3) H(5) 1.01 . . no
C(4) H(6) 0.94 . . no
C(4) H(7) 0.99 . . no
C(5) H(8) 1.03 . . no
C(5) H(9) 1.02 . . no
C(6) H(10) 0.93 . . no
C(6) H(11) 1.02 . . no
C(6) H(12) 0.96 . . no
C(7) H(13) 1.06 . . no
C(7) H(14) 0.92 . . no
C(7) H(15) 0.98 . . no
C(8) H(16) 1.02 . . no
C(8) H(17) 0.94 . . no
C(8) H(18) 0.92 . . no
