#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:34:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179452 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/49/4334927.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_4334927
loop_
_publ_author_name
'Kati Rosenstengel'
'Axel Schulz'
'Alexander Villinger'
_publ_contact_author_address
;
Universität Rostock
Institut für Chemie
Abteilung für Anorganische Chemie
Albert-Einstein-Strasse 3a 
18059 Rostock
Bundesrepublik Deutschland
;
_publ_contact_author_email
;
axel.schulz@uni-rostock.de, alexander.villinger@uni-rostock.de'
;
_publ_contact_author_fax         '+49 (0)381/498-6382'
_publ_contact_author_name        'Axel Schulz, Alexander Villinger'
_publ_contact_author_phone       '+49 (0)381/498-6400 or 6403'
_publ_section_title
;
 Solid State Structure of Bi(N3)3, Bi(N3)3.Solvates and the Structural
 Dynamics in the [Bi(N3)6]3- Anion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6110
_journal_page_last               6126
_journal_paper_doi               10.1021/ic400493v
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'Bi N9, C2 H6 O S'
_chemical_formula_sum            'C2 H6 Bi N9 O S'
_chemical_formula_weight         413.20
_chemical_name_systematic
;
bismuth azide DMSO adduct
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'Villinger, A.'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.732(2)
_cell_angle_beta                 103.349(2)
_cell_angle_gamma                104.602(2)
_cell_formula_units_Z            2
_cell_length_a                   6.3578(2)
_cell_length_b                   6.9425(2)
_cell_length_c                   11.5741(4)
_cell_measurement_reflns_used    8414
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      65.381
_cell_measurement_theta_min      6.195
_cell_volume                     470.83(3)
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_collection       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex Kappa-II-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19747
_diffrn_reflns_theta_full        34.99
_diffrn_reflns_theta_max         34.99
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    18.932
_exptl_absorpt_correction_T_max  0.3127
_exptl_absorpt_correction_T_min  0.1234
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.915
_exptl_crystal_description       block
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.798
_refine_diff_density_min         -1.194
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         4144
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0115P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0378
_refine_ls_wR_factor_ref         0.0393
_reflns_number_gt                3666
_reflns_number_total             4144
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic400493v_si_002_04.cif
_cod_data_source_block           kr08_Bi(N3)3_dmso_RT
_cod_original_cell_volume        470.82(3)
_cod_database_code               4334927
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.1225(5) 0.6544(6) 0.9038(3) 0.0402(8) Uani 1 1 d .
H1A H 0.1565 0.7831 0.9575 0.060 Uiso 1 1 calc R
H1B H 0.1366 0.5518 0.9506 0.060 Uiso 1 1 calc R
H1C H -0.0293 0.6189 0.8524 0.060 Uiso 1 1 calc R
C2 C 0.5729(5) 0.7591(5) 0.9300(3) 0.0332(7) Uani 1 1 d .
H2A H 0.6949 0.8100 0.8960 0.050 Uiso 1 1 calc R
H2B H 0.5981 0.6487 0.9676 0.050 Uiso 1 1 calc R
H2C H 0.5657 0.8658 0.9896 0.050 Uiso 1 1 calc R
N1 N -0.1284(4) 0.5666(4) 0.5723(3) 0.0344(6) Uani 1 1 d .
N2 N -0.2722(4) 0.6262(4) 0.6026(2) 0.0236(5) Uani 1 1 d .
N3 N -0.4079(4) 0.6851(4) 0.6341(2) 0.0336(6) Uani 1 1 d .
N4 N 0.5263(4) 1.1331(4) 0.6051(2) 0.0225(5) Uani 1 1 d .
N5 N 0.5568(4) 1.2317(3) 0.7051(2) 0.0209(5) Uani 1 1 d .
N6 N 0.5849(5) 1.3241(4) 0.7991(3) 0.0369(6) Uani 1 1 d .
N7 N 0.0224(4) 1.0634(4) 0.6160(2) 0.0218(5) Uani 1 1 d .
N8 N 0.0134(4) 1.0968(4) 0.7200(2) 0.0247(5) Uani 1 1 d .
N9 N 0.0025(5) 1.1257(6) 0.8172(3) 0.0473(8) Uani 1 1 d .
O1 O 0.3011(3) 0.8590(3) 0.75939(18) 0.0256(4) Uani 1 1 d .
S1 S 0.31410(12) 0.67159(11) 0.81315(6) 0.02233(14) Uani 1 1 d .
Bi1 Bi 0.218576(14) 0.827737(14) 0.545086(8) 0.01647(3) Uani 1 1 d .
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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 '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
S1 C1 H1A 109.5 . .
S1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
S1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
S1 C2 H2A 109.5 . .
S1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
S1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
N2 N1 Bi1 119.01(19) . .
N2 N1 Bi1 121.08(18) . 2_566
Bi1 N1 Bi1 116.32(9) . 2_566
N3 N2 N1 178.6(3) . .
N5 N4 Bi1 115.58(16) . .
N5 N4 Bi1 129.89(16) . 2_676
Bi1 N4 Bi1 113.83(9) . 2_676
N6 N5 N4 179.8(3) . .
N8 N7 Bi1 121.22(18) . 2_576
N8 N7 Bi1 122.52(19) . .
Bi1 N7 Bi1 115.14(9) 2_576 .
N9 N8 N7 179.0(4) . .
S1 O1 Bi1 119.03(11) . .
O1 S1 C1 104.07(15) . .
O1 S1 C2 103.60(14) . .
C1 S1 C2 99.20(16) . .
O1 Bi1 N4 81.00(7) . .
O1 Bi1 N7 138.39(7) . 2_576
N4 Bi1 N7 96.81(8) . 2_576
O1 Bi1 N7 73.81(7) . .
N4 Bi1 N7 81.16(8) . .
N7 Bi1 N7 64.86(9) 2_576 .
O1 Bi1 N1 76.77(8) . .
N4 Bi1 N1 154.49(8) . .
N7 Bi1 N1 91.64(9) 2_576 .
N7 Bi1 N1 80.76(8) . .
O1 Bi1 N4 133.09(7) . 2_676
N4 Bi1 N4 66.17(9) . 2_676
N7 Bi1 N4 80.35(7) 2_576 2_676
N7 Bi1 N4 128.65(8) . 2_676
N1 Bi1 N4 139.22(8) . 2_676
O1 Bi1 N1 111.79(8) . 2_566
N4 Bi1 N1 138.04(7) . 2_566
N7 Bi1 N1 97.52(9) 2_576 2_566
N7 Bi1 N1 140.27(8) . 2_566
N1 Bi1 N1 63.68(9) . 2_566
N4 Bi1 N1 77.73(7) 2_676 2_566
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 S1 1.775(3) .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 S1 1.776(3) .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
N1 N2 1.196(3) .
N1 Bi1 2.591(2) .
N1 Bi1 2.742(3) 2_566
N2 N3 1.152(3) .
N4 N5 1.209(3) .
N4 Bi1 2.385(2) .
N4 Bi1 2.633(2) 2_676
N5 N6 1.136(3) .
N7 N8 1.212(3) .
N7 Bi1 2.457(2) 2_576
N7 Bi1 2.459(2) .
N8 N9 1.137(3) .
O1 S1 1.528(2) .
O1 Bi1 2.3816(19) .
Bi1 N7 2.457(2) 2_576
Bi1 N4 2.633(2) 2_676
Bi1 N1 2.742(3) 2_566
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
Bi1 N1 N2 N3 -74(13) . .
Bi1 N1 N2 N3 128(12) 2_566 .
Bi1 N4 N5 N6 -11(100) . .
Bi1 N4 N5 N6 179(100) 2_676 .
Bi1 N7 N8 N9 85(20) 2_576 .
Bi1 N7 N8 N9 -82(20) . .
Bi1 O1 S1 C1 -125.88(15) . .
Bi1 O1 S1 C2 130.81(14) . .
S1 O1 Bi1 N4 -134.19(13) . .
S1 O1 Bi1 N7 135.68(12) . 2_576
S1 O1 Bi1 N7 142.47(14) . .
S1 O1 Bi1 N1 58.41(12) . .
S1 O1 Bi1 N4 -89.29(14) . 2_676
S1 O1 Bi1 N1 4.19(14) . 2_566
N5 N4 Bi1 O1 -25.7(2) . .
Bi1 N4 Bi1 O1 145.70(10) 2_676 .
N5 N4 Bi1 N7 112.3(2) . 2_576
Bi1 N4 Bi1 N7 -76.28(10) 2_676 2_576
N5 N4 Bi1 N7 49.2(2) . .
Bi1 N4 Bi1 N7 -139.43(11) 2_676 .
N5 N4 Bi1 N1 3.9(3) . .
Bi1 N4 Bi1 N1 175.25(16) 2_676 .
N5 N4 Bi1 N4 -171.4(3) . 2_676
Bi1 N4 Bi1 N4 0.0 2_676 2_676
N5 N4 Bi1 N1 -138.39(19) . 2_566
Bi1 N4 Bi1 N1 32.99(17) 2_676 2_566
N8 N7 Bi1 O1 -7.0(2) . .
Bi1 N7 Bi1 O1 -175.02(12) 2_576 .
N8 N7 Bi1 N4 -90.2(2) . .
Bi1 N7 Bi1 N4 101.85(11) 2_576 .
N8 N7 Bi1 N7 168.0(3) . 2_576
Bi1 N7 Bi1 N7 0.0 2_576 2_576
N8 N7 Bi1 N1 71.8(2) . .
Bi1 N7 Bi1 N1 -96.22(11) 2_576 .
N8 N7 Bi1 N4 -139.8(2) . 2_676
Bi1 N7 Bi1 N4 52.24(13) 2_576 2_676
N8 N7 Bi1 N1 97.8(2) . 2_566
Bi1 N7 Bi1 N1 -70.22(16) 2_576 2_566
N2 N1 Bi1 O1 78.3(2) . .
Bi1 N1 Bi1 O1 -122.81(13) 2_566 .
N2 N1 Bi1 N4 48.3(4) . .
Bi1 N1 Bi1 N4 -152.84(15) 2_566 .
N2 N1 Bi1 N7 -61.3(2) . 2_576
Bi1 N1 Bi1 N7 97.58(12) 2_566 2_576
N2 N1 Bi1 N7 2.9(2) . .
Bi1 N1 Bi1 N7 161.78(13) 2_566 .
N2 N1 Bi1 N4 -138.4(2) . 2_676
Bi1 N1 Bi1 N4 20.5(2) 2_566 2_676
N2 N1 Bi1 N1 -158.9(3) . 2_566
Bi1 N1 Bi1 N1 0.0 2_566 2_566
