Solid State Structure of Bi(N3)3, Bi(N3)3.Solvates and the Structural Dynamics in the [Bi(N3)6]3- Anion
Kati Rosenstengel; Axel Schulz; Alexander Villinger; Inorganic Chemistry 52 (2013) 6110–6126; doi:10.1021/ic400493v

data_4334927
_publ_contact_author_address
;
Universit\"at Rostock
Institut f\"ur Chemie
Abteilung f\"ur 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/[\s^2^(Fo^2^)+(0.0115P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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     >2\s(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