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_4334930
_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 Cl0.12 N17.64 3-, 3(C24 H20 P +)'
_chemical_formula_sum            'C72 H60 Bi Cl0.12 N17.64 P3'
_chemical_formula_weight         1478.60
_chemical_name_systematic
;
tris(tetraphenylphosphonium) hexaazidobismuthate/ pentaazido(chloro)bismuthate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                90.00
_cell_angle_beta                 97.025(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2880(5)
_cell_length_b                   22.6627(9)
_cell_length_c                   22.0071(9)
_cell_measurement_reflns_used    9089
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      55.135
_cell_measurement_theta_min      4.739
_cell_volume                     6577.5(5)
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            110034
_diffrn_reflns_theta_full        30.10
_diffrn_reflns_theta_max         30.10
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    2.817
_exptl_absorpt_correction_T_max  0.5279
_exptl_absorpt_correction_T_min  0.3390
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       block
_exptl_crystal_F_000             2982
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.990
_refine_diff_density_min         -2.198
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     902
_refine_ls_number_reflns         19085
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0147P)^2^+7.7386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0579
_refine_ls_wR_factor_ref         0.0665
_reflns_number_gt                13931
_reflns_number_total             19085
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic400493v_si_002_07.cif
_cod_data_source_block           av494c_Ph4P_Bi(N3)6_Cl/N3
_cod_original_cell_volume        6577.5(4)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4334930