Binary Group 15 Polyazides. Structural Characterization of [Bi(N3)4]-, [Bi(N3)5]2-, [bipy.Bi(N3)5]2-, [Bi(N3)6]3-, bipy.As(N3)3, bipy.Sb(N3)3, and [(bipy)2.Bi(N3)3]2and on the Lone Pair Activation of Valence Electrons
Ralf Haiges; Martin Rahm; David A. Dixon; Edward B. Garner; Karl O. Christe; Inorganic Chemistry 51 (2012) 1127–1141; doi:10.1021/ic202307a

data_4328049
_publ_contact_author_address
;Loker Research Institute and Department of Chemistry
University of Southern California
Los Angeles, CA 90089-1661
USA
;
_publ_contact_author_email       haiges@usc.edu
_publ_contact_author_name        'Ralf Haiges'
_publ_section_title
;
 Binary Group 15 Polyazides. Structural Characterization of [Bi(N3)4]-,
 [Bi(N3)5]2-, [bipy.Bi(N3)5]2-, [Bi(N3)6]3-, bipy.As(N3)3, bipy.Sb(N3)3,
 and [(bipy)2.Bi(N3)3]2and on the Lone Pair Activation of Valence
 Electrons
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1127
_journal_page_last               1141
_journal_paper_doi               10.1021/ic202307a
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C40 H32 Bi2 N26'
_chemical_formula_sum            'C40 H32 Bi2 N26'
_chemical_formula_weight         1294.88
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.6040(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.9891(5)
_cell_length_b                   22.1991(12)
_cell_length_c                   10.9374(6)
_cell_measurement_reflns_used    5892
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.51
_cell_volume                     2121.3(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12973
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    8.352
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS V2.10'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.027
_exptl_crystal_description       prism
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.073
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         4785
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0264P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0630
_reflns_number_gt                4118
_reflns_number_total             4785
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202307a_si_002_4.cif
_cod_data_source_block           C40H32Bi2N26
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4328049