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_4328046
_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         'C10 H8 As N11'
_chemical_formula_sum            'C10 H8 As N11'
_chemical_formula_weight         357.19
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2011-09-06 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 108.6600(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.1835(7)
_cell_length_b                   18.7740(17)
_cell_length_c                   10.6709(10)
_cell_measurement_reflns_used    9881
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.4237
_cell_measurement_theta_min      2.2880
_cell_volume                     1363.5(2)
_computing_cell_refinement       'APEX2 v2010.11-3 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v2011.4.0.0'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18248
_diffrn_reflns_theta_full        28.42
_diffrn_reflns_theta_max         28.42
_diffrn_reflns_theta_min         2.17
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.510
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS V2008/1'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_description       prism
_exptl_crystal_F_000             712
_exptl_crystal_recrystallization_method CH3CN
_exptl_crystal_size_max          0.511
_exptl_crystal_size_mid          0.470
_exptl_crystal_size_min          0.405
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3416
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0222
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0185P)^2^+0.7808P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0510
_refine_ls_wR_factor_ref         0.0522
_reflns_number_gt                3086
_reflns_number_total             3416
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202307a_si_002_1.cif
_cod_data_source_block           C10H8AsN11
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4328046