# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2011

data_global
_journal_name_full               Chem.Commun.
_journal_coden_cambridge         0182
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
loop_
_publ_author_name
_publ_author_address
S.Schulz
;
Fachbereich Chemie der
Universit\"at Duisburg-Essen
Campus Essen Universit\"atsstr. 7
D-45117 Essen, Germany
;
B.Lyhs
;
Fachbereich Chemie der
Universit\"at Duisburg-Essen
Campus Essen Universit\"atsstr. 7
D-45117 Essen, Germany
;
G.Janssen
;
Fachbereich Chemie der
Universit\"at Duisburg-Essen
Campus Essen Universit\"atsstr. 7
D-45117 Essen, Germany
;
D.Blaser
;
Fachbereich Chemie der
Universit\"at Duisburg-Essen
Campus Essen Universit\"atsstr. 7
D-45117 Essen, Germany
;
C.Wolper
;
Fachbereich Chemie der
Universit\"at Duisburg-Essen
Campus Essen Universit\"atsstr. 7
D-45117 Essen, Germany
;
#TrackingRef '- structures.cif'

_publ_contact_author             
;
Prof. Dr. Schulz, Stephan
Fachbereich Chemie der
Universit\"at Duisburg-Essen
Campus Essen, Universit\"atsstr. 7
D-45141 Essen, Germany
;
_publ_contact_author_email       stephan.schulz@.uni-due.de
_publ_contact_author_fax         '++49 (0)201 183 3830'
_publ_contact_author_phone       '++49 (0)201 183 4635'
_publ_contact_letter             
;
?
;

_publ_requested_coeditor_name    ?

_publ_section_title              
;
Syntheses and Structures of Triazides
of Heavy Group 15 Elements
;
_publ_contact_author_name        'Prof. Dr. Schulz, Stephan'

#=============================================================================
# compound 3
#=============================================================================

data_ben_bin33no3
_database_code_depnum_ccdc_archive 'CCDC 803386'

_ccdc_compound_id                ?

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H10 Bi N11'
_chemical_formula_weight         493.27

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'
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'C m c 21'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   21.7967(16)
_cell_length_b                   10.8375(8)
_cell_length_c                   6.2825(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1484.06(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9892
_cell_measurement_theta_min      3.4
_cell_measurement_theta_max      30.7

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.208
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             920
_exptl_absorpt_coefficient_mu    11.896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5245
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   
;
BRUKER AXS SMART APEX 2 Vers. 3.0-2009
R.H. Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'Triumph graphite'
_diffrn_measurement_device_type  
;
Bruker D8 KAPPA series II with APEX II area detector system
;
_diffrn_measurement_method       
;
Data collection strategy APEX 2/COSMO
;
_diffrn_detector_area_resol_mean 512
_diffrn_reflns_number            31065
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0191
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         30.55
_reflns_number_total             2319
_reflns_number_gt                2234
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_cell_refinement       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_data_reduction        'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_structure_solution    'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_structure_refinement  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_molecular_graphics    'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0121P)^2^+0.5372P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.001(6)
_refine_ls_number_reflns         2319
_refine_ls_number_parameters     106
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0138
_refine_ls_R_factor_gt           0.0126
_refine_ls_wR_factor_ref         0.0287
_refine_ls_wR_factor_gt          0.0284
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_restrained_S_all      1.114
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Bi1 Bi 0.5000 0.870448(8) 0.87697(6) 0.01064(3) Uani 1 2 d S . .
N1 N 0.5000 0.7507(3) 1.1747(5) 0.0186(6) Uani 1 2 d S . .
N2 N 0.5000 0.6405(3) 1.1396(6) 0.0269(8) Uani 1 2 d S . .
N3 N 0.5000 0.5365(4) 1.1149(8) 0.079(2) Uani 1 2 d S . .
N4 N 0.43495(9) 0.9933(2) 1.0736(3) 0.0151(4) Uani 1 1 d . . .
N5 N 0.38534(9) 1.02106(18) 1.0004(3) 0.0134(4) Uani 1 1 d . . .
N6 N 0.33765(10) 1.0494(2) 0.9404(3) 0.0226(5) Uani 1 1 d . . .
N7 N 0.39967(10) 0.74430(19) 0.8050(3) 0.0164(4) Uani 1 1 d . . .
C1 C 0.35158(12) 0.7347(2) 0.9372(4) 0.0191(5) Uani 1 1 d . . .
H1 H 0.3543 0.7720 1.0737 0.023 Uiso 1 1 calc R . .
C2 C 0.29817(10) 0.67274(19) 0.8832(9) 0.0216(4) Uani 1 1 d . . .
H2 H 0.2648 0.6681 0.9803 0.026 Uiso 1 1 calc R . .
C3 C 0.29453(14) 0.6177(2) 0.6843(5) 0.0236(6) Uani 1 1 d . . .
H3 H 0.2587 0.5741 0.6427 0.028 Uiso 1 1 calc R . .
C4 C 0.34389(16) 0.6274(2) 0.5477(5) 0.0265(6) Uani 1 1 d . . .
H4 H 0.3426 0.5908 0.4104 0.032 Uiso 1 1 calc R . .
C5 C 0.39528(14) 0.6916(2) 0.6149(4) 0.0218(5) Uani 1 1 d . . .
H5 H 0.4291 0.6983 0.5202 0.026 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Bi1 0.00867(4) 0.01337(4) 0.00986(5) -0.00038(12) 0.000 0.000
N1 0.0211(16) 0.0213(14) 0.0134(14) 0.0038(11) 0.000 0.000
N2 0.040(2) 0.0243(17) 0.0165(17) 0.0054(12) 0.000 0.000
N3 0.177(7) 0.022(2) 0.038(3) 0.011(2) 0.000 0.000
N4 0.0100(9) 0.0223(9) 0.0130(11) -0.0025(10) 0.0007(7) 0.0014(8)
N5 0.0114(9) 0.0169(9) 0.0118(9) -0.0026(7) 0.0017(8) 0.0011(7)
N6 0.0144(10) 0.0317(11) 0.0217(13) -0.0037(8) -0.0024(8) 0.0058(9)
N7 0.0147(10) 0.0185(9) 0.0160(9) 0.0000(7) -0.0004(8) -0.0040(7)
C1 0.0196(12) 0.0175(10) 0.0201(14) 0.0002(8) -0.0001(9) -0.0022(9)
C2 0.0149(9) 0.0179(8) 0.0322(13) 0.002(2) 0.004(2) -0.0025(7)
C3 0.0198(13) 0.0180(12) 0.0331(16) 0.0031(11) -0.0089(12) -0.0053(10)
C4 0.0348(17) 0.0254(13) 0.0193(14) -0.0009(10) -0.0058(12) -0.0104(11)
C5 0.0235(14) 0.0236(12) 0.0184(13) -0.0002(10) 0.0024(11) -0.0077(11)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Bi1 N1 2.277(3) . ?
Bi1 N4 2.304(2) 4_655 ?
Bi1 N4 2.304(2) . ?
Bi1 N7 2.618(2) . ?
Bi1 N7 2.618(2) 4_655 ?
Bi1 N4 2.797(2) 3_574 ?
Bi1 N4 2.797(2) 2_674 ?
N1 N2 1.214(4) . ?
N2 N3 1.138(5) . ?
N4 N5 1.213(3) . ?
N4 Bi1 2.797(2) 2_675 ?
N5 N6 1.148(3) . ?
N7 C5 1.327(3) . ?
N7 C1 1.341(3) . ?
C1 C2 1.386(3) . ?
C2 C3 1.387(6) . ?
C3 C4 1.380(5) . ?
C4 C5 1.385(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
_geom_angle_publ_flag
N1 Bi1 N4 83.62(9) . 4_655 ?
N1 Bi1 N4 83.62(9) . . ?
N4 Bi1 N4 75.96(10) 4_655 . ?
N1 Bi1 N7 81.04(6) . . ?
N4 Bi1 N7 155.27(7) 4_655 . ?
N4 Bi1 N7 83.13(7) . . ?
N1 Bi1 N7 81.04(6) . 4_655 ?
N4 Bi1 N7 83.13(7) 4_655 4_655 ?
N4 Bi1 N7 155.27(7) . 4_655 ?
N7 Bi1 N7 113.27(9) . 4_655 ?
N1 Bi1 N4 149.40(4) . 3_574 ?
N4 Bi1 N4 111.86(4) 4_655 3_574 ?
N4 Bi1 N4 75.42(4) . 3_574 ?
N7 Bi1 N4 74.61(6) . 3_574 ?
N7 Bi1 N4 125.54(7) 4_655 3_574 ?
N1 Bi1 N4 149.40(4) . 2_674 ?
N4 Bi1 N4 75.42(4) 4_655 2_674 ?
N4 Bi1 N4 111.86(4) . 2_674 ?
N7 Bi1 N4 125.54(7) . 2_674 ?
N7 Bi1 N4 74.61(6) 4_655 2_674 ?
N4 Bi1 N4 60.92(8) 3_574 2_674 ?
N2 N1 Bi1 114.3(3) . . ?
N3 N2 N1 177.4(5) . . ?
N5 N4 Bi1 119.25(15) . . ?
N5 N4 Bi1 125.40(16) . 2_675 ?
Bi1 N4 Bi1 111.00(8) . 2_675 ?
N6 N5 N4 176.8(2) . . ?
C5 N7 C1 117.9(2) . . ?
C5 N7 Bi1 116.13(18) . . ?
C1 N7 Bi1 125.88(16) . . ?
N7 C1 C2 122.9(3) . . ?
C1 C2 C3 118.5(3) . . ?
C4 C3 C2 118.9(3) . . ?
C3 C4 C5 118.6(3) . . ?
N7 C5 C4 123.3(3) . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N4 Bi1 N1 N2 -141.74(5) 4_655 . . . ?
N4 Bi1 N1 N2 141.74(5) . . . . ?
N7 Bi1 N1 N2 57.72(5) . . . . ?
N7 Bi1 N1 N2 -57.72(5) 4_655 . . . ?
N4 Bi1 N1 N2 95.10(17) 3_574 . . . ?
N4 Bi1 N1 N2 -95.10(17) 2_674 . . . ?
N1 Bi1 N4 N5 -125.8(2) . . . . ?
N4 Bi1 N4 N5 149.20(16) 4_655 . . . ?
N7 Bi1 N4 N5 -44.11(19) . . . . ?
N7 Bi1 N4 N5 -177.69(16) 4_655 . . . ?
N4 Bi1 N4 N5 31.72(17) 3_574 . . . ?
N4 Bi1 N4 N5 81.52(17) 2_674 . . . ?
N1 Bi1 N4 Bi1 76.35(8) . . . 2_675 ?
N4 Bi1 N4 Bi1 -8.64(11) 4_655 . . 2_675 ?
N7 Bi1 N4 Bi1 158.05(9) . . . 2_675 ?
N7 Bi1 N4 Bi1 24.5(2) 4_655 . . 2_675 ?
N4 Bi1 N4 Bi1 -126.13(11) 3_574 . . 2_675 ?
N4 Bi1 N4 Bi1 -76.32(11) 2_674 . . 2_675 ?
N1 Bi1 N7 C5 -129.4(2) . . . . ?
N4 Bi1 N7 C5 178.30(19) 4_655 . . . ?
N4 Bi1 N7 C5 146.0(2) . . . . ?
N7 Bi1 N7 C5 -53.2(2) 4_655 . . . ?
N4 Bi1 N7 C5 69.32(19) 3_574 . . . ?
N4 Bi1 N7 C5 34.0(2) 2_674 . . . ?
N1 Bi1 N7 C1 54.8(2) . . . . ?
N4 Bi1 N7 C1 2.4(3) 4_655 . . . ?
N4 Bi1 N7 C1 -29.8(2) . . . . ?
N7 Bi1 N7 C1 130.92(18) 4_655 . . . ?
N4 Bi1 N7 C1 -106.5(2) 3_574 . . . ?
N4 Bi1 N7 C1 -141.83(19) 2_674 . . . ?
C5 N7 C1 C2 -0.1(4) . . . . ?
Bi1 N7 C1 C2 175.72(19) . . . . ?
N7 C1 C2 C3 0.4(4) . . . . ?
C1 C2 C3 C4 -0.4(4) . . . . ?
C2 C3 C4 C5 0.1(4) . . . . ?
C1 N7 C5 C4 -0.2(4) . . . . ?
Bi1 N7 C5 C4 -176.4(2) . . . . ?
C3 C4 C5 N7 0.2(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C2 H2 N6 0.95 2.59 3.268(3) 128.6 8_545

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        30.55
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.038
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.091

_vrf_PLAT220_ben_bin33no3        
;
PROBLEM: Large Non-Solvent N Ueq(max)/Ueq(min) ...
RESPONSE: The ADP's of N1, N2 and N3 indicate either a
strong thermal movement of terminal group (ADPs increase towards
the end of the azido-group) or a minor disorder with the N atoms
placed slightly off the mirror plane. It was not possible to identify
separate positions for disorderd atoms.
;


data_ben_084lt
_database_code_depnum_ccdc_archive 'CCDC 808989'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'N9 Sb'
_chemical_formula_weight         247.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.6694(6)
_cell_length_b                   6.9045(6)
_cell_length_c                   7.0314(6)
_cell_angle_alpha                83.651(5)
_cell_angle_beta                 65.850(5)
_cell_angle_gamma                83.595(5)
_cell_volume                     292.85(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    2561
_cell_measurement_theta_min      2.97
_cell_measurement_theta_max      25.12

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.811
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             228
_exptl_absorpt_coefficient_mu    4.642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_process_details   
;
BRUKER AXS SMART APEX 2 Vers. 3.0-2009
R.H. Blessing, Acta Cryst. (1995) A51 33-38
;

_exptl_special_details           
;
The crystallization was performed on the diffractometer at a temperature of
296 K with a sublimation procedure using focussed infrared-laser-
radiation according to: R. Boese, M. Nussbaumer, "In Situ Crystallisation
Techniques", in: "Organic Crystal Chemistry",
Ed. D.W. Jones, Oxford University Press, Oxford, England, (1994) 20-37
;

_diffrn_ambient_temperature      103(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'Triumph graphite'
_diffrn_measurement_device_type  
;
Bruker D8 KAPPA series II with APEX II area detector system
;
_diffrn_measurement_method       
;
Data collection strategy APEX 2/COSMO
;
_diffrn_detector_area_resol_mean 512
_diffrn_reflns_number            3719
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.98
_diffrn_reflns_theta_max         25.20
_reflns_number_total             1012
_reflns_number_gt                933
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_cell_refinement       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_data_reduction        'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_structure_solution    'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_structure_refinement  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_molecular_graphics    'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+2.1026P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   notdet
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1012
_refine_ls_number_parameters     91
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0254
_refine_ls_wR_factor_ref         0.0639
_refine_ls_wR_factor_gt          0.0622
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_restrained_S_all      1.120
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb 0.16997(6) 0.45382(6) 0.68458(6) 0.01478(15) Uani 1 1 d . . .
N1 N 0.1364(9) 0.6458(7) 0.9185(8) 0.0186(11) Uani 1 1 d . . .
N2 N 0.1992(9) 0.8114(8) 0.8589(8) 0.0190(11) Uani 1 1 d . . .
N3 N 0.2559(10) 0.9634(8) 0.8088(9) 0.0282(13) Uani 1 1 d . . .
N4 N 0.3750(8) 0.6537(7) 0.4561(8) 0.0190(11) Uani 1 1 d . . .
N5 N 0.2798(8) 0.7867(7) 0.3815(8) 0.0195(11) Uani 1 1 d . . .
N6 N 0.2000(9) 0.9062(8) 0.3070(9) 0.0267(13) Uani 1 1 d . . .
N7 N -0.1127(8) 0.6091(7) 0.6556(8) 0.0175(11) Uani 1 1 d . . .
N8 N -0.2619(8) 0.6668(7) 0.8172(8) 0.0179(12) Uani 1 1 d . . .
N9 N -0.4045(9) 0.7186(8) 0.9623(9) 0.0254(12) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sb1 0.0124(2) 0.0201(2) 0.0109(2) 0.00043(15) -0.00386(17) -0.00225(15)
N1 0.023(3) 0.022(3) 0.010(3) 0.000(2) -0.005(2) -0.006(2)
N2 0.024(3) 0.025(3) 0.012(3) 0.000(2) -0.012(2) -0.003(2)
N3 0.040(4) 0.025(3) 0.026(3) 0.003(3) -0.019(3) -0.009(3)
N4 0.011(3) 0.026(3) 0.016(3) 0.006(2) -0.001(2) -0.005(2)
N5 0.016(3) 0.024(3) 0.010(3) 0.001(2) 0.003(2) -0.003(2)
N6 0.022(3) 0.029(3) 0.018(3) 0.004(2) 0.000(3) 0.005(2)
N7 0.011(3) 0.029(3) 0.009(3) -0.004(2) -0.003(2) 0.008(2)
N8 0.015(3) 0.022(3) 0.020(3) 0.002(2) -0.010(3) -0.004(2)
N9 0.017(3) 0.038(3) 0.016(3) -0.003(3) -0.002(3) 0.006(3)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.

Operators for generating equivalent atoms:

$1 -x, -y+1, -z+2
$2 -x+1, -y+1, -z+1
$3 -x, -y+1, -z+1

Distance DIST

2.7678 (0.0051) Sb1 - N1_$1
2.8185 (0.0050) Sb1 - N4_$2
2.6592 (0.0048) Sb1 - N7_$3

Angle ANGL

65.11 ( 0.20) N1 - Sb1 - N1_$1
99.21 ( 0.18) N1 - Sb1 - N4_$2
149.69 ( 0.17) N1 - Sb1 - N7_$3
152.34 ( 0.18) N4 - Sb1 - N1_$1
65.24 ( 0.20) N4 - Sb1 - N4_$2
77.47 ( 0.18) N4 - Sb1 - N7_$3
82.12 ( 0.17) N7 - Sb1 - N1_$1
153.53 ( 0.17) N7 - Sb1 - N4_$2
65.12 ( 0.21) N7 - Sb1 - N7_$3
124.12 ( 0.14) N1_$1 - Sb1 - N4_$2
121.62 ( 0.15) N1_$1 - Sb1 - N7_$3
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb1 N4 2.119(5) . ?
Sb1 N7 2.136(5) . ?
Sb1 N1 2.151(5) . ?
N1 N2 1.231(7) . ?
N2 N3 1.125(7) . ?
N4 N5 1.248(7) . ?
N5 N6 1.128(7) . ?
N7 N8 1.235(7) . ?
N8 N9 1.133(8) . ?

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
_geom_angle_publ_flag
N4 Sb1 N7 89.92(19) . . ?
N4 Sb1 N1 88.4(2) . . ?
N7 Sb1 N1 88.52(19) . . ?
N2 N1 Sb1 117.8(4) . . ?
N3 N2 N1 178.5(6) . . ?
N5 N4 Sb1 116.1(4) . . ?
N6 N5 N4 177.4(6) . . ?
N8 N7 Sb1 117.1(4) . . ?
N9 N8 N7 177.4(6) . . ?

_diffrn_measured_fraction_theta_max 0.963
_diffrn_reflns_theta_full        25.20
_diffrn_measured_fraction_theta_full 0.963
_refine_diff_density_max         1.269
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.165