# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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data_compound1


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H30 B2 N24 Na2 O5 S6, H2 O'
_chemical_formula_sum            'C12 H32 B2 N24 Na2 O6 S6'
_chemical_formula_weight         868.58

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   9.3355(2)
_cell_length_b                   12.8329(3)
_cell_length_c                   15.7966(3)
_cell_angle_alpha                83.0920(13)
_cell_angle_beta                 89.0734(15)
_cell_angle_gamma                85.1892(11)
_cell_volume                     1872.06(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    61457
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             896
_exptl_absorpt_coefficient_mu    0.455
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8755
_exptl_absorpt_correction_T_max  0.9820
_exptl_absorpt_process_details   
'Denzo and Scalepack (Otwinowski & Minor, 1997)'

_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  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16165
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0521
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.21
_diffrn_reflns_theta_max         27.50
_reflns_number_total             8547
_reflns_number_gt                6514
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect, Bruker AXS, 2004'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-PLUS (1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'



_refine_special_details          
; 
 H atoms at oxygen were refined with Ueq=1.5 of the U(eq) value of 
 corresponding atom. All O-H distances were restrained to have a value 
 of 0.84 Ang. H6e and H6f are  disordered in the ratio of 1:1. 

 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0534P)²+0.3754P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8547
_refine_ls_number_parameters     525
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0399
_refine_ls_wR_factor_ref         0.1057
_refine_ls_wR_factor_gt          0.0959
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.130
_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
S1 S 0.78286(7) 0.41871(5) 0.24793(4) 0.02732(15) Uani 1 1 d . . .
S2 S 0.55046(7) 0.17153(5) 0.10250(4) 0.02440(14) Uani 1 1 d . . .
S3 S 1.07016(7) 0.14815(5) 0.03830(4) 0.02818(16) Uani 1 1 d . . .
S4 S 0.61357(6) 0.65433(5) 0.09138(4) 0.02187(14) Uani 1 1 d . . .
S5 S 0.06133(7) 0.66273(5) 0.14001(4) 0.02478(14) Uani 1 1 d . . .
S6 S 0.34209(7) 0.35698(5) 0.31751(4) 0.02382(14) Uani 1 1 d . . .
Na1 Na 0.88523(10) 0.50374(7) 0.08777(6) 0.0226(2) Uani 1 1 d . . .
Na2 Na 0.5000 0.5000 0.0000 0.0232(3) Uani 1 2 d S . .
Na3 Na 0.5000 0.0000 0.5000 0.0274(3) Uani 1 2 d S . .
N1 N 0.9274(2) 0.22312(15) 0.28237(12) 0.0198(4) Uani 1 1 d . . .
N2 N 1.0202(2) 0.17193(15) 0.34237(13) 0.0231(4) Uani 1 1 d . . .
N3 N 1.0510(2) 0.23630(15) 0.39380(13) 0.0253(5) Uani 1 1 d . . .
N4 N 0.9764(2) 0.33029(15) 0.36827(12) 0.0216(4) Uani 1 1 d . . .
N5 N 0.7143(2) 0.13194(15) 0.24766(12) 0.0193(4) Uani 1 1 d . . .
N6 N 0.6953(2) 0.09750(16) 0.33206(12) 0.0234(4) Uani 1 1 d . . .
N7 N 0.5628(2) 0.08236(15) 0.34483(12) 0.0219(4) Uani 1 1 d . . .
N8 N 0.4944(2) 0.10692(14) 0.26920(12) 0.0186(4) Uani 1 1 d . . .
N9 N 0.9616(2) 0.07138(15) 0.19416(12) 0.0206(4) Uani 1 1 d . . .
N10 N 0.9813(2) -0.01994(16) 0.24976(13) 0.0249(5) Uani 1 1 d . . .
N11 N 1.0738(2) -0.08317(15) 0.21774(12) 0.0240(4) Uani 1 1 d . . .
N12 N 1.1162(2) -0.03451(15) 0.14160(12) 0.0204(4) Uani 1 1 d . . .
N13 N 0.4504(2) 0.71374(14) 0.22803(11) 0.0172(4) Uani 1 1 d . . .
N14 N 0.4335(2) 0.80008(14) 0.27123(12) 0.0212(4) Uani 1 1 d . . .
N15 N 0.5131(2) 0.87007(15) 0.23583(13) 0.0240(4) Uani 1 1 d . . .
N16 N 0.5831(2) 0.82941(14) 0.16991(12) 0.0201(4) Uani 1 1 d . . .
N17 N 0.2199(2) 0.64601(14) 0.28682(11) 0.0175(4) Uani 1 1 d . . .
N18 N 0.1959(2) 0.66203(16) 0.37004(12) 0.0240(4) Uani 1 1 d . . .
N19 N 0.0621(2) 0.68630(16) 0.38072(13) 0.0237(4) Uani 1 1 d . . .
N20 N -0.0028(2) 0.68685(14) 0.30487(12) 0.0192(4) Uani 1 1 d . . .
N21 N 0.45682(19) 0.54566(14) 0.32576(11) 0.0167(4) Uani 1 1 d . . .
N22 N 0.5586(2) 0.58383(15) 0.37224(12) 0.0192(4) Uani 1 1 d . . .
N23 N 0.6149(2) 0.50803(14) 0.42478(12) 0.0191(4) Uani 1 1 d . . .
N24 N 0.5495(2) 0.42043(14) 0.41313(12) 0.0176(4) Uani 1 1 d . . .
O1 O 1.08790(18) 0.39974(13) 0.05099(11) 0.0224(4) Uani 1 1 d D . .
H1A H 1.165(2) 0.397(2) 0.0750(17) 0.034 Uiso 1 1 d D . .
H1B H 1.076(3) 0.3348(15) 0.0529(18) 0.034 Uiso 1 1 d D . .
O2 O 0.72547(18) 0.39730(13) 0.02169(11) 0.0228(4) Uani 1 1 d D . .
H2A H 0.762(3) 0.378(2) -0.0217(14) 0.034 Uiso 1 1 d D . .
H2B H 0.716(3) 0.3431(17) 0.0540(16) 0.034 Uiso 1 1 d D . .
O3 O 0.36999(18) 0.39671(13) 0.10708(11) 0.0228(4) Uani 1 1 d D . .
H3A H 0.370(3) 0.405(2) 0.1577(12) 0.034 Uiso 1 1 d D . .
H3B H 0.403(3) 0.3354(16) 0.1040(18) 0.034 Uiso 1 1 d D . .
O4 O 0.6922(2) -0.13335(18) 0.49374(15) 0.0485(6) Uani 1 1 d D . .
H4A H 0.776(3) -0.122(3) 0.478(2) 0.073 Uiso 1 1 d D . .
H4B H 0.706(4) -0.177(3) 0.5360(18) 0.073 Uiso 1 1 d D . .
O5 O 0.6718(2) 0.09703(15) 0.56513(12) 0.0329(4) Uani 1 1 d D . .
H5A H 0.761(2) 0.099(3) 0.560(2) 0.049 Uiso 1 1 d D . .
H5B H 0.655(3) 0.135(2) 0.6046(17) 0.049 Uiso 1 1 d D . .
O6 O 0.9972(3) -0.0725(2) 0.43950(14) 0.0558(6) Uani 1 1 d D . .
H6D H 0.994(5) -0.038(3) 0.3899(16) 0.084 Uiso 1 1 d D . .
H6E H 0.931(7) -0.111(6) 0.429(6) 0.084 Uiso 0.50 1 d PD . .
H6F H 0.995(11) -0.023(5) 0.472(5) 0.084 Uiso 0.50 1 d PD . .
B1 B 0.8603(3) 0.1679(2) 0.21318(17) 0.0212(6) Uani 1 1 d . . .
H1 H 0.839(2) 0.2250(18) 0.1547(15) 0.018(6) Uiso 1 1 d . . .
B2 B 0.3714(3) 0.6135(2) 0.25343(17) 0.0186(5) Uani 1 1 d . . .
H2 H 0.363(2) 0.5721(18) 0.1959(14) 0.014(6) Uiso 1 1 d . . .
C1 C 0.8969(2) 0.32452(18) 0.29811(15) 0.0211(5) Uani 1 1 d . . .
C2 C 0.9930(3) 0.42205(19) 0.41147(16) 0.0290(6) Uani 1 1 d . . .
H2C H 1.0611 0.4662 0.3796 0.044 Uiso 1 1 calc R . .
H2D H 1.0294 0.3994 0.4692 0.044 Uiso 1 1 calc R . .
H2E H 0.8997 0.4625 0.4148 0.044 Uiso 1 1 calc R . .
C3 C 0.5871(2) 0.13795(17) 0.20668(15) 0.0195(5) Uani 1 1 d . . .
C4 C 0.3407(2) 0.09893(19) 0.26235(17) 0.0256(5) Uani 1 1 d . . .
H4C H 0.2972 0.1619 0.2279 0.038 Uiso 1 1 calc R . .
H4D H 0.2972 0.0931 0.3194 0.038 Uiso 1 1 calc R . .
H4E H 0.3241 0.0364 0.2351 0.038 Uiso 1 1 calc R . .
C5 C 1.0480(2) 0.06312(18) 0.12515(14) 0.0197(5) Uani 1 1 d . . .
C6 C 1.2258(3) -0.08382(19) 0.08923(16) 0.0255(5) Uani 1 1 d . . .
H6A H 1.1879 -0.0850 0.0319 0.038 Uiso 1 1 calc R . .
H6B H 1.2523 -0.1561 0.1150 0.038 Uiso 1 1 calc R . .
H6C H 1.3108 -0.0435 0.0856 0.038 Uiso 1 1 calc R . .
C7 C 0.5467(2) 0.73092(17) 0.16368(14) 0.0169(5) Uani 1 1 d . . .
C8 C 0.6817(3) 0.88823(19) 0.11476(17) 0.0308(6) Uani 1 1 d . . .
H8A H 0.7798 0.8555 0.1237 0.046 Uiso 1 1 calc R . .
H8B H 0.6770 0.9610 0.1282 0.046 Uiso 1 1 calc R . .
H8C H 0.6548 0.8878 0.0551 0.046 Uiso 1 1 calc R . .
C9 C 0.0939(2) 0.66316(16) 0.24403(14) 0.0181(5) Uani 1 1 d . . .
C10 C -0.1571(2) 0.7138(2) 0.29607(17) 0.0282(6) Uani 1 1 d . . .
H10A H -0.2037 0.7014 0.3520 0.042 Uiso 1 1 calc R . .
H10B H -0.1964 0.6699 0.2569 0.042 Uiso 1 1 calc R . .
H10C H -0.1748 0.7882 0.2734 0.042 Uiso 1 1 calc R . .
C11 C 0.4501(2) 0.44137(17) 0.35163(14) 0.0184(5) Uani 1 1 d . . .
C12 C 0.5945(3) 0.31806(18) 0.45949(15) 0.0237(5) Uani 1 1 d . . .
H12A H 0.6326 0.2702 0.4192 0.036 Uiso 1 1 calc R . .
H12B H 0.5119 0.2890 0.4900 0.036 Uiso 1 1 calc R . .
H12C H 0.6693 0.3262 0.5004 0.036 Uiso 1 1 calc R . .


_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
S1 C1 1.675(2) . ?
S1 Na1 2.8173(11) . ?
S2 C3 1.683(2) . ?
S3 C5 1.669(2) . ?
S4 C7 1.675(2) . ?
S4 Na2 2.8670(6) . ?
S4 Na1 3.0609(11) . ?
S5 C9 1.677(2) . ?
S5 Na1 2.9253(11) 1_455 ?
S6 C11 1.680(2) . ?
Na1 O1 2.3294(19) . ?
Na1 O1 2.4049(19) 2_765 ?
Na1 O2 2.4322(19) . ?
Na1 S5 2.9253(11) 1_655 ?
Na1 Na1 3.4825(17) 2_765 ?
Na1 Na2 3.8814(9) . ?
Na2 O2 2.3946(17) 2_665 ?
Na2 O2 2.3946(17) . ?
Na2 O3 2.3990(17) . ?
Na2 O3 2.3990(17) 2_665 ?
Na2 S4 2.8669(6) 2_665 ?
Na2 Na1 3.8814(9) 2_665 ?
Na3 O4 2.382(2) 2_656 ?
Na3 O4 2.382(2) . ?
Na3 O5 2.4242(19) . ?
Na3 O5 2.4242(19) 2_656 ?
Na3 N7 2.6272(19) . ?
Na3 N7 2.6273(19) 2_656 ?
N1 C1 1.360(3) . ?
N1 N2 1.365(3) . ?
N1 B1 1.540(3) . ?
N2 N3 1.278(3) . ?
N3 N4 1.361(3) . ?
N4 C1 1.356(3) . ?
N4 C2 1.450(3) . ?
N5 C3 1.354(3) . ?
N5 N6 1.367(3) . ?
N5 B1 1.546(3) . ?
N6 N7 1.278(3) . ?
N7 N8 1.354(3) . ?
N8 C3 1.348(3) . ?
N8 C4 1.454(3) . ?
N9 C5 1.354(3) . ?
N9 N10 1.378(3) . ?
N9 B1 1.550(3) . ?
N10 N11 1.276(3) . ?
N11 N12 1.356(3) . ?
N12 C5 1.355(3) . ?
N12 C6 1.456(3) . ?
N13 C7 1.356(3) . ?
N13 N14 1.367(2) . ?
N13 B2 1.544(3) . ?
N14 N15 1.285(3) . ?
N15 N16 1.354(3) . ?
N16 C7 1.351(3) . ?
N16 C8 1.452(3) . ?
N17 C9 1.355(3) . ?
N17 N18 1.367(3) . ?
N17 B2 1.543(3) . ?
N18 N19 1.275(3) . ?
N19 N20 1.350(3) . ?
N20 C9 1.352(3) . ?
N20 C10 1.457(3) . ?
N21 C11 1.358(3) . ?
N21 N22 1.367(3) . ?
N21 B2 1.541(3) . ?
N22 N23 1.283(3) . ?
N23 N24 1.356(2) . ?
N24 C11 1.342(3) . ?
N24 C12 1.458(3) . ?
O1 Na1 2.4049(19) 2_765 ?
O1 H1A 0.819(18) . ?
O1 H1B 0.847(18) . ?
O2 H2A 0.817(18) . ?
O2 H2B 0.822(18) . ?
O3 H3A 0.820(18) . ?
O3 H3B 0.827(18) . ?
O4 H4A 0.84(2) . ?
O4 H4B 0.83(2) . ?
O5 H5A 0.840(19) . ?
O5 H5B 0.843(19) . ?
O6 H6D 0.85(2) . ?
O6 H6E 0.85(2) . ?
O6 H6F 0.87(2) . ?
B1 H1 1.12(2) . ?
B2 H2 1.11(2) . ?
C2 H2C 0.9800 . ?
C2 H2D 0.9800 . ?
C2 H2E 0.9800 . ?
C4 H4C 0.9800 . ?
C4 H4D 0.9800 . ?
C4 H4E 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?

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
C1 S1 Na1 113.29(8) . . ?
C7 S4 Na2 134.48(8) . . ?
C7 S4 Na1 132.50(8) . . ?
Na2 S4 Na1 81.73(2) . . ?
C9 S5 Na1 118.90(8) . 1_455 ?
O1 Na1 O1 85.30(7) . 2_765 ?
O1 Na1 O2 91.99(6) . . ?
O1 Na1 O2 87.14(6) 2_765 . ?
O1 Na1 S1 108.95(6) . . ?
O1 Na1 S1 165.20(6) 2_765 . ?
O2 Na1 S1 88.35(5) . . ?
O1 Na1 S5 91.83(5) . 1_655 ?
O1 Na1 S5 82.86(5) 2_765 1_655 ?
O2 Na1 S5 168.96(6) . 1_655 ?
S1 Na1 S5 100.18(3) . 1_655 ?
O1 Na1 S4 166.69(6) . . ?
O1 Na1 S4 82.20(5) 2_765 . ?
O2 Na1 S4 82.89(5) . . ?
S1 Na1 S4 83.26(3) . . ?
S5 Na1 S4 91.11(3) 1_655 . ?
O1 Na1 Na1 43.49(5) . 2_765 ?
O1 Na1 Na1 41.81(4) 2_765 2_765 ?
O2 Na1 Na1 89.36(5) . 2_765 ?
S1 Na1 Na1 152.24(5) . 2_765 ?
S5 Na1 Na1 86.30(4) 1_655 2_765 ?
S4 Na1 Na1 123.86(4) . 2_765 ?
O1 Na1 Na2 126.06(5) . . ?
O1 Na1 Na2 79.93(5) 2_765 . ?
O2 Na1 Na2 36.15(4) . . ?
S1 Na1 Na2 88.13(3) . . ?
S5 Na1 Na2 136.28(3) 1_655 . ?
S4 Na1 Na2 46.968(17) . . ?
Na1 Na1 Na2 105.85(4) 2_765 . ?
O2 Na2 O2 180.0 2_665 . ?
O2 Na2 O3 84.01(6) 2_665 . ?
O2 Na2 O3 95.99(6) . . ?
O2 Na2 O3 95.99(6) 2_665 2_665 ?
O2 Na2 O3 84.01(6) . 2_665 ?
O3 Na2 O3 180.0 . 2_665 ?
O2 Na2 S4 87.86(4) 2_665 2_665 ?
O2 Na2 S4 92.14(4) . 2_665 ?
O3 Na2 S4 76.41(4) . 2_665 ?
O3 Na2 S4 103.59(4) 2_665 2_665 ?
O2 Na2 S4 92.14(4) 2_665 . ?
O2 Na2 S4 87.86(4) . . ?
O3 Na2 S4 103.59(4) . . ?
O3 Na2 S4 76.41(4) 2_665 . ?
S4 Na2 S4 180.000(15) 2_665 . ?
O2 Na2 Na1 143.19(4) 2_665 . ?
O2 Na2 Na1 36.81(4) . . ?
O3 Na2 Na1 106.39(4) . . ?
O3 Na2 Na1 73.61(4) 2_665 . ?
S4 Na2 Na1 128.700(18) 2_665 . ?
S4 Na2 Na1 51.300(18) . . ?
O2 Na2 Na1 36.81(4) 2_665 2_665 ?
O2 Na2 Na1 143.19(4) . 2_665 ?
O3 Na2 Na1 73.61(4) . 2_665 ?
O3 Na2 Na1 106.39(4) 2_665 2_665 ?
S4 Na2 Na1 51.300(18) 2_665 2_665 ?
S4 Na2 Na1 128.700(18) . 2_665 ?
Na1 Na2 Na1 180.0 . 2_665 ?
O4 Na3 O4 180.0 2_656 . ?
O4 Na3 O5 93.99(7) 2_656 . ?
O4 Na3 O5 86.01(7) . . ?
O4 Na3 O5 86.01(7) 2_656 2_656 ?
O4 Na3 O5 93.99(7) . 2_656 ?
O5 Na3 O5 180.00(7) . 2_656 ?
O4 Na3 N7 89.81(7) 2_656 . ?
O4 Na3 N7 90.19(7) . . ?
O5 Na3 N7 93.18(6) . . ?
O5 Na3 N7 86.82(6) 2_656 . ?
O4 Na3 N7 90.19(7) 2_656 2_656 ?
O4 Na3 N7 89.81(7) . 2_656 ?
O5 Na3 N7 86.82(6) . 2_656 ?
O5 Na3 N7 93.18(6) 2_656 2_656 ?
N7 Na3 N7 180.0 . 2_656 ?
C1 N1 N2 109.77(19) . . ?
C1 N1 B1 126.9(2) . . ?
N2 N1 B1 123.15(19) . . ?
N3 N2 N1 108.93(19) . . ?
N2 N3 N4 107.27(19) . . ?
C1 N4 N3 111.06(19) . . ?
C1 N4 C2 127.8(2) . . ?
N3 N4 C2 121.0(2) . . ?
C3 N5 N6 109.63(18) . . ?
C3 N5 B1 128.85(19) . . ?
N6 N5 B1 121.21(19) . . ?
N7 N6 N5 108.46(19) . . ?
N6 N7 N8 107.58(18) . . ?
N6 N7 Na3 114.84(15) . . ?
N8 N7 Na3 137.31(14) . . ?
C3 N8 N7 110.97(18) . . ?
C3 N8 C4 127.8(2) . . ?
N7 N8 C4 121.20(19) . . ?
C5 N9 N10 109.26(18) . . ?
C5 N9 B1 127.4(2) . . ?
N10 N9 B1 123.29(18) . . ?
N11 N10 N9 108.70(18) . . ?
N10 N11 N12 107.52(19) . . ?
C5 N12 N11 111.09(18) . . ?
C5 N12 C6 127.04(19) . . ?
N11 N12 C6 121.82(19) . . ?
C7 N13 N14 109.39(17) . . ?
C7 N13 B2 127.65(18) . . ?
N14 N13 B2 122.95(18) . . ?
N15 N14 N13 108.68(18) . . ?
N14 N15 N16 107.39(18) . . ?
C7 N16 N15 110.98(17) . . ?
C7 N16 C8 126.73(18) . . ?
N15 N16 C8 122.29(18) . . ?
C9 N17 N18 109.22(18) . . ?
C9 N17 B2 129.04(19) . . ?
N18 N17 B2 121.75(18) . . ?
N19 N18 N17 108.87(19) . . ?
N18 N19 N20 107.53(18) . . ?
N19 N20 C9 110.96(18) . . ?
N19 N20 C10 120.64(18) . . ?
C9 N20 C10 128.4(2) . . ?
C11 N21 N22 109.28(18) . . ?
C11 N21 B2 127.55(19) . . ?
N22 N21 B2 123.12(18) . . ?
N23 N22 N21 108.56(17) . . ?
N22 N23 N24 107.38(18) . . ?
C11 N24 N23 111.09(18) . . ?
C11 N24 C12 127.22(19) . . ?
N23 N24 C12 121.55(19) . . ?
Na1 O1 Na1 94.70(7) . 2_765 ?
Na1 O1 H1A 123(2) . . ?
Na1 O1 H1A 107(2) 2_765 . ?
Na1 O1 H1B 114.4(19) . . ?
Na1 O1 H1B 117.1(19) 2_765 . ?
H1A O1 H1B 101(3) . . ?
Na2 O2 Na1 107.05(7) . . ?
Na2 O2 H2A 114(2) . . ?
Na1 O2 H2A 110(2) . . ?
Na2 O2 H2B 111(2) . . ?
Na1 O2 H2B 109(2) . . ?
H2A O2 H2B 106(3) . . ?
Na2 O3 H3A 123(2) . . ?
Na2 O3 H3B 104(2) . . ?
H3A O3 H3B 107(3) . . ?
Na3 O4 H4A 124(3) . . ?
Na3 O4 H4B 118(3) . . ?
H4A O4 H4B 102(4) . . ?
Na3 O5 H5A 132(2) . . ?
Na3 O5 H5B 127(2) . . ?
H5A O5 H5B 101(3) . . ?
H6D O6 H6E 93(6) . . ?
H6D O6 H6F 103(7) . . ?
H6E O6 H6F 129(9) . . ?
N1 B1 N5 107.69(18) . . ?
N1 B1 N9 109.5(2) . . ?
N5 B1 N9 110.19(19) . . ?
N1 B1 H1 109.7(12) . . ?
N5 B1 H1 108.0(12) . . ?
N9 B1 H1 111.7(12) . . ?
N21 B2 N17 109.02(18) . . ?
N21 B2 N13 107.89(19) . . ?
N17 B2 N13 108.81(18) . . ?
N21 B2 H2 112.5(12) . . ?
N17 B2 H2 110.1(12) . . ?
N13 B2 H2 108.4(11) . . ?
N4 C1 N1 103.0(2) . . ?
N4 C1 S1 127.56(18) . . ?
N1 C1 S1 129.39(19) . . ?
N4 C2 H2C 109.5 . . ?
N4 C2 H2D 109.5 . . ?
H2C C2 H2D 109.5 . . ?
N4 C2 H2E 109.5 . . ?
H2C C2 H2E 109.5 . . ?
H2D C2 H2E 109.5 . . ?
N8 C3 N5 103.36(19) . . ?
N8 C3 S2 127.23(18) . . ?
N5 C3 S2 129.38(17) . . ?
N8 C4 H4C 109.5 . . ?
N8 C4 H4D 109.5 . . ?
H4C C4 H4D 109.5 . . ?
N8 C4 H4E 109.5 . . ?
H4C C4 H4E 109.5 . . ?
H4D C4 H4E 109.5 . . ?
N9 C5 N12 103.42(19) . . ?
N9 C5 S3 130.63(18) . . ?
N12 C5 S3 125.95(17) . . ?
N12 C6 H6A 109.5 . . ?
N12 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N12 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N16 C7 N13 103.55(18) . . ?
N16 C7 S4 124.91(17) . . ?
N13 C7 S4 131.54(17) . . ?
N16 C8 H8A 109.5 . . ?
N16 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N16 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N20 C9 N17 103.41(19) . . ?
N20 C9 S5 126.73(18) . . ?
N17 C9 S5 129.78(17) . . ?
N20 C10 H10A 109.5 . . ?
N20 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N20 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N24 C11 N21 103.68(19) . . ?
N24 C11 S6 127.19(17) . . ?
N21 C11 S6 129.11(18) . . ?
N24 C12 H12A 109.5 . . ?
N24 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N24 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.070
_database_code_depnum_ccdc_archive 'CCDC 981804'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound2a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
  
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H14 B K N12 O2 S3'
_chemical_formula_sum            'C6 H14 B K N12 O2 S3'
_chemical_formula_weight         432.38

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   8.82110(10)
_cell_length_b                   16.10670(10)
_cell_length_c                   12.83460(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.1234(6)
_cell_angle_gamma                90.00
_cell_volume                     1775.90(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    43244
_cell_measurement_theta_min      2.910
_cell_measurement_theta_max      30.034

_exptl_crystal_description       fragment
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             888
_exptl_absorpt_coefficient_mu    0.683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8214
_exptl_absorpt_correction_T_max  0.8986
_exptl_absorpt_process_details   
'Denzo and Scalepack (Otwinowski & Minor, 1997)'

_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  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            71800
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.50
_diffrn_reflns_theta_max         30.00
_reflns_number_total             5164
_reflns_number_gt                4541
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect, Bruker AXS, 2004'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-PLUS (1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'



_refine_special_details          
; 
 Hydrogens were refined isotropically.

 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0371P)²+0.4231P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5164
_refine_ls_number_parameters     282
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0248
_refine_ls_wR_factor_ref         0.0659
_refine_ls_wR_factor_gt          0.0634
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.001
_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
K1 K 0.37794(3) 0.608737(15) 0.961980(18) 0.01783(6) Uani 1 1 d . . .
S1 S 0.18936(3) 0.559125(15) 0.71332(2) 0.01448(6) Uani 1 1 d . . .
S2 S 0.02784(3) 0.686399(16) 0.94791(2) 0.01710(6) Uani 1 1 d . . .
S3 S 0.55469(3) 0.808609(18) 0.83551(2) 0.02060(7) Uani 1 1 d . . .
O1 O 0.56555(10) 0.50545(5) 0.87594(6) 0.01820(16) Uani 1 1 d . . .
H1A H 0.517(2) 0.4789(11) 0.8237(15) 0.038(5) Uiso 1 1 d . . .
H1B H 0.619(2) 0.5396(13) 0.8497(16) 0.052(6) Uiso 1 1 d . . .
N1 N 0.05802(10) 0.71408(5) 0.67054(7) 0.01301(16) Uani 1 1 d . . .
N2 N -0.07682(10) 0.74712(6) 0.61020(7) 0.01636(17) Uani 1 1 d . . .
N3 N -0.16213(11) 0.68787(6) 0.56298(7) 0.01677(18) Uani 1 1 d . . .
N4 N -0.08473(10) 0.61586(5) 0.59214(7) 0.01396(17) Uani 1 1 d . . .
N5 N 0.08281(10) 0.81536(5) 0.82185(7) 0.01274(16) Uani 1 1 d . . .
N6 N 0.05552(11) 0.89849(5) 0.81359(7) 0.01518(17) Uani 1 1 d . . .
N7 N -0.01087(11) 0.92099(6) 0.88810(7) 0.01618(17) Uani 1 1 d . . .
N8 N -0.02717(10) 0.85239(5) 0.94559(7) 0.01456(17) Uani 1 1 d . . .
N9 N 0.26670(10) 0.82688(5) 0.69829(7) 0.01270(16) Uani 1 1 d . . .
N10 N 0.20201(10) 0.87414(5) 0.61105(7) 0.01464(17) Uani 1 1 d . . .
N11 N 0.30803(10) 0.92092(6) 0.58887(7) 0.01542(17) Uani 1 1 d . . .
N12 N 0.44204(10) 0.90424(6) 0.66099(7) 0.01451(17) Uani 1 1 d . . .
B1 B 0.17450(13) 0.76599(7) 0.75212(9) 0.0131(2) Uani 1 1 d . . .
H1 H 0.2532(15) 0.7242(8) 0.8031(10) 0.013(3) Uiso 1 1 d . . .
C1 C 0.05500(12) 0.62991(6) 0.66001(8) 0.01242(18) Uani 1 1 d . . .
C2 C -0.15835(13) 0.53702(7) 0.55613(9) 0.0184(2) Uani 1 1 d . . .
H2A H -0.1807(17) 0.5345(9) 0.4816(13) 0.025(4) Uiso 1 1 d . . .
H2B H -0.0858(17) 0.4935(9) 0.5857(12) 0.023(4) Uiso 1 1 d . . .
H2C H -0.2530(17) 0.5340(9) 0.5806(11) 0.019(3) Uiso 1 1 d . . .
C3 C 0.02904(11) 0.78472(6) 0.90493(8) 0.01347(19) Uani 1 1 d . . .
C4 C -0.09238(14) 0.85724(8) 1.03972(9) 0.0202(2) Uani 1 1 d . . .
H4A H -0.198(3) 0.8452(13) 1.0228(17) 0.059(6) Uiso 1 1 d . . .
H4B H -0.039(2) 0.8210(12) 1.0889(16) 0.050(5) Uiso 1 1 d . . .
H4C H -0.080(2) 0.9146(12) 1.0651(14) 0.046(5) Uiso 1 1 d . . .
C5 C 0.42041(12) 0.84589(6) 0.73151(8) 0.01375(19) Uani 1 1 d . . .
C6 C 0.58509(14) 0.94845(8) 0.65900(10) 0.0211(2) Uani 1 1 d . . .
H6A H 0.575(2) 0.9712(11) 0.5890(15) 0.040(5) Uiso 1 1 d . . .
H6B H 0.666(2) 0.9090(12) 0.6689(15) 0.046(5) Uiso 1 1 d . . .
H6C H 0.604(2) 0.9839(12) 0.7127(16) 0.051(5) Uiso 1 1 d . . .
O2 O 0.79041(12) 0.12887(6) 0.71859(8) 0.02725(19) Uani 1 1 d . . .
H2D H 0.712(3) 0.1400(12) 0.6795(17) 0.051(6) Uiso 1 1 d . . .
H2E H 0.844(2) 0.1702(13) 0.7195(15) 0.044(5) Uiso 1 1 d . . .


_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
K1 O1 2.7363(9) 3_667 ?
K1 O1 2.7487(8) . ?
K1 N2 2.9705(9) 4_676 ?
K1 N10 3.0700(9) 4_676 ?
K1 S2 3.2987(4) . ?
K1 S1 3.3437(3) . ?
K1 N11 3.4326(10) 2_546 ?
K1 K1 4.1116(5) 3_667 ?
K1 H1B 3.04(2) . ?
K1 H1 2.795(13) . ?
S1 C1 1.6746(11) . ?
S2 C3 1.6777(11) . ?
S3 C5 1.6814(11) . ?
O1 K1 2.7363(9) 3_667 ?
O1 H1A 0.829(19) . ?
O1 H1B 0.85(2) . ?
N1 C1 1.3621(13) . ?
N1 N2 1.3709(12) . ?
N1 B1 1.5370(14) . ?
N2 N3 1.2795(13) . ?
N2 K1 2.9705(9) 4_575 ?
N3 N4 1.3548(12) . ?
N4 C1 1.3571(13) . ?
N4 C2 1.4531(13) . ?
N5 C3 1.3547(13) . ?
N5 N6 1.3602(12) . ?
N5 B1 1.5544(14) . ?
N6 N7 1.2818(13) . ?
N7 N8 1.3544(12) . ?
N8 C3 1.3505(13) . ?
N8 C4 1.4533(14) . ?
N9 C5 1.3608(13) . ?
N9 N10 1.3670(12) . ?
N9 B1 1.5348(14) . ?
N10 N11 1.2823(13) . ?
N10 K1 3.0700(9) 4_575 ?
N11 N12 1.3526(12) . ?
N11 K1 3.4326(10) 2_556 ?
N12 C5 1.3481(13) . ?
N12 C6 1.4542(14) . ?
B1 H1 1.076(13) . ?
C2 H2A 0.933(16) . ?
C2 H2B 0.967(15) . ?
C2 H2C 0.957(15) . ?
C4 H4A 0.93(2) . ?
C4 H4B 0.91(2) . ?
C4 H4C 0.98(2) . ?
C6 H6A 0.956(19) . ?
C6 H6B 0.94(2) . ?
C6 H6C 0.88(2) . ?
O2 H2D 0.78(2) . ?
O2 H2E 0.81(2) . ?

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
O1 K1 O1 82.89(3) 3_667 . ?
O1 K1 N2 93.65(3) 3_667 4_676 ?
O1 K1 N2 136.44(3) . 4_676 ?
O1 K1 N10 66.64(3) 3_667 4_676 ?
O1 K1 N10 75.19(2) . 4_676 ?
N2 K1 N10 63.89(2) 4_676 4_676 ?
O1 K1 S2 107.650(19) 3_667 . ?
O1 K1 S2 148.11(2) . . ?
N2 K1 S2 74.136(19) 4_676 . ?
N10 K1 S2 136.698(18) 4_676 . ?
O1 K1 S1 122.02(2) 3_667 . ?
O1 K1 S1 71.722(19) . . ?
N2 K1 S1 139.77(2) 4_676 . ?
N10 K1 S1 143.841(19) 4_676 . ?
S2 K1 S1 77.389(8) . . ?
O1 K1 N11 63.18(2) 3_667 2_546 ?
O1 K1 N11 72.28(2) . 2_546 ?
N2 K1 N11 143.08(2) 4_676 2_546 ?
N10 K1 N11 122.33(2) 4_676 2_546 ?
S2 K1 N11 85.567(17) . 2_546 ?
S1 K1 N11 59.682(16) . 2_546 ?
O1 K1 K1 41.559(17) 3_667 3_667 ?
O1 K1 K1 41.330(18) . 3_667 ?
N2 K1 K1 121.80(2) 4_676 3_667 ?
N10 K1 K1 64.228(18) 4_676 3_667 ?
S2 K1 K1 140.302(11) . 3_667 ?
S1 K1 K1 98.234(9) . 3_667 ?
N11 K1 K1 59.751(16) 2_546 3_667 ?
O1 K1 H1B 95.0(4) 3_667 . ?
O1 K1 H1B 15.8(4) . . ?
N2 K1 H1B 125.7(4) 4_676 . ?
N10 K1 H1B 71.0(4) 4_676 . ?
S2 K1 H1B 149.4(4) . . ?
S1 K1 H1B 73.2(4) . . ?
N11 K1 H1B 86.7(4) 2_546 . ?
K1 K1 H1B 54.2(4) 3_667 . ?
O1 K1 H1 167.3(3) 3_667 . ?
O1 K1 H1 106.4(3) . . ?
N2 K1 H1 85.4(3) 4_676 . ?
N10 K1 H1 123.5(3) 4_676 . ?
S2 K1 H1 59.9(3) . . ?
S1 K1 H1 55.6(3) . . ?
N11 K1 H1 110.9(3) 2_546 . ?
K1 K1 H1 147.0(3) 3_667 . ?
H1B K1 H1 95.7(5) . . ?
C1 S1 K1 112.32(4) . . ?
C3 S2 K1 107.47(4) . . ?
K1 O1 K1 97.11(3) 3_667 . ?
K1 O1 H1A 103.9(13) 3_667 . ?
K1 O1 H1A 113.0(12) . . ?
K1 O1 H1B 135.9(14) 3_667 . ?
K1 O1 H1B 102.1(14) . . ?
H1A O1 H1B 104.4(18) . . ?
C1 N1 N2 109.60(8) . . ?
C1 N1 B1 127.15(9) . . ?
N2 N1 B1 122.26(8) . . ?
N3 N2 N1 108.64(8) . . ?
N3 N2 K1 107.49(6) . 4_575 ?
N1 N2 K1 129.67(6) . 4_575 ?
N2 N3 N4 107.60(8) . . ?
N3 N4 C1 111.22(8) . . ?
N3 N4 C2 119.96(9) . . ?
C1 N4 C2 128.69(9) . . ?
C3 N5 N6 109.42(8) . . ?
C3 N5 B1 125.99(9) . . ?
N6 N5 B1 124.38(8) . . ?
N7 N6 N5 108.84(8) . . ?
N6 N7 N8 107.38(8) . . ?
C3 N8 N7 110.75(8) . . ?
C3 N8 C4 127.88(9) . . ?
N7 N8 C4 121.33(9) . . ?
C5 N9 N10 109.41(8) . . ?
C5 N9 B1 126.51(9) . . ?
N10 N9 B1 124.00(8) . . ?
N11 N10 N9 108.61(8) . . ?
N11 N10 K1 115.58(6) . 4_575 ?
N9 N10 K1 135.80(6) . 4_575 ?
N10 N11 N12 107.43(8) . . ?
N10 N11 K1 102.64(6) . 2_556 ?
N12 N11 K1 127.65(6) . 2_556 ?
C5 N12 N11 111.28(8) . . ?
C5 N12 C6 127.50(10) . . ?
N11 N12 C6 121.19(9) . . ?
N9 B1 N1 112.44(8) . . ?
N9 B1 N5 109.29(8) . . ?
N1 B1 N5 108.40(8) . . ?
N9 B1 H1 109.8(7) . . ?
N1 B1 H1 108.3(7) . . ?
N5 B1 H1 108.6(7) . . ?
N4 C1 N1 102.95(8) . . ?
N4 C1 S1 127.17(8) . . ?
N1 C1 S1 129.87(8) . . ?
N4 C2 H2A 109.9(9) . . ?
N4 C2 H2B 107.5(9) . . ?
H2A C2 H2B 109.7(13) . . ?
N4 C2 H2C 107.5(8) . . ?
H2A C2 H2C 109.7(13) . . ?
H2B C2 H2C 112.5(12) . . ?
N8 C3 N5 103.59(9) . . ?
N8 C3 S2 127.19(8) . . ?
N5 C3 S2 129.21(8) . . ?
N8 C4 H4A 111.1(13) . . ?
N8 C4 H4B 107.7(12) . . ?
H4A C4 H4B 111.2(18) . . ?
N8 C4 H4C 106.9(11) . . ?
H4A C4 H4C 108.0(16) . . ?
H4B C4 H4C 111.9(16) . . ?
N12 C5 N9 103.26(9) . . ?
N12 C5 S3 126.90(8) . . ?
N9 C5 S3 129.84(8) . . ?
N12 C6 H6A 108.0(11) . . ?
N12 C6 H6B 107.4(12) . . ?
H6A C6 H6B 107.0(15) . . ?
N12 C6 H6C 108.4(13) . . ?
H6A C6 H6C 116.6(16) . . ?
H6B C6 H6C 109.1(17) . . ?
H2D O2 H2E 105(2) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.055
_database_code_depnum_ccdc_archive 'CCDC 981805'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound2b

_audit_creation_date             2013-09-24
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C4 H8 B N8 S2, K'
_chemical_formula_sum            'C4 H8 B K N8 S2'
_chemical_formula_weight         282.21
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C6 H10 N12 K S3'
_chemical_oxdiff_usercomment     'Vers.Nr. 253'
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y, -z+1/2'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z-1/2'
'x, -y-1/2, z-1/2'

_cell_length_a                   7.23114(12)
_cell_length_b                   17.5695(3)
_cell_length_c                   8.60830(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1093.67(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    26421
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      32.6700
_cell_measurement_theta_min      4.3050
_exptl_absorpt_coefficient_mu    0.852
_exptl_absorpt_correction_T_max  1.045
_exptl_absorpt_correction_T_min  0.935
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.1311
_exptl_crystal_size_mid          0.0492
_exptl_crystal_size_min          0.0459
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0083
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            59018
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.022
_diffrn_reflns_theta_min         3.046
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 5.3114
_diffrn_measured_fraction_theta_full 0.9973
_diffrn_measured_fraction_theta_max 0.9973
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -84.00    8.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235  -57.0000  120.0000 92

#__ type_ start__ end____ width___ exp.time_
  2 omega  -90.00  -63.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235  153.0000 -119.5911 27

#__ type_ start__ end____ width___ exp.time_
  3 omega  -75.00  -39.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235  131.0000   29.0897 36

#__ type_ start__ end____ width___ exp.time_
  4 omega  -59.00   33.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5485  -19.0000   60.0000 92

#__ type_ start__ end____ width___ exp.time_
  5 omega    1.00   86.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5485   38.0000   30.0000 85

#__ type_ start__ end____ width___ exp.time_
  6 omega   -2.00   77.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5485   38.0000  -60.0000 79

#__ type_ start__ end____ width___ exp.time_
  7 omega  -51.00   40.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5485  -57.0000  -90.0000 91

#__ type_ start__ end____ width___ exp.time_
  8 omega  -12.00   56.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5485  -99.0000 -150.0000 68

#__ type_ start__ end____ width___ exp.time_
  9 omega  -38.00   37.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5485  -38.0000  -30.0000 75

#__ type_ start__ end____ width___ exp.time_
 10 omega   -9.00   83.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5485   77.0000   60.0000 92

#__ type_ start__ end____ width___ exp.time_
 11 omega  -88.00   13.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235  -77.0000    0.0000 101

#__ type_ start__ end____ width___ exp.time_
 12 omega  -75.00  -27.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235  131.0000 -171.7148 48

#__ type_ start__ end____ width___ exp.time_
 13 omega  -88.00    4.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235  -38.0000 -150.0000 92

#__ type_ start__ end____ width___ exp.time_
 14 omega -101.00  -55.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235  178.0000   30.0000 46

#__ type_ start__ end____ width___ exp.time_
 15 omega  -16.00   95.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5485   19.0000 -150.0000 111

#__ type_ start__ end____ width___ exp.time_
 16 omega   35.00  101.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5485  178.0000  -90.0000 66

#__ type_ start__ end____ width___ exp.time_
 17 omega  -20.00   56.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5485  -99.0000   30.0000 76

#__ type_ start__ end____ width___ exp.time_
 18 omega  -53.00   38.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5485  -38.0000 -150.0000 91

#__ type_ start__ end____ width___ exp.time_
 19 omega  -91.00  -40.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235  156.0000   93.6202 51

#__ type_ start__ end____ width___ exp.time_
 20 omega  -74.00  -27.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235  130.0000  -26.7999 47

#__ type_ start__ end____ width___ exp.time_
 21 omega  -38.00   54.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235   38.0000   90.0000 92

#__ type_ start__ end____ width___ exp.time_
 22 omega  -86.00  -35.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235  148.0000  -88.7192 51

#__ type_ start__ end____ width___ exp.time_
 23 omega  -85.00    8.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235  -57.0000   30.0000 93

#__ type_ start__ end____ width___ exp.time_
 24 omega  -75.00  -27.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235  131.0000   29.0897 48

#__ type_ start__ end____ width___ exp.time_
 25 omega  -13.00   89.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5485   77.0000    0.0000 102

#__ type_ start__ end____ width___ exp.time_
 26 omega  -54.00   48.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5485  -77.0000 -180.0000 102

#__ type_ start__ end____ width___ exp.time_
 27 omega  -90.00  -61.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235  153.0000  -17.7573 29
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0802645000
_diffrn_orient_matrix_UB_12      -0.0231811000
_diffrn_orient_matrix_UB_13      0.0020245000
_diffrn_orient_matrix_UB_21      0.0302868000
_diffrn_orient_matrix_UB_22      -0.0161976000
_diffrn_orient_matrix_UB_23      0.0710904000
_diffrn_orient_matrix_UB_31      -0.0475727000
_diffrn_orient_matrix_UB_32      0.0288088000
_diffrn_orient_matrix_UB_33      0.0416054000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1560
_reflns_number_total             1592
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'J. Appl. Cryst. (2007) 40, 786-790'
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.197
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.208
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         1592
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0264
_refine_ls_restrained_S_all      1.208
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0137P)²+1.0286P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0588
_refine_special_details          
;
 Disorder of the ligand, except the boron, on two positions (93:7)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.7500 0.2500 0.04502(5) 0.01416(9) Uani 1 2 d S T P . .
S1A S 0.55172(4) 0.36909(2) 0.28967(4) 0.01303(9) Uani 0.9343(9) 1 d . . P A 1
N1A N 0.20321(17) 0.31910(6) 0.20708(13) 0.0107(2) Uani 0.9343(9) 1 d . . P A 1
N2A N 0.02414(16) 0.33871(7) 0.23831(14) 0.0130(2) Uani 0.9343(9) 1 d . . P A 1
N3A N 0.02354(16) 0.39526(7) 0.33304(14) 0.0142(2) Uani 0.9343(9) 1 d . . P A 1
N4A N 0.20247(18) 0.41224(6) 0.36533(14) 0.0120(2) Uani 0.9343(9) 1 d . . P A 1
C1A C 0.31881(18) 0.36545(7) 0.28693(15) 0.0107(2) Uani 0.9343(9) 1 d . . P A 1
C2A C 0.2513(6) 0.47409(12) 0.4689(4) 0.0147(4) Uani 0.9343(9) 1 d . . P A 1
H2AA H 0.1535 0.4818 0.5426 0.022 Uiso 0.9343(9) 1 calc R U P A 1
H2AB H 0.2694 0.5198 0.4097 0.022 Uiso 0.9343(9) 1 calc R U P A 1
H2AC H 0.3633 0.4616 0.5231 0.022 Uiso 0.9343(9) 1 calc R U P A 1
S1B S -0.0506(7) 0.3694(3) 0.2872(6) 0.01303(9) Uani 0.0657(9) 1 d . . P A 2
N1B N 0.298(3) 0.3227(9) 0.2099(19) 0.0107(2) Uani 0.0657(9) 1 d . . P A 2
N2B N 0.476(2) 0.3403(10) 0.238(2) 0.0130(2) Uani 0.0657(9) 1 d . . P A 2
N3B N 0.469(2) 0.3985(10) 0.335(2) 0.0142(2) Uani 0.0657(9) 1 d . . P A 2
N4B N 0.293(3) 0.4098(10) 0.360(2) 0.0120(2) Uani 0.0657(9) 1 d . . P A 2
C1B C 0.184(3) 0.3664(10) 0.286(2) 0.0107(2) Uani 0.0657(9) 1 d . . P A 2
C2B C 0.255(10) 0.487(3) 0.457(7) 0.0147(4) Uani 0.0657(9) 1 d . . P A 2
H2BA H 0.3666 0.5163 0.4623 0.022 Uiso 0.0657(9) 1 calc R U P A 2
H2BB H 0.2152 0.4740 0.5600 0.022 Uiso 0.0657(9) 1 calc R U P A 2
H2BC H 0.1604 0.5159 0.4059 0.022 Uiso 0.0657(9) 1 calc R U P A 2
B1 B 0.2500 0.2500 0.1008(2) 0.0113(3) Uani 1 2 d S T P . .
H1 H 0.376(3) 0.2620(10) 0.030(2) 0.025(5) Uiso 1 1 d . . . . .


_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
K1 S1A 3.2968(4) 2_655 ?
K1 S1A 3.2968(4) . ?
K1 S1A 3.3563(4) 8_565 ?
K1 S1A 3.3563(4) 7_755 ?
K1 N2A 3.0212(12) 2 ?
K1 N2A 3.0212(12) 1_655 ?
K1 S1B 3.377(5) 8_665 ?
K1 S1B 3.377(5) 7_655 ?
K1 S1B 3.290(5) 1_655 ?
K1 S1B 3.290(5) 2 ?
K1 N2B 3.033(16) 2_655 ?
K1 N2B 3.033(16) . ?
K1 H1 2.714(19) . ?
S1A K1 3.3564(4) 7_756 ?
S1A C1A 1.6856(14) . ?
N1A N2A 1.3666(16) . ?
N1A C1A 1.3544(17) . ?
N1A B1 1.5576(16) . ?
N2A K1 3.0212(12) 1_455 ?
N2A N3A 1.2853(17) . ?
N3A N4A 1.3566(17) . ?
N4A C1A 1.3560(17) . ?
N4A C2A 1.450(4) . ?
C2A H2AA 0.9600 . ?
C2A H2AB 0.9600 . ?
C2A H2AC 0.9600 . ?
S1B K1 3.377(5) 7_656 ?
S1B K1 3.290(5) 1_455 ?
S1B C1B 1.70(2) . ?
N1B N2B 1.35(2) . ?
N1B C1B 1.30(2) . ?
N1B B1 1.623(17) . ?
N2B N3B 1.32(2) . ?
N3B N4B 1.31(3) . ?
N4B C1B 1.27(3) . ?
N4B C2B 1.61(6) . ?
C2B H2BA 0.9600 . ?
C2B H2BB 0.9600 . ?
C2B H2BC 0.9600 . ?
B1 N1A 1.5576(16) 2 ?
B1 N1B 1.623(17) 2 ?
B1 H1 1.116(18) . ?

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
S1A K1 S1A 128.918(11) . 8_565 ?
S1A K1 S1A 102.037(10) 2_655 8_565 ?
S1A K1 S1A 100.592(16) 2_655 . ?
S1A K1 S1A 98.175(15) 8_565 7_755 ?
S1A K1 S1A 102.036(10) . 7_755 ?
S1A K1 S1A 128.918(11) 2_655 7_755 ?
S1A K1 H1 110.3(4) 7_755 . ?
S1A K1 H1 65.9(4) 8_565 . ?
S1A K1 H1 63.1(4) . . ?
S1A K1 H1 120.8(4) 2_655 . ?
N2A K1 S1A 76.04(2) 2 8_565 ?
N2A K1 S1A 164.28(2) 2 7_755 ?
N2A K1 S1A 76.04(2) 1_655 7_755 ?
N2A K1 S1A 71.95(2) 1_655 2_655 ?
N2A K1 S1A 66.80(2) 2 2_655 ?
N2A K1 S1A 66.80(2) 1_655 . ?
N2A K1 S1A 164.28(2) 1_655 8_565 ?
N2A K1 S1A 71.95(2) 2 . ?
N2A K1 N2A 113.16(5) 1_655 2 ?
N2A K1 H1 54.0(4) 2 . ?
N2A K1 H1 129.7(4) 1_655 . ?
S1B K1 S1B 101.97(15) 2 8_665 ?
S1B K1 S1B 101.97(15) 1_655 7_655 ?
S1B K1 S1B 128.71(16) 1_655 8_665 ?
S1B K1 S1B 97.84(19) 8_665 7_655 ?
S1B K1 S1B 101.36(17) 1_655 2 ?
S1B K1 S1B 128.71(16) 2 7_655 ?
S1B K1 H1 116.3(4) 8_665 . ?
S1B K1 H1 59.7(4) 7_655 . ?
S1B K1 H1 69.1(4) 2 . ?
S1B K1 H1 114.6(4) 1_655 . ?
N2B K1 S1B 75.9(3) 2_655 8_665 ?
N2B K1 S1B 72.6(3) . 2 ?
N2B K1 S1B 66.8(4) 2_655 2 ?
N2B K1 S1B 66.8(4) . 1_655 ?
N2B K1 S1B 72.6(3) 2_655 1_655 ?
N2B K1 S1B 75.9(3) . 7_655 ?
N2B K1 S1B 164.5(4) 2_655 7_655 ?
N2B K1 S1B 164.5(4) . 8_665 ?
N2B K1 N2B 113.5(6) 2_655 . ?
N2B K1 H1 48.3(5) . . ?
N2B K1 H1 135.8(5) 2_655 . ?
K1 S1A K1 80.616(7) . 7_756 ?
C1A S1A K1 114.35(5) . 7_756 ?
C1A S1A K1 113.67(5) . . ?
N2A N1A B1 121.20(9) . . ?
C1A N1A N2A 109.47(11) . . ?
C1A N1A B1 129.26(10) . . ?
N1A N2A K1 112.54(8) . 1_455 ?
N3A N2A K1 138.24(9) . 1_455 ?
N3A N2A N1A 108.84(11) . . ?
N2A N3A N4A 107.26(11) . . ?
N3A N4A C2A 121.55(19) . . ?
C1A N4A N3A 110.88(11) . . ?
C1A N4A C2A 127.6(2) . . ?
N1A C1A S1A 130.28(10) . . ?
N1A C1A N4A 103.54(11) . . ?
N4A C1A S1A 126.15(10) . . ?
N4A C2A H2AA 109.5 . . ?
N4A C2A H2AB 109.5 . . ?
N4A C2A H2AC 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
K1 S1B K1 80.40(11) 1_455 7_656 ?
C1B S1B K1 114.4(7) . 1_455 ?
C1B S1B K1 114.3(6) . 7_656 ?
N2B N1B B1 119.4(14) . . ?
C1B N1B N2B 112.4(16) . . ?
C1B N1B B1 128.2(16) . . ?
N1B N2B K1 113.9(12) . . ?
N3B N2B K1 140.9(13) . . ?
N3B N2B N1B 104.8(15) . . ?
N4B N3B N2B 105.1(16) . . ?
N3B N4B C2B 112(3) . . ?
C1B N4B N3B 115.6(18) . . ?
C1B N4B C2B 131(3) . . ?
N1B C1B S1B 130.9(16) . . ?
N4B C1B S1B 127.0(16) . . ?
N4B C1B N1B 102.1(18) . . ?
N4B C2B H2BA 109.5 . . ?
N4B C2B H2BB 109.5 . . ?
N4B C2B H2BC 109.5 . . ?
H2BA C2B H2BB 109.5 . . ?
H2BA C2B H2BC 109.5 . . ?
H2BB C2B H2BC 109.5 . . ?
N1A B1 N1A 108.02(14) 2 . ?
N1A B1 H1 110.5(9) . . ?
N1A B1 H1 106.8(9) 2 . ?
N1B B1 N1B 109.2(12) 2 . ?
N1B B1 H1 89.5(11) . . ?
N1B B1 H1 129.7(11) 2 . ?

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
C2B H2BA S1B 0.96 3.00 3.57(5) 119.6 3_565
C2B H2BA N3B 0.96 2.59 3.36(7) 136.9 5_666

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
K1 S1A C1A N1A -86.25(13) 7_756 . . . ?
K1 S1A C1A N1A 3.92(14) . . . . ?
K1 S1A C1A N4A 95.75(12) 7_756 . . . ?
K1 S1A C1A N4A -174.07(10) . . . . ?
K1 N2A N3A N4A -172.64(9) 1_455 . . . ?
K1 S1B C1B N1B -3(2) 1_455 . . . ?
K1 S1B C1B N1B 87.1(19) 7_656 . . . ?
K1 S1B C1B N4B -94.9(18) 7_656 . . . ?
K1 S1B C1B N4B 174.9(16) 1_455 . . . ?
K1 N2B N3B N4B 173.3(14) . . . . ?
N1A N2A N3A N4A -0.65(14) . . . . ?
N2A N1A C1A S1A -178.22(10) . . . . ?
N2A N1A C1A N4A 0.12(14) . . . . ?
N2A N1A B1 N1A -98.95(11) . . . 2 ?
N2A N1A B1 N1B 178.8(14) . . . . ?
N2A N1A B1 N1B -73.6(7) . . . 2 ?
N2A N3A N4A C1A 0.75(15) . . . . ?
N2A N3A N4A C2A 179.67(15) . . . . ?
N3A N4A C1A S1A 177.91(10) . . . . ?
N3A N4A C1A N1A -0.52(14) . . . . ?
C1A N1A N2A K1 174.57(8) . . . 1_455 ?
C1A N1A N2A N3A 0.34(15) . . . . ?
C1A N1A B1 N1A 77.50(12) . . . 2 ?
C1A N1A B1 N1B 102.9(7) . . . 2 ?
C1A N1A B1 N1B -4.7(14) . . . . ?
C2A N4A C1A S1A -0.9(2) . . . . ?
C2A N4A C1A N1A -179.36(16) . . . . ?
N1B N2B N3B N4B 2(2) . . . . ?
N2B N1B C1B S1B 178.1(15) . . . . ?
N2B N1B C1B N4B 0(2) . . . . ?
N2B N1B B1 N1A 73.2(15) . . . 2 ?
N2B N1B B1 N1A 178(3) . . . . ?
N2B N1B B1 N1B 98.4(15) . . . 2 ?
N2B N3B N4B C1B -2(2) . . . . ?
N2B N3B N4B C2B -172(2) . . . . ?
N3B N4B C1B S1B -176.9(15) . . . . ?
N3B N4B C1B N1B 2(2) . . . . ?
C1B N1B N2B K1 -175.1(12) . . . . ?
C1B N1B N2B N3B -1(2) . . . . ?
C1B N1B B1 N1A -102.2(17) . . . 2 ?
C1B N1B B1 N1A 2.5(10) . . . . ?
C1B N1B B1 N1B -77.0(17) . . . 2 ?
C2B N4B C1B S1B -10(4) . . . . ?
C2B N4B C1B N1B 169(3) . . . . ?
B1 N1A N2A K1 -8.35(14) . . . 1_455 ?
B1 N1A N2A N3A 177.42(11) . . . . ?
B1 N1A C1A S1A 5.0(2) . . . . ?
B1 N1A C1A N4A -176.66(12) . . . . ?
B1 N1B N2B K1 8.7(18) . . . . ?
B1 N1B N2B N3B -177.1(13) . . . . ?
B1 N1B C1B S1B -6(3) . . . . ?
B1 N1B C1B N4B 175.4(14) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 0 1 0.0655 0.0003 -0.0019 0.9992 0.0020 0.0711 0.0415
0 -1 0 0.0229 -0.0003 -0.9992 -0.0008 0.0232 0.0161 -0.0288
0 1 0 0.0229 0.0003 0.9992 0.0008 -0.0232 -0.0161 0.0288
0 0 -1 0.0655 -0.0003 0.0019 -0.9992 -0.0020 -0.0711 -0.0415
1 0 0 0.0246 0.9993 0.0002 -0.0006 -0.0802 0.0302 -0.0476
-1 0 0 0.0246 -0.9993 -0.0002 0.0006 0.0802 -0.0302 0.0476

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-2
_database_code_depnum_ccdc_archive 'CCDC 981806'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H16 B N8 Na O2 S2'
_chemical_formula_sum            'C14 H16 B N8 Na O2 S2'
_chemical_formula_weight         426.27

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   7.1466(2)
_cell_length_b                   6.1686(2)
_cell_length_c                   43.2407(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.3920(10)
_cell_angle_gamma                90.00
_cell_volume                     1904.58(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9948
_cell_measurement_theta_min      6.137
_cell_measurement_theta_max      143.679

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             880
_exptl_absorpt_coefficient_mu    3.021
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5334
_exptl_absorpt_correction_T_max  0.7685
_exptl_absorpt_process_details   
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'


_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'I\mS Incoatec Microfocus'
_diffrn_radiation_monochromator  'Quazar Montel multilayer optic Montel200'
_diffrn_measurement_device_type  'Bruker AXS X8 Prospector Ultra with APEX II'
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12737
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_theta_min         2.05
_diffrn_reflns_theta_max         71.84
_reflns_number_total             3598
_reflns_number_gt                3580
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX 2, Bruker AXS'
_computing_cell_refinement       'APEX 2, Bruker AXS'
_computing_data_reduction        'APEX 2, Bruker AXS'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-PLUS (1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
; 
 H atoms at oxygen were refined with Ueq=1.5 of the U(eq) value of 
 corresponding atom. All O-H distances were restrained to have a 
 value of 0.84 Ang.


 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0000P)²+5.2560P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3598
_refine_ls_number_parameters     265
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0507
_refine_ls_wR_factor_ref         0.1155
_refine_ls_wR_factor_gt          0.1154
_refine_ls_goodness_of_fit_ref   1.286
_refine_ls_restrained_S_all      1.288
_refine_ls_shift/su_max          0.001
_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
Na1 Na 0.72619(16) 0.3077(2) 0.37552(3) 0.0198(3) Uani 1 1 d . . .
S1 S 0.49936(9) 0.62753(12) 0.334052(16) 0.01715(17) Uani 1 1 d . . .
S2 S -0.05994(10) 0.54824(13) 0.423918(16) 0.01907(18) Uani 1 1 d . . .
N1 N 0.1553(3) 0.4748(4) 0.34979(5) 0.0145(5) Uani 1 1 d . . .
N2 N -0.0286(3) 0.5193(4) 0.34301(5) 0.0172(5) Uani 1 1 d . . .
N3 N -0.0413(3) 0.6738(4) 0.32323(5) 0.0177(5) Uani 1 1 d . . .
N4 N 0.1376(3) 0.7326(4) 0.31694(5) 0.0158(5) Uani 1 1 d . . .
N5 N 0.2802(3) 0.4165(4) 0.40380(5) 0.0142(5) Uani 1 1 d . . .
N6 N 0.4654(3) 0.4413(4) 0.41238(6) 0.0168(5) Uani 1 1 d . . .
N7 N 0.4800(3) 0.5669(4) 0.43597(5) 0.0174(5) Uani 1 1 d . . .
N8 N 0.3022(3) 0.6285(4) 0.44280(5) 0.0157(5) Uani 1 1 d . . .
O1 O 0.6582(4) 0.1345(4) 0.32493(6) 0.0321(6) Uani 1 1 d D . .
H1C H 0.564(5) 0.216(7) 0.3183(10) 0.048 Uiso 1 1 d D . .
H1D H 0.615(6) -0.003(4) 0.3227(10) 0.048 Uiso 1 1 d D . .
O2 O 0.6976(4) -0.0401(5) 0.39405(7) 0.0422(7) Uani 1 1 d . . .
H2A H 0.733(7) -0.028(9) 0.3732(12) 0.063 Uiso 1 1 d . . .
H2B H 0.788(7) -0.139(9) 0.4047(12) 0.063 Uiso 1 1 d . . .
B1 B 0.2165(4) 0.2933(5) 0.37379(7) 0.0152(6) Uani 1 1 d . . .
H1A H 0.1103 0.1955 0.3778 0.018 Uiso 1 1 calc R . .
H1B H 0.3208 0.2062 0.3660 0.018 Uiso 1 1 calc R . .
C1 C 0.2633(4) 0.6103(5) 0.33371(6) 0.0153(6) Uani 1 1 d . . .
C2 C 0.1719(4) 0.8959(5) 0.29414(6) 0.0149(6) Uani 1 1 d . . .
C3 C 0.0812(4) 1.0948(5) 0.29577(7) 0.0178(6) Uani 1 1 d . . .
H3 H -0.0011 1.1244 0.3119 0.021 Uiso 1 1 calc R . .
C4 C 0.1138(4) 1.2488(5) 0.27328(7) 0.0205(6) Uani 1 1 d . . .
H4 H 0.0532 1.3856 0.2740 0.025 Uiso 1 1 calc R . .
C5 C 0.2348(4) 1.2043(5) 0.24963(7) 0.0209(6) Uani 1 1 d . . .
H5 H 0.2587 1.3116 0.2345 0.025 Uiso 1 1 calc R . .
C6 C 0.3202(4) 1.0035(5) 0.24820(7) 0.0197(6) Uani 1 1 d . . .
H6 H 0.4006 0.9721 0.2318 0.024 Uiso 1 1 calc R . .
C7 C 0.2892(4) 0.8475(5) 0.27054(7) 0.0186(6) Uani 1 1 d . . .
H7 H 0.3477 0.7096 0.2696 0.022 Uiso 1 1 calc R . .
C8 C 0.1744(4) 0.5332(5) 0.42295(6) 0.0146(6) Uani 1 1 d . . .
C9 C 0.2722(4) 0.7835(5) 0.46677(6) 0.0164(6) Uani 1 1 d . . .
C10 C 0.3145(4) 0.7290(5) 0.49733(7) 0.0182(6) Uani 1 1 d . . .
H10 H 0.3558 0.5869 0.5027 0.022 Uiso 1 1 calc R . .
C11 C 0.2954(4) 0.8856(5) 0.52002(7) 0.0195(6) Uani 1 1 d . . .
H11 H 0.3257 0.8516 0.5411 0.023 Uiso 1 1 calc R . .
C12 C 0.2320(4) 1.0918(5) 0.51207(7) 0.0198(6) Uani 1 1 d . . .
H12 H 0.2205 1.1991 0.5276 0.024 Uiso 1 1 calc R . .
C13 C 0.1857(4) 1.1411(5) 0.48145(7) 0.0192(6) Uani 1 1 d . . .
H13 H 0.1390 1.2811 0.4762 0.023 Uiso 1 1 calc R . .
C14 C 0.2067(4) 0.9878(5) 0.45841(7) 0.0179(6) Uani 1 1 d . . .
H14 H 0.1768 1.0219 0.4373 0.021 Uiso 1 1 calc R . .


_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
Na1 O2 2.302(3) . ?
Na1 O1 2.465(3) . ?
Na1 N6 2.634(3) . ?
Na1 N2 2.637(3) 1_655 ?
Na1 S2 2.9411(14) 1_655 ?
Na1 S1 3.0811(14) . ?
Na1 H2A 2.07(6) . ?
S1 C1 1.690(3) . ?
S2 C8 1.680(3) . ?
S2 Na1 2.9411(14) 1_455 ?
N1 C1 1.351(4) . ?
N1 N2 1.362(3) . ?
N1 B1 1.576(4) . ?
N2 N3 1.281(4) . ?
N2 Na1 2.637(3) 1_455 ?
N3 N4 1.368(3) . ?
N4 C1 1.359(4) . ?
N4 C2 1.438(4) . ?
N5 C8 1.352(4) . ?
N5 N6 1.369(3) . ?
N5 B1 1.555(4) . ?
N6 N7 1.282(3) . ?
N7 N8 1.370(3) . ?
N8 C8 1.360(4) . ?
N8 C9 1.433(4) . ?
O1 H1C 0.876(19) . ?
O1 H1D 0.909(19) . ?
O2 H2A 0.95(5) . ?
O2 H2B 0.99(6) . ?
B1 H1A 0.9900 . ?
B1 H1B 0.9900 . ?
C2 C7 1.380(4) . ?
C2 C3 1.390(4) . ?
C3 C4 1.386(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.394(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.383(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.387(4) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C9 C10 1.385(4) . ?
C9 C14 1.387(4) . ?
C10 C11 1.387(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.389(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.385(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.387(4) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?

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
O2 Na1 O1 83.56(11) . . ?
O2 Na1 N6 90.34(11) . . ?
O1 Na1 N6 123.67(9) . . ?
O2 Na1 N2 135.82(11) . 1_655 ?
O1 Na1 N2 81.50(9) . 1_655 ?
N6 Na1 N2 132.07(9) . 1_655 ?
O2 Na1 S2 105.88(9) . 1_655 ?
O1 Na1 S2 158.06(8) . 1_655 ?
N6 Na1 S2 76.78(6) . 1_655 ?
N2 Na1 S2 78.03(6) 1_655 1_655 ?
O2 Na1 S1 138.34(9) . . ?
O1 Na1 S1 71.42(7) . . ?
N6 Na1 S1 77.49(6) . . ?
N2 Na1 S1 73.62(6) 1_655 . ?
S2 Na1 S1 109.65(4) 1_655 . ?
O2 Na1 H2A 24.3(14) . . ?
O1 Na1 H2A 61.9(14) . . ?
N6 Na1 H2A 111.1(15) . . ?
N2 Na1 H2A 116.8(15) 1_655 . ?
S2 Na1 H2A 121.7(14) 1_655 . ?
S1 Na1 H2A 128.6(14) . . ?
C1 S1 Na1 117.76(11) . . ?
C8 S2 Na1 116.33(10) . 1_455 ?
C1 N1 N2 109.4(2) . . ?
C1 N1 B1 129.0(2) . . ?
N2 N1 B1 121.6(2) . . ?
N3 N2 N1 109.5(2) . . ?
N3 N2 Na1 133.93(18) . 1_455 ?
N1 N2 Na1 116.22(17) . 1_455 ?
N2 N3 N4 106.8(2) . . ?
C1 N4 N3 110.4(2) . . ?
C1 N4 C2 128.8(2) . . ?
N3 N4 C2 120.6(2) . . ?
C8 N5 N6 109.5(2) . . ?
C8 N5 B1 128.3(2) . . ?
N6 N5 B1 121.8(2) . . ?
N7 N6 N5 109.2(2) . . ?
N7 N6 Na1 129.41(18) . . ?
N5 N6 Na1 120.11(17) . . ?
N6 N7 N8 107.1(2) . . ?
C8 N8 N7 110.4(2) . . ?
C8 N8 C9 128.9(2) . . ?
N7 N8 C9 120.6(2) . . ?
Na1 O1 H1C 99(3) . . ?
Na1 O1 H1D 124(3) . . ?
H1C O1 H1D 104(4) . . ?
Na1 O2 H2A 64(3) . . ?
Na1 O2 H2B 132(3) . . ?
H2A O2 H2B 107(4) . . ?
N5 B1 N1 105.4(2) . . ?
N5 B1 H1A 110.7 . . ?
N1 B1 H1A 110.7 . . ?
N5 B1 H1B 110.7 . . ?
N1 B1 H1B 110.7 . . ?
H1A B1 H1B 108.8 . . ?
N1 C1 N4 103.8(2) . . ?
N1 C1 S1 128.8(2) . . ?
N4 C1 S1 127.4(2) . . ?
C7 C2 C3 121.8(3) . . ?
C7 C2 N4 118.8(3) . . ?
C3 C2 N4 119.4(3) . . ?
C4 C3 C2 118.5(3) . . ?
C4 C3 H3 120.8 . . ?
C2 C3 H3 120.8 . . ?
C3 C4 C5 120.5(3) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C6 C5 C4 119.8(3) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C7 120.4(3) . . ?
C5 C6 H6 119.8 . . ?
C7 C6 H6 119.8 . . ?
C2 C7 C6 119.0(3) . . ?
C2 C7 H7 120.5 . . ?
C6 C7 H7 120.5 . . ?
N5 C8 N8 103.8(2) . . ?
N5 C8 S2 128.9(2) . . ?
N8 C8 S2 127.2(2) . . ?
C10 C9 C14 121.8(3) . . ?
C10 C9 N8 119.7(3) . . ?
C14 C9 N8 118.4(3) . . ?
C9 C10 C11 118.8(3) . . ?
C9 C10 H10 120.6 . . ?
C11 C10 H10 120.6 . . ?
C10 C11 C12 120.2(3) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C13 C12 C11 120.0(3) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 120.6(3) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 H13 119.7 . . ?
C13 C14 C9 118.5(3) . . ?
C13 C14 H14 120.7 . . ?
C9 C14 H14 120.7 . . ?

_diffrn_measured_fraction_theta_max 0.959
_diffrn_reflns_theta_full        71.84
_diffrn_measured_fraction_theta_full 0.959
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.075
_database_code_depnum_ccdc_archive 'CCDC 981807'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound5

_audit_creation_date             2013-08-01
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C14 H23 B2 Bi N24 O2 S6'
_chemical_formula_sum            'C14 H23 B2 Bi N24 O2 S6'
_chemical_formula_weight         982.52
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C8 H8 B Bi N12 o2 S3'
_chemical_oxdiff_usercomment     'V.Nr. 340 '
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'
B B 0.0013 0.0007 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.5137(3)
_cell_length_b                   11.80455(11)
_cell_length_c                   19.3087(2)
_cell_angle_alpha                90
_cell_angle_beta                 104.4135(14)
_cell_angle_gamma                90
_cell_volume                     3645.50(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    75298
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.4300
_cell_measurement_theta_min      3.2790
_exptl_absorpt_coefficient_mu    5.236
_exptl_absorpt_correction_T_max  1.267
_exptl_absorpt_correction_T_min  0.253
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.3357
_exptl_crystal_size_mid          0.2227
_exptl_crystal_size_min          0.0362
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            240962
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.86
_diffrn_reflns_theta_min         2.78
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 5.3114
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.9759
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -89.00  -64.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235  152.0000   34.4160 25

#__ type_ start__ end____ width___ exp.time_
  2 omega  -23.00   55.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235   19.0000   30.0000 78

#__ type_ start__ end____ width___ exp.time_
  3 omega   18.00   47.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5485   38.0000  -60.0000 29

#__ type_ start__ end____ width___ exp.time_
  4 omega  -11.00   86.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5485   77.0000   30.0000 97

#__ type_ start__ end____ width___ exp.time_
  5 omega   -4.00   86.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5485   57.0000  150.0000 90

#__ type_ start__ end____ width___ exp.time_
  6 omega   55.00   89.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5485   38.0000  -60.0000 34

#__ type_ start__ end____ width___ exp.time_
  7 omega    7.00   77.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5485 -133.0000  109.8304 70

#__ type_ start__ end____ width___ exp.time_
  8 omega  -50.00   37.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5485  -38.0000  120.0000 87

#__ type_ start__ end____ width___ exp.time_
  9 omega  -20.00   56.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5485  -99.0000 -120.0000 76

#__ type_ start__ end____ width___ exp.time_
 10 omega   -7.00   83.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5485   57.0000  -90.0000 90

#__ type_ start__ end____ width___ exp.time_
 11 omega   16.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5485 -153.0000   13.7306 75

#__ type_ start__ end____ width___ exp.time_
 12 omega  -74.00  -27.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235  130.0000  137.5764 47

#__ type_ start__ end____ width___ exp.time_
 13 omega  -85.00    8.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235  -57.0000 -180.0000 93

#__ type_ start__ end____ width___ exp.time_
 14 omega  -38.00   54.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235   38.0000  120.0000 92

#__ type_ start__ end____ width___ exp.time_
 15 omega  -71.00  -23.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235  125.0000  -58.6215 48

#__ type_ start__ end____ width___ exp.time_
 16 omega  -88.00   13.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235  -77.0000   60.0000 101

#__ type_ start__ end____ width___ exp.time_
 17 omega  -38.00   15.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235  -84.0000  -96.0000 53

#__ type_ start__ end____ width___ exp.time_
 18 omega   -3.00   89.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5485   38.0000   30.0000 92

#__ type_ start__ end____ width___ exp.time_
 19 omega   35.00  101.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5485  178.0000  -90.0000 66

#__ type_ start__ end____ width___ exp.time_
 20 omega  -51.00   43.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5485  -57.0000  -90.0000 94

#__ type_ start__ end____ width___ exp.time_
 21 omega  -94.00   16.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235  -19.0000  120.0000 110

#__ type_ start__ end____ width___ exp.time_
 22 omega  -75.00  -27.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235  131.0000  -25.8039 48

#__ type_ start__ end____ width___ exp.time_
 23 omega  -75.00  -27.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235  131.0000 -147.9806 48

#__ type_ start__ end____ width___ exp.time_
 24 omega  -86.00  -35.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235  148.0000   80.1268 51

#__ type_ start__ end____ width___ exp.time_
 25 omega  -88.00   13.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235  -77.0000   90.0000 101

#__ type_ start__ end____ width___ exp.time_
 26 omega  -88.00    4.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235  -38.0000  -90.0000 92

#__ type_ start__ end____ width___ exp.time_
 27 omega  -38.00   54.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235   38.0000  -90.0000 92

#__ type_ start__ end____ width___ exp.time_
 28 omega  -75.00  -27.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9235  131.0000 -164.5388 48

#__ type_ start__ end____ width___ exp.time_
 29 omega    7.00   77.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5485 -133.0000  109.8304 70

#__ type_ start__ end____ width___ exp.time_
 30 omega   16.00   41.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5485 -153.0000   13.7306 25
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0177721000
_diffrn_orient_matrix_UB_12      -0.0230153000
_diffrn_orient_matrix_UB_13      0.0267846000
_diffrn_orient_matrix_UB_21      -0.0403545000
_diffrn_orient_matrix_UB_22      0.0163125000
_diffrn_orient_matrix_UB_23      -0.0200968000
_diffrn_orient_matrix_UB_31      -0.0047129000
_diffrn_orient_matrix_UB_32      -0.0530589000
_diffrn_orient_matrix_UB_33      -0.0178131000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9338
_reflns_number_total             10616
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.97
_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         1.436
_refine_diff_density_min         -2.345
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         10616
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0311
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0394P)²+10.7679P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0829
_refine_special_details          
;
 0.5 H2O in the asymmetric unit was highly disordered and therefore treated with
 the SQUEEZE procedure of the Olex2 program (Dolomanov, O.V.; Bourhis, L.J.; 
 Gildea, R.J.; Howard, J.A.K.; Puschmann, H., 
 J. Appl. Cryst. (2009), 42, 339-341.)
 The sum formular and further calculations disregard this electron density.
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Bi1 Bi 0.28079(2) 0.40643(2) 0.10281(2) 0.02135(4) Uani 1 1 d . . . . .
S1 S 0.30657(6) 0.34424(8) -0.03674(5) 0.03108(19) Uani 1 1 d . . . . .
S2 S 0.43187(5) 0.30166(7) 0.16997(4) 0.02383(16) Uani 1 1 d . . . . .
S3 S 0.19652(5) 0.18006(7) 0.09214(4) 0.02424(15) Uani 1 1 d . . . . .
S4 S 0.13753(6) 0.54533(8) 0.05219(5) 0.03229(19) Uani 1 1 d . . . . .
S5 S 0.23660(6) 0.37629(7) 0.23192(5) 0.02767(17) Uani 1 1 d . . . . .
S6 S -0.00692(11) 0.60155(15) 0.27900(14) 0.0833(6) Uani 1 1 d . . . . .
O1 O 0.37762(19) 0.5435(2) 0.06656(13) 0.0329(6) Uani 1 1 d . . . . .
O2 O 0.34567(17) 0.5639(2) 0.16952(13) 0.0285(5) Uani 1 1 d . . . . .
N1 N 0.3006(2) 0.1128(3) -0.01985(17) 0.0314(7) Uani 1 1 d . . . . .
N2 N 0.2477(3) 0.0251(3) -0.04697(19) 0.0434(9) Uani 1 1 d . . . . .
N3 N 0.1829(3) 0.0671(4) -0.0913(2) 0.0493(10) Uani 1 1 d . . . . .
N4 N 0.1935(2) 0.1805(4) -0.09342(17) 0.0419(9) Uani 1 1 d . . . . .
N5 N 0.44526(19) 0.1735(2) 0.05301(15) 0.0250(6) Uani 1 1 d . . . . .
N6 N 0.4944(2) 0.1721(3) 0.00595(16) 0.0280(6) Uani 1 1 d . . . . .
N7 N 0.5464(2) 0.2544(3) 0.02025(15) 0.0272(6) Uani 1 1 d . . . . .
N8 N 0.53098(19) 0.3109(2) 0.07656(15) 0.0238(5) Uani 1 1 d . . . . .
N9 N 0.34766(19) 0.0668(2) 0.11255(16) 0.0257(6) Uani 1 1 d . . . . .
N10 N 0.4007(2) 0.0080(3) 0.16593(18) 0.0334(7) Uani 1 1 d . . . . .
N11 N 0.3694(2) 0.0054(3) 0.22045(18) 0.0337(7) Uani 1 1 d . . . . .
N12 N 0.2958(2) 0.0626(3) 0.20245(16) 0.0267(6) Uani 1 1 d . . . . .
N13 N 0.1878(2) 0.7077(3) 0.15880(19) 0.0350(7) Uani 1 1 d . . . . .
N14 N 0.2304(3) 0.8088(3) 0.1667(2) 0.0423(9) Uani 1 1 d . . . . .
N15 N 0.2477(3) 0.8329(3) 0.1072(2) 0.0421(8) Uani 1 1 d . . . . .
N16 N 0.2194(2) 0.7463(3) 0.06073(18) 0.0324(7) Uani 1 1 d . . . . .
N17 N 0.2450(3) 0.6011(3) 0.27385(18) 0.0382(8) Uani 1 1 d . . . . .
N18 N 0.3032(3) 0.6683(3) 0.3203(2) 0.0487(10) Uani 1 1 d . . . . .
N19 N 0.3664(3) 0.6096(4) 0.3500(2) 0.0476(10) Uani 1 1 d . . . . .
N20 N 0.3512(3) 0.5041(3) 0.32476(16) 0.0403(9) Uani 1 1 d . . . . .
N21 N 0.1276(3) 0.7303(3) 0.2667(2) 0.0461(9) Uani 1 1 d . . . . .
N22 N 0.1624(3) 0.8322(4) 0.2913(3) 0.0645(14) Uani 1 1 d . . . . .
N23 N 0.1157(3) 0.8819(4) 0.3274(3) 0.0574(11) Uani 1 1 d . . . . .
N24 N 0.0514(3) 0.8102(4) 0.3269(2) 0.0493(9) Uani 1 1 d . . . . .
C1 C 0.2671(2) 0.2104(4) -0.04864(18) 0.0313(8) Uani 1 1 d . . . . .
C2 C 0.1288(3) 0.2509(6) -0.1372(2) 0.0543(14) Uani 1 1 d . . . . .
H2A H 0.0804 0.2501 -0.1180 0.081 Uiso 1 1 calc R U . . .
H2B H 0.1140 0.2221 -0.1852 0.081 Uiso 1 1 calc R U . . .
H2C H 0.1490 0.3271 -0.1373 0.081 Uiso 1 1 calc R U . . .
C3 C 0.4684(2) 0.2612(3) 0.09833(17) 0.0222(6) Uani 1 1 d . . . . .
C4 C 0.5814(3) 0.4081(3) 0.1062(2) 0.0336(8) Uani 1 1 d . . . . .
H4A H 0.6330 0.3828 0.1373 0.050 Uiso 1 1 calc R U . . .
H4B H 0.5516 0.4537 0.1328 0.050 Uiso 1 1 calc R U . . .
H4C H 0.5931 0.4523 0.0681 0.050 Uiso 1 1 calc R U . . .
C5 C 0.2809(2) 0.1030(3) 0.13503(18) 0.0230(6) Uani 1 1 d . . . . .
C6 C 0.2437(3) 0.0699(4) 0.2528(2) 0.0341(8) Uani 1 1 d . . . . .
H6A H 0.1933 0.1102 0.2312 0.051 Uiso 1 1 calc R U . . .
H6B H 0.2735 0.1093 0.2950 0.051 Uiso 1 1 calc R U . . .
H6C H 0.2300 -0.0050 0.2655 0.051 Uiso 1 1 calc R U . . .
C7 C 0.1816(3) 0.6673(3) 0.0919(2) 0.0320(8) Uani 1 1 d . . . . .
C8 C 0.2312(3) 0.7473(4) -0.0120(2) 0.0383(9) Uani 1 1 d . . . . .
H8A H 0.2345 0.6708 -0.0280 0.057 Uiso 1 1 calc R U . . .
H8B H 0.2820 0.7867 -0.0122 0.057 Uiso 1 1 calc R U . . .
H8C H 0.1848 0.7850 -0.0434 0.057 Uiso 1 1 calc R U . . .
C9 C 0.2766(3) 0.4972(3) 0.27664(18) 0.0314(8) Uani 1 1 d . . . . .
C10 C 0.4148(3) 0.4155(4) 0.3456(2) 0.0437(11) Uani 1 1 d . . . . .
H10A H 0.3881 0.3446 0.3499 0.066 Uiso 1 1 calc R U . . .
H10B H 0.4520 0.4348 0.3907 0.066 Uiso 1 1 calc R U . . .
H10C H 0.4459 0.4092 0.3099 0.066 Uiso 1 1 calc R U . . .
C11 C 0.0568(3) 0.7143(4) 0.2903(3) 0.0475(11) Uani 1 1 d . . . . .
C12 C -0.0103(4) 0.8470(6) 0.3627(4) 0.0663(16) Uani 1 1 d . . . . .
H12A H -0.0035 0.8059 0.4067 0.099 Uiso 1 1 calc R U . . .
H12B H -0.0651 0.8331 0.3327 0.099 Uiso 1 1 calc R U . . .
H12C H -0.0036 0.9265 0.3728 0.099 Uiso 1 1 calc R U . . .
C13 C 0.3880(2) 0.5929(3) 0.12542(18) 0.0278(7) Uani 1 1 d . . . . .
C14 C 0.4511(3) 0.6868(4) 0.1470(2) 0.0390(9) Uani 1 1 d . . . . .
H14A H 0.4751 0.6836 0.1977 0.058 Uiso 1 1 calc R U . . .
H14B H 0.4240 0.7586 0.1349 0.058 Uiso 1 1 calc R U . . .
H14C H 0.4945 0.6781 0.1223 0.058 Uiso 1 1 calc R U . . .
B1 B 0.3762(3) 0.0811(3) 0.0427(2) 0.0285(8) Uani 1 1 d . . . . .
B2 B 0.1644(4) 0.6480(4) 0.2237(3) 0.0396(11) Uani 1 1 d . . . . .
H2 H 0.124(3) 0.586(4) 0.203(3) 0.031(12) Uiso 1 1 d . . . . .
H1 H 0.396(3) 0.004(4) 0.028(3) 0.041(13) Uiso 1 1 d . . . . .


_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 S1 2.9243(9) . ?
Bi1 S2 2.7973(9) . ?
Bi1 S3 2.9961(8) . ?
Bi1 S4 2.8441(10) . ?
Bi1 S5 2.7891(8) . ?
Bi1 O1 2.495(3) . ?
Bi1 O2 2.361(3) . ?
Bi1 C13 2.790(3) . ?
S1 C1 1.702(4) . ?
S2 C3 1.709(3) . ?
S3 C5 1.698(4) . ?
S4 C7 1.707(4) . ?
S5 C9 1.713(4) . ?
S6 C11 1.676(5) . ?
O1 C13 1.250(4) . ?
O2 C13 1.275(4) . ?
N1 N2 1.372(4) . ?
N1 C1 1.338(6) . ?
N1 B1 1.550(6) . ?
N2 N3 1.292(6) . ?
N3 N4 1.352(6) . ?
N4 C1 1.352(5) . ?
N4 C2 1.448(7) . ?
N5 N6 1.361(4) . ?
N5 C3 1.348(4) . ?
N5 B1 1.554(5) . ?
N6 N7 1.280(4) . ?
N7 N8 1.352(4) . ?
N8 C3 1.343(4) . ?
N8 C4 1.450(4) . ?
N9 N10 1.364(5) . ?
N9 C5 1.350(4) . ?
N9 B1 1.546(5) . ?
N10 N11 1.284(4) . ?
N11 N12 1.357(4) . ?
N12 C5 1.350(4) . ?
N12 C6 1.452(5) . ?
N13 N14 1.374(5) . ?
N13 C7 1.357(5) . ?
N13 B2 1.567(6) . ?
N14 N15 1.282(5) . ?
N15 N16 1.363(5) . ?
N16 C7 1.345(5) . ?
N16 C8 1.464(5) . ?
N17 N18 1.388(5) . ?
N17 C9 1.329(5) . ?
N17 B2 1.541(7) . ?
N18 N19 1.264(6) . ?
N19 N20 1.338(5) . ?
N20 C9 1.348(6) . ?
N20 C10 1.465(6) . ?
N21 N22 1.366(6) . ?
N21 C11 1.371(6) . ?
N21 B2 1.500(6) . ?
N22 N23 1.301(6) . ?
N23 N24 1.355(6) . ?
N24 C11 1.349(6) . ?
N24 C12 1.434(7) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.508(5) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
B1 H1 1.03(5) . ?
B2 H2 1.00(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
S1 Bi1 S3 83.36(2) . . ?
S2 Bi1 S1 89.92(3) . . ?
S2 Bi1 S3 89.02(2) . . ?
S2 Bi1 S4 169.66(3) . . ?
S4 Bi1 S1 97.33(3) . . ?
S4 Bi1 S3 99.10(3) . . ?
S5 Bi1 S1 157.22(3) . . ?
S5 Bi1 S2 86.03(3) . . ?
S5 Bi1 S3 74.17(2) . . ?
S5 Bi1 S4 90.02(3) . . ?
S5 Bi1 C13 104.93(8) . . ?
O1 Bi1 S1 69.75(6) . . ?
O1 Bi1 S2 81.77(7) . . ?
O1 Bi1 S3 151.46(6) . . ?
O1 Bi1 S4 93.78(7) . . ?
O1 Bi1 S5 131.46(6) . . ?
O1 Bi1 C13 26.63(9) . . ?
O2 Bi1 S1 123.36(6) . . ?
O2 Bi1 S2 82.17(7) . . ?
O2 Bi1 S3 151.58(6) . . ?
O2 Bi1 S4 87.67(7) . . ?
O2 Bi1 S5 78.28(6) . . ?
O2 Bi1 O1 53.62(8) . . ?
O2 Bi1 C13 27.07(9) . . ?
C13 Bi1 S1 96.32(8) . . ?
C13 Bi1 S2 79.53(8) . . ?
C13 Bi1 S3 168.55(8) . . ?
C13 Bi1 S4 92.30(8) . . ?
C1 S1 Bi1 102.62(11) . . ?
C3 S2 Bi1 101.67(12) . . ?
C5 S3 Bi1 97.66(11) . . ?
C7 S4 Bi1 96.15(14) . . ?
C9 S5 Bi1 100.97(12) . . ?
C13 O1 Bi1 90.0(2) . . ?
C13 O2 Bi1 95.5(2) . . ?
N2 N1 B1 115.4(3) . . ?
C1 N1 N2 109.4(3) . . ?
C1 N1 B1 134.5(3) . . ?
N3 N2 N1 107.9(4) . . ?
N2 N3 N4 107.9(3) . . ?
N3 N4 C2 120.2(4) . . ?
C1 N4 N3 110.0(4) . . ?
C1 N4 C2 129.7(4) . . ?
N6 N5 B1 116.5(3) . . ?
C3 N5 N6 108.8(3) . . ?
C3 N5 B1 134.7(3) . . ?
N7 N6 N5 109.0(3) . . ?
N6 N7 N8 107.3(3) . . ?
N7 N8 C4 120.2(3) . . ?
C3 N8 N7 110.4(3) . . ?
C3 N8 C4 129.3(3) . . ?
N10 N9 B1 115.9(3) . . ?
C5 N9 N10 109.9(3) . . ?
C5 N9 B1 134.2(3) . . ?
N11 N10 N9 108.5(3) . . ?
N10 N11 N12 107.2(3) . . ?
N11 N12 C6 120.0(3) . . ?
C5 N12 N11 111.0(3) . . ?
C5 N12 C6 129.0(3) . . ?
N14 N13 B2 121.6(3) . . ?
C7 N13 N14 109.0(3) . . ?
C7 N13 B2 128.9(3) . . ?
N15 N14 N13 108.4(3) . . ?
N14 N15 N16 107.9(3) . . ?
N15 N16 C8 121.3(3) . . ?
C7 N16 N15 110.3(3) . . ?
C7 N16 C8 128.4(3) . . ?
N18 N17 B2 123.5(4) . . ?
C9 N17 N18 107.4(4) . . ?
C9 N17 B2 128.8(3) . . ?
N19 N18 N17 109.9(4) . . ?
N18 N19 N20 106.6(4) . . ?
N19 N20 C9 111.3(4) . . ?
N19 N20 C10 120.5(4) . . ?
C9 N20 C10 128.0(4) . . ?
N22 N21 C11 109.0(4) . . ?
N22 N21 B2 124.8(4) . . ?
C11 N21 B2 126.2(4) . . ?
N23 N22 N21 109.3(4) . . ?
N22 N23 N24 106.4(4) . . ?
N23 N24 C12 117.2(5) . . ?
C11 N24 N23 112.0(4) . . ?
C11 N24 C12 130.8(5) . . ?
N1 C1 S1 129.7(3) . . ?
N1 C1 N4 104.7(4) . . ?
N4 C1 S1 125.6(4) . . ?
N4 C2 H2A 109.5 . . ?
N4 C2 H2B 109.5 . . ?
N4 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N5 C3 S2 129.8(3) . . ?
N8 C3 S2 125.8(3) . . ?
N8 C3 N5 104.4(3) . . ?
N8 C4 H4A 109.5 . . ?
N8 C4 H4B 109.5 . . ?
N8 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N9 C5 S3 130.5(3) . . ?
N9 C5 N12 103.4(3) . . ?
N12 C5 S3 126.1(3) . . ?
N12 C6 H6A 109.5 . . ?
N12 C6 H6B 109.5 . . ?
N12 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N13 C7 S4 130.3(3) . . ?
N16 C7 S4 125.3(3) . . ?
N16 C7 N13 104.4(3) . . ?
N16 C8 H8A 109.5 . . ?
N16 C8 H8B 109.5 . . ?
N16 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N17 C9 S5 130.5(3) . . ?
N17 C9 N20 104.7(3) . . ?
N20 C9 S5 124.7(3) . . ?
N20 C10 H10A 109.5 . . ?
N20 C10 H10B 109.5 . . ?
N20 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N21 C11 S6 128.8(4) . . ?
N24 C11 S6 127.9(4) . . ?
N24 C11 N21 103.3(4) . . ?
N24 C12 H12A 109.5 . . ?
N24 C12 H12B 109.5 . . ?
N24 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O1 C13 Bi1 63.41(18) . . ?
O1 C13 O2 120.5(3) . . ?
O1 C13 C14 121.5(3) . . ?
O2 C13 Bi1 57.39(17) . . ?
O2 C13 C14 117.9(3) . . ?
C14 C13 Bi1 172.5(3) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1 B1 N5 110.7(3) . . ?
N1 B1 H1 105(3) . . ?
N5 B1 H1 112(3) . . ?
N9 B1 N1 110.2(3) . . ?
N9 B1 N5 109.7(3) . . ?
N9 B1 H1 109(3) . . ?
N13 B2 H2 106(3) . . ?
N17 B2 N13 108.5(4) . . ?
N17 B2 H2 112(3) . . ?
N21 B2 N13 111.4(3) . . ?
N21 B2 N17 106.8(4) . . ?
N21 B2 H2 112(3) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 156.6 6.6 ?
2 0.000 0.500 0.500 156.6 6.6 ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1 0 0 0.0181 0.9998 -0.0001 -0.0001 -0.0178 -0.0403 -0.0047
-1 0 0 0.0181 -0.9998 0.0001 0.0001 0.0178 0.0403 0.0047
0 0 1 0.1034 -0.0009 -0.0002 1.0001 0.0268 -0.0201 -0.0178
0 0 -1 0.1034 0.0009 0.0002 -1.0001 -0.0268 0.0201 0.0178
0 -1 0 0.1679 -0.0000 -1.0001 0.0000 0.0230 -0.0163 0.0531
0 1 0 0.1679 0.0000 1.0001 -0.0000 -0.0230 0.0163 -0.0531
0 -1 -1 0.1542 0.0008 -0.9999 -1.0001 -0.0038 0.0038 0.0709

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-2
_database_code_depnum_ccdc_archive 'CCDC 981808'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound6a

_audit_creation_date             2013-11-22
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C28 H20 Bi2 N16 S4'
_chemical_formula_sum            'C30 H24 Bi2 N16 O0.50 S4'
_chemical_formula_weight         1162.85
_chemical_melting_point          ?
_chemical_oxdiff_formula         'c33 h10 i n2 s2 bi S2'
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'
Bi Bi -4.1077 10.2566 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.6264(3)
_cell_length_b                   6.72789(5)
_cell_length_c                   24.3264(2)
_cell_angle_alpha                90
_cell_angle_beta                 95.9510(8)
_cell_angle_gamma                90
_cell_volume                     3845.97(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    118225
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      31.9630
_cell_measurement_theta_min      3.1280
_exptl_absorpt_coefficient_mu    9.404
_exptl_absorpt_correction_T_max  0.668
_exptl_absorpt_correction_T_min  0.073
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.008
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.3625
_exptl_crystal_size_mid          0.1123
_exptl_crystal_size_min          0.0793
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.0125
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            241494
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.08
_diffrn_reflns_theta_min         2.53
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 8.0951
_diffrn_measured_fraction_theta_full 0.9990
_diffrn_measured_fraction_theta_max 0.9990
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   60.00   87.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421    0.0000   60.0000 27

#__ type_ start__ end____ width___ exp.time_
  2 omega  -46.00   78.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421    0.0000  -90.0000 124

#__ type_ start__ end____ width___ exp.time_
  3 omega  -41.00   47.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -38.0000 -150.0000 88

#__ type_ start__ end____ width___ exp.time_
  4 omega   -4.00   94.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   77.0000   60.0000 98

#__ type_ start__ end____ width___ exp.time_
  5 omega   -4.00   94.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   77.0000 -120.0000 98

#__ type_ start__ end____ width___ exp.time_
  6 omega   19.00   77.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421 -120.0000  -12.0000 58

#__ type_ start__ end____ width___ exp.time_
  7 omega    7.00   56.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   57.0000 -180.0000 49

#__ type_ start__ end____ width___ exp.time_
  8 omega    7.00   78.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   57.0000    0.0000 71

#__ type_ start__ end____ width___ exp.time_
  9 omega  -19.00   66.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -99.0000 -180.0000 85

#__ type_ start__ end____ width___ exp.time_
 10 omega    2.00   66.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -99.0000   60.0000 64

#__ type_ start__ end____ width___ exp.time_
 11 omega  -44.00   28.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421    0.0000   60.0000 72

#__ type_ start__ end____ width___ exp.time_
 12 omega  -94.00   -1.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000  -38.0000  -60.0000 93

#__ type_ start__ end____ width___ exp.time_
 13 omega  -52.00   46.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000   77.0000   60.0000 98

#__ type_ start__ end____ width___ exp.time_
 14 omega  -92.00   -5.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000  -57.0000   60.0000 87

#__ type_ start__ end____ width___ exp.time_
 15 omega  -42.00   45.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000   57.0000 -150.0000 87

#__ type_ start__ end____ width___ exp.time_
 16 omega  -93.00    5.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000  -77.0000 -180.0000 98

#__ type_ start__ end____ width___ exp.time_
 17 omega  -93.00    5.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000  -77.0000  -60.0000 98

#__ type_ start__ end____ width___ exp.time_
 18 omega   35.00   99.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  178.0000  150.0000 64

#__ type_ start__ end____ width___ exp.time_
 19 omega   -2.00   77.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421 -120.0000  -12.0000 79

#__ type_ start__ end____ width___ exp.time_
 20 omega   35.00   99.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  178.0000 -150.0000 64

#__ type_ start__ end____ width___ exp.time_
 21 omega  -97.00  -35.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000 -178.0000  150.0000 62

#__ type_ start__ end____ width___ exp.time_
 22 omega   -4.00   94.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   77.0000  -60.0000 98

#__ type_ start__ end____ width___ exp.time_
 23 omega   -4.00   94.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   77.0000 -150.0000 98

#__ type_ start__ end____ width___ exp.time_
 24 omega   35.00   99.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  178.0000   60.0000 64

#__ type_ start__ end____ width___ exp.time_
 25 omega  -20.00   66.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -99.0000 -150.0000 86

#__ type_ start__ end____ width___ exp.time_
 26 omega  -20.00   66.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -99.0000  120.0000 86

#__ type_ start__ end____ width___ exp.time_
 27 omega  -43.00   44.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -57.0000 -150.0000 87

#__ type_ start__ end____ width___ exp.time_
 28 omega    7.00   93.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   57.0000   30.0000 86

#__ type_ start__ end____ width___ exp.time_
 29 omega   -4.00   94.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   77.0000   90.0000 98

#__ type_ start__ end____ width___ exp.time_
 30 omega  -20.00   50.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -99.0000  -90.0000 70

#__ type_ start__ end____ width___ exp.time_
 31 omega  -46.00   47.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000   38.0000   60.0000 93

#__ type_ start__ end____ width___ exp.time_
 32 omega  -95.00   48.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000  150.0000 143

#__ type_ start__ end____ width___ exp.time_
 33 omega  -95.00   48.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000    0.0000 143

#__ type_ start__ end____ width___ exp.time_
 34 omega  -95.00   48.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000  -60.0000 143

#__ type_ start__ end____ width___ exp.time_
 35 omega  -95.00   48.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000  -90.0000 143

#__ type_ start__ end____ width___ exp.time_
 36 omega  -95.00   48.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000 -150.0000 143

#__ type_ start__ end____ width___ exp.time_
 37 omega  -95.00   48.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000 -120.0000 143

#__ type_ start__ end____ width___ exp.time_
 38 omega  -97.00  -35.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000 -178.0000 -120.0000 62

#__ type_ start__ end____ width___ exp.time_
 39 omega  -95.00   48.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000  -30.0000 143

#__ type_ start__ end____ width___ exp.time_
 40 omega  -61.00   49.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000   19.0000 -150.0000 110

#__ type_ start__ end____ width___ exp.time_
 41 omega  -95.00   48.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000 -180.0000 143

#__ type_ start__ end____ width___ exp.time_
 42 omega  -95.00   48.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000   30.0000 143

#__ type_ start__ end____ width___ exp.time_
 43 omega  -95.00   48.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000   60.0000 143

#__ type_ start__ end____ width___ exp.time_
 44 omega  -95.00   48.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000   90.0000 143

#__ type_ start__ end____ width___ exp.time_
 45 omega  -95.00   48.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000  120.0000 143

#__ type_ start__ end____ width___ exp.time_
 46 omega  -46.00   96.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8858    0.0000    0.0000 142

#__ type_ start__ end____ width___ exp.time_
 47 omega    6.00   93.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8858   57.0000   60.0000 87

#__ type_ start__ end____ width___ exp.time_
 48 omega  -46.00   96.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8858    0.0000  -60.0000 142

#__ type_ start__ end____ width___ exp.time_
 49 omega  -46.00   96.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8858    0.0000  -90.0000 142

#__ type_ start__ end____ width___ exp.time_
 50 omega  -46.00   96.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8858    0.0000 -120.0000 142

#__ type_ start__ end____ width___ exp.time_
 51 omega  -46.00   96.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8858    0.0000 -150.0000 142

#__ type_ start__ end____ width___ exp.time_
 52 omega  -46.00   96.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8858    0.0000  -30.0000 142

#__ type_ start__ end____ width___ exp.time_
 53 omega  -46.00   96.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8858    0.0000 -180.0000 142

#__ type_ start__ end____ width___ exp.time_
 54 omega    6.00   93.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8858   57.0000  -90.0000 87

#__ type_ start__ end____ width___ exp.time_
 55 omega  -46.00   96.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       24.8858    0.0000   30.0000 142
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0020492000
_diffrn_orient_matrix_UB_12      -0.0523440000
_diffrn_orient_matrix_UB_13      -0.0254396000
_diffrn_orient_matrix_UB_21      0.0045240000
_diffrn_orient_matrix_UB_22      0.0898686000
_diffrn_orient_matrix_UB_23      -0.0141480000
_diffrn_orient_matrix_UB_31      0.0297728000
_diffrn_orient_matrix_UB_32      -0.0172682000
_diffrn_orient_matrix_UB_33      0.0034650000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5377
_reflns_number_total             5650
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         2.757
_refine_diff_density_min         -1.684
_refine_diff_density_rms         0.174
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         5650
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0232
_refine_ls_restrained_S_all      1.191
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0278P)²+23.7280P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0604
_refine_special_details          
;
 A half THF on a two fold axes was highly disordered and therefore squeezed. 
 In the sum formular the solvent is included for further calculations.

mask.log:

Miller array info: D:/beendet/imran67b/struct/olex2_imran67b/imran67b.hkl:Iobs,
SigIobs
Observation type: xray.intensity
Type of data: double, size=241494
Type of sigmas: double, size=241494
Number of Miller indices: 241494
Anomalous flag: False
Unit cell: (23.6264, 6.72789, 24.3264, 90, 95.951, 90)
Space group: C 1 2/c 1 (No. 15)
Systematic absences: 8909
Systematic absences not included in following:
Centric reflections: 232585
Resolution range: 8.02306 0.709019

use_set_completion: False
solvent_radius: 1.20
shrink_truncation_radius: 1.20
van der Waals radii:
   Bi     C     H     N     S
 2.00  1.70  1.09  1.55  1.80

Total solvent accessible volume / cell = 676.2 Ang³ [17.6%]
Total electron count / cell = 66.4

gridding: (144,40,144)
Void #Grid points Vol/A³ Vol/%  Centre of mass (frac)   Eigenvectors (frac)
 1        34904   161.8   4.2  ( 0.000,-0.928, 0.250)  1  ( 0.794, 0.176, 0.582)
                                                       2  (-0.435,-0.504, 0.746)
                                                       3  (-0.425, 0.846, 0.324)
 2        34904   161.8   4.2  ( 0.000,-0.600, 0.750)  1  ( 0.764, 0.049, 0.644)
                                                       2  (-0.637,-0.104, 0.764)
                                                       3  (-0.105, 0.993, 0.048)
 3         1555     7.2   0.2  ( 0.000, 0.500,-0.000)  1  ( 0.000, 1.000, 0.000)
                                                       2  ( 0.754, 0.000, 0.657)
                                                       3  (-0.657, 0.000, 0.754)
 4         1555     7.2   0.2  ( 0.000, 0.500, 0.500)  1  ( 0.000, 1.000, 0.000)
                                                       2  ( 0.754, 0.000, 0.657)
                                                       3  (-0.657, 0.000, 0.754)
 5        34904   161.8   4.2  ( 0.500,-0.726, 0.250)  1  ( 0.842, 0.273, 0.465)
                                                       2  (-0.339,-0.403, 0.850)
                                                       3  (-0.420, 0.874, 0.246)
 6        34904   161.8   4.2  ( 0.500,-0.070, 0.750)  1  ( 0.779, 0.264, 0.568)
                                                       2  (-0.217,-0.737, 0.640)
                                                       3  (-0.588, 0.623, 0.517)
 7         1555     7.2   0.2  ( 0.500, 0.000, 0.000)  1  ( 0.000, 1.000, 0.000)
                                                       2  ( 0.754, 0.000, 0.657)
                                                       3  (-0.657, 0.000, 0.754)
 8         1555     7.2   0.2  ( 0.500,-0.000, 0.500)  1  ( 0.000, 1.000, 0.000)
                                                       2  ( 0.754, 0.000, 0.657)
                                                       3  (-0.657, 0.000, 0.754)

Void  Vol/Ang³  #Electrons
   1      161.8         16.3
   2      161.8         16.3
   3        7.2          0.3
   4        7.2          0.3
   5      161.8         16.3
   6      161.8         16.3
   7        7.2          0.3
   8        7.2          0.3
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Bi1 Bi 0.27409(2) 0.95937(2) 0.50341(2) 0.00991(4) Uani 1 1 d . . . . .
S1 S 0.37593(3) 0.86881(11) 0.47207(3) 0.01500(14) Uani 1 1 d . . . . .
N1 N 0.41281(12) 0.5104(4) 0.43619(12) 0.0141(5) Uani 1 1 d . . . . .
C1 C 0.37203(13) 0.6192(5) 0.45785(12) 0.0129(5) Uani 1 1 d . . . . .
C2 C 0.46853(13) 0.5648(5) 0.42316(13) 0.0145(5) Uani 1 1 d . . . . .
N7 N 0.34070(13) 0.9465(4) 0.63745(12) 0.0184(5) Uani 1 1 d . . . . .
N8 N 0.31038(11) 0.8239(4) 0.60064(11) 0.0140(5) Uani 1 1 d . . . . .
N5 N 0.32451(12) 0.6804(4) 0.68019(11) 0.0141(5) Uani 1 1 d . . . . .
N6 N 0.34932(13) 0.8645(4) 0.68508(12) 0.0191(5) Uani 1 1 d . . . . .
C9 C 0.32394(14) 0.5549(5) 0.72774(13) 0.0142(6) Uani 1 1 d . . . . .
C5 C 0.57776(15) 0.6692(6) 0.40434(14) 0.0217(7) Uani 1 1 d . . . . .
H5 H 0.6148 0.7058 0.3994 0.026 Uiso 1 1 calc R U . . .
C14 C 0.29997(14) 0.6286(5) 0.77333(13) 0.0182(6) Uani 1 1 d . . . . .
H14 H 0.2843 0.7555 0.7728 0.022 Uiso 1 1 calc R U . . .
C3 C 0.47829(15) 0.7521(5) 0.40248(16) 0.0214(7) Uani 1 1 d . . . . .
H3 H 0.4484 0.8410 0.3945 0.026 Uiso 1 1 calc R U . . .
C13 C 0.29988(16) 0.5082(6) 0.81992(14) 0.0214(7) Uani 1 1 d . . . . .
H13 H 0.2841 0.5549 0.8509 0.026 Uiso 1 1 calc R U . . .
C7 C 0.51180(14) 0.4256(5) 0.43255(13) 0.0173(6) Uani 1 1 d . . . . .
H7 H 0.5044 0.2992 0.4455 0.021 Uiso 1 1 calc R U . . .
C10 C 0.34730(15) 0.3658(5) 0.72733(13) 0.0196(6) Uani 1 1 d . . . . .
H10 H 0.3629 0.3187 0.6963 0.023 Uiso 1 1 calc R U . . .
C6 C 0.56663(15) 0.4796(6) 0.42211(14) 0.0214(7) Uani 1 1 d . . . . .
H6 H 0.5960 0.3872 0.4272 0.026 Uiso 1 1 calc R U . . .
C12 C 0.32316(16) 0.3196(5) 0.82031(14) 0.0220(7) Uani 1 1 d . . . . .
H12 H 0.3229 0.2402 0.8516 0.026 Uiso 1 1 calc R U . . .
C4 C 0.53396(16) 0.8047(6) 0.39389(17) 0.0255(7) Uani 1 1 d . . . . .
H4 H 0.5416 0.9312 0.3811 0.031 Uiso 1 1 calc R U . . .
C11 C 0.34688(16) 0.2478(5) 0.77438(14) 0.0223(7) Uani 1 1 d . . . . .
H11 H 0.3625 0.1209 0.7750 0.027 Uiso 1 1 calc R U . . .
S2 S 0.26292(4) 0.44962(11) 0.60337(3) 0.01489(14) Uani 1 1 d . . . . .
N4 N 0.32996(12) 0.4939(4) 0.46639(12) 0.0143(5) Uani 1 1 d . . . . .
N2 N 0.39556(12) 0.3168(4) 0.43231(12) 0.0172(5) Uani 1 1 d . . . . .
N3 N 0.34603(12) 0.3107(4) 0.45023(12) 0.0178(5) Uani 1 1 d . . . . .
C8 C 0.30028(13) 0.6562(4) 0.62757(12) 0.0123(5) Uani 1 1 d . . . . .


_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 Bi1 3.0367(2) 7_566 ?
Bi1 S1 2.6685(8) . ?
Bi1 N8 2.596(3) . ?
Bi1 S2 2.7232(8) 7_566 ?
Bi1 N4 2.657(3) 7_566 ?
S1 C1 1.715(3) . ?
N1 C1 1.359(4) . ?
N1 C2 1.433(4) . ?
N1 N2 1.365(4) . ?
C1 N4 1.336(4) . ?
C2 C3 1.385(4) . ?
C2 C7 1.388(4) . ?
N7 N8 1.365(4) . ?
N7 N6 1.280(4) . ?
N8 C8 1.338(4) . ?
N5 N6 1.370(4) . ?
N5 C9 1.434(4) . ?
N5 C8 1.357(4) . ?
C9 C14 1.388(4) . ?
C9 C10 1.387(5) . ?
C5 H5 0.9300 . ?
C5 C6 1.380(5) . ?
C5 C4 1.383(5) . ?
C14 H14 0.9300 . ?
C14 C13 1.393(5) . ?
C3 H3 0.9300 . ?
C3 C4 1.399(5) . ?
C13 H13 0.9300 . ?
C13 C12 1.383(5) . ?
C7 H7 0.9300 . ?
C7 C6 1.394(5) . ?
C10 H10 0.9300 . ?
C10 C11 1.394(4) . ?
C6 H6 0.9300 . ?
C12 H12 0.9300 . ?
C12 C11 1.387(5) . ?
C4 H4 0.9300 . ?
C11 H11 0.9300 . ?
S2 Bi1 2.7232(8) 7_566 ?
S2 C8 1.718(3) . ?
N4 Bi1 2.657(3) 7_566 ?
N4 N3 1.360(4) . ?
N2 N3 1.291(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
S1 Bi1 Bi1 96.698(17) . 7_566 ?
S1 Bi1 S2 89.36(3) . 7_566 ?
N8 Bi1 Bi1 79.07(6) . 7_566 ?
N8 Bi1 S1 87.58(6) . . ?
N8 Bi1 S2 172.32(6) . 7_566 ?
N8 Bi1 N4 90.98(9) . 7_566 ?
S2 Bi1 Bi1 94.301(16) 7_566 7_566 ?
N4 Bi1 Bi1 76.85(6) 7_566 7_566 ?
N4 Bi1 S1 173.55(6) 7_566 . ?
N4 Bi1 S2 91.28(6) 7_566 7_566 ?
C1 S1 Bi1 104.48(11) . . ?
C1 N1 C2 130.7(3) . . ?
C1 N1 N2 108.8(3) . . ?
N2 N1 C2 120.2(3) . . ?
N1 C1 S1 125.5(2) . . ?
N4 C1 S1 127.7(2) . . ?
N4 C1 N1 106.8(3) . . ?
C3 C2 N1 120.3(3) . . ?
C3 C2 C7 121.8(3) . . ?
C7 C2 N1 118.0(3) . . ?
N6 N7 N8 110.9(3) . . ?
N7 N8 Bi1 119.12(19) . . ?
C8 N8 Bi1 133.1(2) . . ?
C8 N8 N7 107.2(2) . . ?
N6 N5 C9 120.2(2) . . ?
C8 N5 N6 109.0(2) . . ?
C8 N5 C9 130.7(3) . . ?
N7 N6 N5 106.5(3) . . ?
C14 C9 N5 118.2(3) . . ?
C10 C9 N5 119.8(3) . . ?
C10 C9 C14 121.9(3) . . ?
C6 C5 H5 119.9 . . ?
C6 C5 C4 120.2(3) . . ?
C4 C5 H5 119.9 . . ?
C9 C14 H14 120.7 . . ?
C9 C14 C13 118.5(3) . . ?
C13 C14 H14 120.7 . . ?
C2 C3 H3 120.7 . . ?
C2 C3 C4 118.6(3) . . ?
C4 C3 H3 120.7 . . ?
C14 C13 H13 119.8 . . ?
C12 C13 C14 120.3(3) . . ?
C12 C13 H13 119.8 . . ?
C2 C7 H7 120.8 . . ?
C2 C7 C6 118.4(3) . . ?
C6 C7 H7 120.8 . . ?
C9 C10 H10 120.7 . . ?
C9 C10 C11 118.7(3) . . ?
C11 C10 H10 120.7 . . ?
C5 C6 C7 120.6(3) . . ?
C5 C6 H6 119.7 . . ?
C7 C6 H6 119.7 . . ?
C13 C12 H12 119.8 . . ?
C13 C12 C11 120.5(3) . . ?
C11 C12 H12 119.8 . . ?
C5 C4 C3 120.2(3) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C10 C11 H11 120.0 . . ?
C12 C11 C10 120.1(3) . . ?
C12 C11 H11 120.0 . . ?
C8 S2 Bi1 104.35(10) . 7_566 ?
C1 N4 Bi1 133.9(2) . 7_566 ?
C1 N4 N3 107.0(3) . . ?
N3 N4 Bi1 118.78(19) . 7_566 ?
N3 N2 N1 106.3(3) . . ?
N2 N3 N4 111.0(3) . . ?
N8 C8 N5 106.4(3) . . ?
N8 C8 S2 128.7(2) . . ?
N5 C8 S2 124.9(2) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 -0.928 0.250 161.8 16.3 ?
2 0.000 -0.600 0.750 161.8 16.3 ?
3 0.000 0.500 0.000 7.2 0.3 ?
4 0.000 0.500 0.500 7.2 0.3 ?
5 0.500 -0.726 0.250 161.8 16.3 ?
6 0.500 -0.070 0.750 161.8 16.3 ?
7 0.500 0.000 0.000 7.2 0.3 ?
8 0.500 0.000 0.500 7.2 0.3 ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 0 -1 0.0396 -0.0000 0.0000 -0.9988 0.0254 0.0141 -0.0035
1 0 0 0.0462 0.9990 0.0003 0.0007 -0.0021 0.0045 0.0297
-1 0 0 0.0572 -0.9990 -0.0003 -0.0007 0.0021 -0.0045 -0.0297
0 0 1 0.0396 0.0000 -0.0000 0.9988 -0.0254 -0.0141 0.0035
0 1 0 0.1812 -0.0043 0.9992 0.0044 -0.0524 0.0897 -0.0174
0 -1 0 0.1812 0.0043 -0.9992 -0.0044 0.0524 -0.0897 0.0174

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-2
_database_code_depnum_ccdc_archive 'CCDC 981809'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound6b

_audit_creation_date             2013-11-06
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C28 H20 Bi2 N16 S4, 2(C2 H3 N)'
_chemical_formula_sum            'C32 H26 Bi2 N18 S4'
_chemical_formula_weight         1208.91
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C16 h18 B Bi N2 O4 S2'
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'
Bi Bi -4.1077 10.2566 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.07185(17)
_cell_length_b                   11.5039(4)
_cell_length_c                   13.7591(5)
_cell_angle_alpha                67.741(3)
_cell_angle_beta                 89.501(2)
_cell_angle_gamma                78.825(2)
_cell_volume                     1013.72(6)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    34915
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.9580
_cell_measurement_theta_min      3.0480
_exptl_absorpt_coefficient_mu    8.924
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.112
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.980
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             574
_exptl_crystal_size_max          0.5349
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.0451
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            59206
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.079
_diffrn_reflns_theta_min         2.944
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 8.0951
_diffrn_measured_fraction_theta_full 0.9995
_diffrn_measured_fraction_theta_max 0.9425
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -42.00   59.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -19.0000  150.0000 101

#__ type_ start__ end____ width___ exp.time_
  2 omega   16.00   83.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421 -134.0000  117.0000 67

#__ type_ start__ end____ width___ exp.time_
  3 omega   -4.00   94.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   77.0000   90.0000 98

#__ type_ start__ end____ width___ exp.time_
  4 omega   10.00   86.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421 -135.0000  -61.0000 76

#__ type_ start__ end____ width___ exp.time_
  5 omega   -4.00   43.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   77.0000 -150.0000 47

#__ type_ start__ end____ width___ exp.time_
  6 omega  -42.00   54.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -77.0000  120.0000 96

#__ type_ start__ end____ width___ exp.time_
  7 omega   -4.00   88.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   77.0000  -30.0000 92

#__ type_ start__ end____ width___ exp.time_
  8 omega  -40.00   46.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -77.0000  -30.0000 86

#__ type_ start__ end____ width___ exp.time_
  9 omega    7.00   85.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   57.0000  -90.0000 78

#__ type_ start__ end____ width___ exp.time_
 10 omega    1.00   90.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421    0.0000  -90.0000 89

#__ type_ start__ end____ width___ exp.time_
 11 omega  -97.00  -35.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000 -178.0000  -60.0000 62

#__ type_ start__ end____ width___ exp.time_
 12 omega  -92.00   -5.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000  -57.0000   90.0000 87

#__ type_ start__ end____ width___ exp.time_
 13 omega    3.00   96.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   38.0000 -120.0000 93

#__ type_ start__ end____ width___ exp.time_
 14 omega  -20.00   66.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -99.0000 -180.0000 86

#__ type_ start__ end____ width___ exp.time_
 15 omega   -4.00   94.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   77.0000   60.0000 98

#__ type_ start__ end____ width___ exp.time_
 16 omega    8.00   86.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421 -135.0000  -61.0000 78

#__ type_ start__ end____ width___ exp.time_
 17 omega  -46.00   47.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -38.0000  -90.0000 93

#__ type_ start__ end____ width___ exp.time_
 18 omega  -13.00   97.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   19.0000    0.0000 110

#__ type_ start__ end____ width___ exp.time_
 19 omega  -95.00   48.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000 -180.0000 143

#__ type_ start__ end____ width___ exp.time_
 20 omega  -97.00  -35.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000 -178.0000 -180.0000 62

#__ type_ start__ end____ width___ exp.time_
 21 omega  -95.00   48.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000 -150.0000 143

#__ type_ start__ end____ width___ exp.time_
 22 omega  -92.00   -5.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000  -57.0000  150.0000 87

#__ type_ start__ end____ width___ exp.time_
 23 omega  -20.00   66.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  -99.0000   30.0000 86

#__ type_ start__ end____ width___ exp.time_
 24 omega    7.00   93.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   57.0000    0.0000 86

#__ type_ start__ end____ width___ exp.time_
 25 omega   35.00   99.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421  178.0000 -180.0000 64

#__ type_ start__ end____ width___ exp.time_
 26 omega   -4.00   94.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0421   77.0000  -60.0000 98

#__ type_ start__ end____ width___ exp.time_
 27 omega  -95.00   46.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000 -120.0000 141
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0008942000
_diffrn_orient_matrix_UB_12      0.0077729000
_diffrn_orient_matrix_UB_13      0.0487204000
_diffrn_orient_matrix_UB_21      -0.0142997000
_diffrn_orient_matrix_UB_22      0.0674702000
_diffrn_orient_matrix_UB_23      -0.0272915000
_diffrn_orient_matrix_UB_31      -0.1014918000
_diffrn_orient_matrix_UB_32      0.0047159000
_diffrn_orient_matrix_UB_33      0.0002552000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5688
_reflns_number_total             5928
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         3.633
_refine_diff_density_min         -1.461
_refine_diff_density_rms         0.161
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         5928
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0260
_refine_ls_restrained_S_all      1.158
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0200P)²+5.4021P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0647
_refine_ls_wR_factor_ref         0.0656
_refine_special_details          
;
 Disorder of CH3CN over two positions (40:60)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Bi1 Bi 0.31323(2) 0.49508(2) 1.05591(2) 0.01117(4) Uani 1 1 d . . . . .
S1 S 0.22339(14) 0.31295(9) 0.99636(8) 0.01495(17) Uani 1 1 d . . . . .
S2 S 0.52960(14) 0.69754(10) 0.76438(8) 0.01605(18) Uani 1 1 d . . . . .
N1 N 0.3850(5) 0.2278(3) 0.8479(3) 0.0170(7) Uani 1 1 d . . . . .
N2 N 0.5293(6) 0.2466(4) 0.7802(3) 0.0246(8) Uani 1 1 d . . . . .
N3 N 0.6020(6) 0.3361(4) 0.7895(3) 0.0248(8) Uani 1 1 d . . . . .
N4 N 0.5116(5) 0.3771(4) 0.8624(3) 0.0190(7) Uani 1 1 d . . . . .
N5 N 0.1590(5) 0.7439(3) 0.6846(3) 0.0159(6) Uani 1 1 d . . . . .
N6 N -0.0180(5) 0.7196(4) 0.7159(3) 0.0199(7) Uani 1 1 d . . . . .
N7 N 0.0053(5) 0.6541(3) 0.8158(3) 0.0177(7) Uani 1 1 d . . . . .
N8 N 0.1927(5) 0.6342(3) 0.8526(3) 0.0156(6) Uani 1 1 d . . . . .
C1 C 0.3749(6) 0.3090(4) 0.8987(3) 0.0154(7) Uani 1 1 d . . . . .
C2 C 0.2823(6) 0.1282(4) 0.8608(3) 0.0161(7) Uani 1 1 d . . . . .
C3 C 0.0826(6) 0.1559(4) 0.8528(3) 0.0180(8) Uani 1 1 d . . . . .
H3 H 0.0142 0.2388 0.8390 0.022 Uiso 1 1 calc R U . . .
C4 C -0.0140(7) 0.0569(5) 0.8658(4) 0.0232(9) Uani 1 1 d . . . . .
H4 H -0.1483 0.0738 0.8615 0.028 Uiso 1 1 calc R U . . .
C5 C 0.0872(7) -0.0661(4) 0.8849(4) 0.0226(9) Uani 1 1 d . . . . .
H5 H 0.0213 -0.1314 0.8931 0.027 Uiso 1 1 calc R U . . .
C6 C 0.2879(7) -0.0915(4) 0.8919(4) 0.0221(8) Uani 1 1 d . . . . .
H6 H 0.3563 -0.1740 0.9042 0.026 Uiso 1 1 calc R U . . .
C7 C 0.3870(6) 0.0054(4) 0.8806(4) 0.0210(8) Uani 1 1 d . . . . .
H7 H 0.5214 -0.0117 0.8862 0.025 Uiso 1 1 calc R U . . .
C8 C 0.2889(5) 0.6904(4) 0.7696(3) 0.0135(7) Uani 1 1 d . . . . .
C9 C 0.1886(6) 0.8146(4) 0.5765(3) 0.0189(8) Uani 1 1 d . . . . .
C10 C 0.1539(8) 0.7652(5) 0.5023(4) 0.0310(11) Uani 1 1 d . . . . .
H10 H 0.1119 0.6882 0.5221 0.037 Uiso 1 1 calc R U . . .
C11 C 0.1832(9) 0.8335(6) 0.3975(4) 0.0408(14) Uani 1 1 d . . . . .
H11 H 0.1612 0.8021 0.3464 0.049 Uiso 1 1 calc R U . . .
C12 C 0.2448(8) 0.9477(6) 0.3698(4) 0.0371(13) Uani 1 1 d . . . . .
H12 H 0.2644 0.9928 0.2997 0.045 Uiso 1 1 calc R U . . .
C13 C 0.2780(7) 0.9961(5) 0.4445(4) 0.0316(12) Uani 1 1 d . . . . .
H13 H 0.3196 1.0733 0.4245 0.038 Uiso 1 1 calc R U . . .
C14 C 0.2490(6) 0.9291(5) 0.5500(3) 0.0238(9) Uani 1 1 d . . . . .
H14 H 0.2698 0.9609 0.6010 0.029 Uiso 1 1 calc R U . . .
N9A N 1.035(3) 0.4489(15) 0.6539(12) 0.053(4) Uani 0.402(13) 1 d . . P A 1
C15A C 0.886(2) 0.4966(16) 0.6133(13) 0.044(4) Uani 0.402(13) 1 d . . P A 1
C16A C 0.696(8) 0.571(6) 0.558(3) 0.070(13) Uani 0.402(13) 1 d . . P A 1
H16D H 0.6957 0.5779 0.4861 0.106 Uiso 0.402(13) 1 calc R U P A 1
H16E H 0.6740 0.6552 0.5595 0.106 Uiso 0.402(13) 1 calc R U P A 1
H16F H 0.5960 0.5280 0.5921 0.106 Uiso 0.402(13) 1 calc R U P A 1
N9B N 0.1597(19) 0.4271(11) 0.6276(9) 0.060(3) Uani 0.598(13) 1 d . . P A 2
C15B C 0.2256(15) 0.4036(11) 0.5607(9) 0.043(3) Uani 0.598(13) 1 d . . P A 2
C16B C 0.317(6) 0.380(5) 0.472(3) 0.099(14) Uani 0.598(13) 1 d . . P A 2
H16A H 0.2514 0.4421 0.4074 0.148 Uiso 0.598(13) 1 calc R U P A 2
H16B H 0.3086 0.2952 0.4775 0.148 Uiso 0.598(13) 1 calc R U P A 2
H16C H 0.4499 0.3859 0.4743 0.148 Uiso 0.598(13) 1 calc R U P A 2


_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 Bi1 3.0449(3) 2_667 ?
Bi1 S1 2.7001(10) . ?
Bi1 S2 2.6836(10) 2_667 ?
Bi1 N4 2.635(4) 2_667 ?
Bi1 N8 2.689(3) . ?
S1 C1 1.720(4) . ?
S2 Bi1 2.6836(10) 2_667 ?
S2 C8 1.720(4) . ?
N1 N2 1.369(5) . ?
N1 C1 1.353(5) . ?
N1 C2 1.427(5) . ?
N2 N3 1.283(5) . ?
N3 N4 1.366(5) . ?
N4 Bi1 2.634(4) 2_667 ?
N4 C1 1.337(5) . ?
N5 N6 1.366(5) . ?
N5 C8 1.359(5) . ?
N5 C9 1.435(5) . ?
N6 N7 1.287(5) . ?
N7 N8 1.368(5) . ?
N8 C8 1.335(5) . ?
C2 C3 1.382(6) . ?
C2 C7 1.387(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.393(6) . ?
C4 H4 0.9300 . ?
C4 C5 1.383(7) . ?
C5 H5 0.9300 . ?
C5 C6 1.389(6) . ?
C6 H6 0.9300 . ?
C6 C7 1.389(6) . ?
C7 H7 0.9300 . ?
C9 C10 1.387(7) . ?
C9 C14 1.379(6) . ?
C10 H10 0.9300 . ?
C10 C11 1.393(7) . ?
C11 H11 0.9300 . ?
C11 C12 1.379(9) . ?
C12 H12 0.9300 . ?
C12 C13 1.383(8) . ?
C13 H13 0.9300 . ?
C13 C14 1.397(6) . ?
C14 H14 0.9300 . ?
N9A C15A 1.13(2) . ?
C15A C16A 1.48(5) . ?
C16A H16D 0.9600 . ?
C16A H16E 0.9600 . ?
C16A H16F 0.9600 . ?
N9B C15B 1.127(17) . ?
C15B C16B 1.46(4) . ?
C16B H16A 0.9600 . ?
C16B H16B 0.9600 . ?
C16B H16C 0.9600 . ?

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
S1 Bi1 Bi1 93.95(2) . 2_667 ?
S2 Bi1 Bi1 95.55(2) 2_667 2_667 ?
S2 Bi1 S1 86.55(3) 2_667 . ?
S2 Bi1 N8 162.89(8) 2_667 . ?
N4 Bi1 Bi1 77.84(8) 2_667 2_667 ?
N4 Bi1 S1 163.94(8) 2_667 . ?
N4 Bi1 S2 80.62(9) 2_667 2_667 ?
N4 Bi1 N8 111.68(11) 2_667 . ?
N8 Bi1 Bi1 76.38(7) . 2_667 ?
N8 Bi1 S1 79.11(8) . . ?
C1 S1 Bi1 104.57(14) . . ?
C8 S2 Bi1 102.41(13) . 2_667 ?
N2 N1 C2 120.3(3) . . ?
C1 N1 N2 109.0(3) . . ?
C1 N1 C2 130.5(3) . . ?
N3 N2 N1 106.5(3) . . ?
N2 N3 N4 110.8(3) . . ?
N3 N4 Bi1 118.6(3) . 2_667 ?
C1 N4 Bi1 131.1(3) . 2_667 ?
C1 N4 N3 107.1(3) . . ?
N6 N5 C9 121.8(3) . . ?
C8 N5 N6 109.1(3) . . ?
C8 N5 C9 129.1(3) . . ?
N7 N6 N5 106.1(3) . . ?
N6 N7 N8 111.3(3) . . ?
N7 N8 Bi1 122.0(2) . . ?
C8 N8 Bi1 131.3(3) . . ?
C8 N8 N7 106.7(3) . . ?
N1 C1 S1 125.2(3) . . ?
N4 C1 S1 128.1(3) . . ?
N4 C1 N1 106.6(3) . . ?
C3 C2 N1 119.7(4) . . ?
C3 C2 C7 121.6(4) . . ?
C7 C2 N1 118.7(4) . . ?
C2 C3 H3 120.7 . . ?
C2 C3 C4 118.5(4) . . ?
C4 C3 H3 120.7 . . ?
C3 C4 H4 119.5 . . ?
C5 C4 C3 120.9(4) . . ?
C5 C4 H4 119.5 . . ?
C4 C5 H5 120.2 . . ?
C4 C5 C6 119.6(4) . . ?
C6 C5 H5 120.2 . . ?
C5 C6 H6 119.8 . . ?
C5 C6 C7 120.4(4) . . ?
C7 C6 H6 119.8 . . ?
C2 C7 C6 118.9(4) . . ?
C2 C7 H7 120.5 . . ?
C6 C7 H7 120.5 . . ?
N5 C8 S2 124.1(3) . . ?
N8 C8 S2 129.0(3) . . ?
N8 C8 N5 106.8(3) . . ?
C10 C9 N5 118.5(4) . . ?
C14 C9 N5 119.2(4) . . ?
C14 C9 C10 122.4(4) . . ?
C9 C10 H10 120.7 . . ?
C9 C10 C11 118.5(5) . . ?
C11 C10 H10 120.7 . . ?
C10 C11 H11 120.1 . . ?
C12 C11 C10 119.8(5) . . ?
C12 C11 H11 120.1 . . ?
C11 C12 H12 119.5 . . ?
C11 C12 C13 121.0(5) . . ?
C13 C12 H12 119.5 . . ?
C12 C13 H13 120.0 . . ?
C12 C13 C14 120.0(5) . . ?
C14 C13 H13 120.0 . . ?
C9 C14 C13 118.3(5) . . ?
C9 C14 H14 120.9 . . ?
C13 C14 H14 120.9 . . ?
N9A C15A C16A 174(4) . . ?
C15A C16A H16D 109.5 . . ?
C15A C16A H16E 109.5 . . ?
C15A C16A H16F 109.5 . . ?
H16D C16A H16E 109.5 . . ?
H16D C16A H16F 109.5 . . ?
H16E C16A H16F 109.5 . . ?
N9B C15B C16B 177(3) . . ?
C15B C16B H16A 109.5 . . ?
C15B C16B H16B 109.5 . . ?
C15B C16B H16C 109.5 . . ?
H16A C16B H16B 109.5 . . ?
H16A C16B H16C 109.5 . . ?
H16B C16B H16C 109.5 . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 1 -1 0.0342 -0.0000 1.0000 -1.0000 -0.0409 0.0948 0.0045
0 1 1 0.0295 0.0000 1.0000 0.9999 0.0565 0.0402 0.0050
0 -1 -1 0.0155 -0.0000 -1.0000 -0.9999 -0.0565 -0.0402 -0.0050
1 0 0 0.2369 1.0000 0.0000 -0.0000 0.0009 -0.0143 -0.1015
-1 0 0 0.2689 -1.0000 -0.0000 0.0000 -0.0009 0.0143 0.1015
0 -1 1 0.0492 0.0000 -1.0000 1.0000 0.0409 -0.0948 -0.0045

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-2
_database_code_depnum_ccdc_archive 'CCDC 981810'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound7

_audit_creation_date             2013-01-08
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '3(C7 H5 Bi0.33 N4 S)'
_chemical_formula_sum            'C21 H15 Bi N12 S3'
_chemical_formula_weight         740.61
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Bi Bi -4.0111 8.9310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           158
_space_group_name_H-M_alt        'P 3 c 1'
_space_group_name_Hall           'P 3 -2"c'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-y, x-y, z'
3 '-x+y, -x, z'
4 '-x+y, y, z+1/2'
5 'x, x-y, z+1/2'
6 '-y, -x, z+1/2'

_cell_length_a                   24.0122(6)
_cell_length_b                   24.0122(6)
_cell_length_c                   7.8167(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3903.17(17)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.85
_cell_measurement_theta_min      3.68
_exptl_absorpt_coefficient_mu    15.861
_exptl_absorpt_correction_T_max  0.5624
_exptl_absorpt_correction_T_min  0.1024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.890
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.041
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            52485
_diffrn_reflns_theta_full        71.98
_diffrn_reflns_theta_max         71.98
_diffrn_reflns_theta_min         2.12
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         0
_reflns_number_gt                4804
_reflns_number_total             5043
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         1.108
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.029(6)
_refine_ls_extinction_coef       0.000039(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.215
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         5043
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0185
_refine_ls_R_factor_gt           0.0176
_refine_ls_restrained_S_all      1.215
_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/[σ²(Fo²)+(0.0143P)²+3.7235P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0478
_refine_ls_wR_factor_ref         0.0484
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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 0.0000 0.0000 -0.03646(4) 0.01441(6) Uani 1 3 d S . .
Bi2 Bi 0.6667 0.3333 0.94882(2) 0.01371(7) Uani 1 3 d S . .
Bi3 Bi 0.3333 0.6667 0.84022(3) 0.01378(6) Uani 1 3 d S . .
S1 S 0.05349(3) 0.10394(4) 0.16882(13) 0.01604(19) Uani 1 1 d . . .
S2 S 0.56376(5) 0.28258(4) 0.74394(12) 0.0161(2) Uani 1 1 d . . .
S3 S 0.38323(4) 0.61411(3) 0.63389(13) 0.01586(18) Uani 1 1 d . . .
N1 N 0.18366(13) 0.17551(14) 0.1031(4) 0.0204(6) Uani 1 1 d . . .
N2 N 0.22776(14) 0.17230(14) -0.0021(4) 0.0260(7) Uani 1 1 d . . .
N3 N 0.19706(14) 0.11847(14) -0.0840(4) 0.0253(6) Uani 1 1 d . . .
N4 N 0.13401(13) 0.08569(14) -0.0352(4) 0.0206(6) Uani 1 1 d . . .
N5 N 0.48716(14) 0.33550(14) 0.8102(4) 0.0213(6) Uani 1 1 d . . .
N6 N 0.48722(15) 0.38062(15) 0.9174(4) 0.0267(7) Uani 1 1 d . . .
N7 N 0.54045(16) 0.40516(15) 1.0020(4) 0.0271(7) Uani 1 1 d . . .
N8 N 0.57632(13) 0.37829(13) 0.9540(4) 0.0199(6) Uani 1 1 d . . .
N9 N 0.32837(14) 0.48437(13) 0.6985(4) 0.0208(6) Uani 1 1 d . . .
N10 N 0.28448(15) 0.43955(14) 0.8079(4) 0.0250(6) Uani 1 1 d . . .
N11 N 0.26110(14) 0.46928(14) 0.8949(4) 0.0246(6) Uani 1 1 d . . .
N12 N 0.28839(13) 0.53216(13) 0.8468(4) 0.0205(6) Uani 1 1 d . . .
C1 C 0.12700(15) 0.12176(16) 0.0798(5) 0.0180(6) Uani 1 1 d . . .
C2 C 0.19891(16) 0.23006(16) 0.2100(5) 0.0209(7) Uani 1 1 d . . .
C3 C 0.18193(17) 0.21976(17) 0.3800(5) 0.0219(7) Uani 1 1 d . . .
H3 H 0.1690(18) 0.1834(19) 0.419(5) 0.017(10) Uiso 1 1 d . . .
C4 C 0.19266(18) 0.27189(18) 0.4809(6) 0.0282(8) Uani 1 1 d . . .
H4 H 0.182(2) 0.267(2) 0.608(6) 0.030(11) Uiso 1 1 d . . .
C5 C 0.2214(2) 0.3334(2) 0.4099(6) 0.0334(9) Uani 1 1 d . . .
H5 H 0.228(2) 0.372(2) 0.479(6) 0.038(12) Uiso 1 1 d . . .
C6 C 0.2389(2) 0.34252(18) 0.2408(6) 0.0326(9) Uani 1 1 d . . .
H6 H 0.256(2) 0.381(2) 0.200(6) 0.028(11) Uiso 1 1 d . . .
C7 C 0.22770(19) 0.29063(18) 0.1367(6) 0.0288(8) Uani 1 1 d . . .
H7 H 0.2401(17) 0.2934(16) 0.033(5) 0.008(8) Uiso 1 1 d . . .
C8 C 0.54236(16) 0.33473(15) 0.8345(4) 0.0177(7) Uani 1 1 d . . .
C9 C 0.43596(16) 0.29895(17) 0.6926(5) 0.0228(7) Uani 1 1 d . . .
C10 C 0.45133(18) 0.29501(18) 0.5244(5) 0.0244(7) Uani 1 1 d . . .
H10 H 0.491(2) 0.3184(19) 0.490(5) 0.016(9) Uiso 1 1 d . . .
C11 C 0.40252(18) 0.25906(19) 0.4087(5) 0.0288(8) Uani 1 1 d . . .
H11 H 0.4115(18) 0.2511(18) 0.298(5) 0.014(9) Uiso 1 1 d . . .
C12 C 0.3390(2) 0.2283(2) 0.4640(6) 0.0330(9) Uani 1 1 d . . .
H12 H 0.308(3) 0.214(3) 0.400(7) 0.046(15) Uiso 1 1 d . . .
C13 C 0.3245(2) 0.2327(2) 0.6324(6) 0.0373(10) Uani 1 1 d . . .
H13 H 0.283(2) 0.214(2) 0.661(5) 0.027(11) Uiso 1 1 d . . .
C14 C 0.37278(19) 0.2678(2) 0.7498(6) 0.0298(8) Uani 1 1 d . . .
H14 H 0.359(2) 0.267(2) 0.843(6) 0.028(12) Uiso 1 1 d . . .
C15 C 0.33048(15) 0.54032(15) 0.7250(4) 0.0170(6) Uani 1 1 d . . .
C16 C 0.36558(17) 0.47044(16) 0.5801(5) 0.0234(7) Uani 1 1 d . . .
C17 C 0.4026(2) 0.44449(19) 0.6406(6) 0.0298(9) Uani 1 1 d . . .
H17 H 0.4072(19) 0.4396(19) 0.730(6) 0.013(11) Uiso 1 1 d . . .
C18 C 0.4415(2) 0.4361(2) 0.5265(7) 0.0383(11) Uani 1 1 d . . .
H18 H 0.467(2) 0.421(2) 0.560(6) 0.038(12) Uiso 1 1 d . . .
C19 C 0.4423(2) 0.4511(2) 0.3560(6) 0.0348(10) Uani 1 1 d . . .
H19 H 0.468(3) 0.453(3) 0.287(7) 0.046(15) Uiso 1 1 d . . .
C20 C 0.4051(2) 0.47670(19) 0.2974(6) 0.0294(8) Uani 1 1 d . . .
H20 H 0.4035(17) 0.4845(17) 0.194(5) 0.007(8) Uiso 1 1 d . . .
C21 C 0.36613(17) 0.48647(16) 0.4111(5) 0.0236(7) Uani 1 1 d . . .
H21 H 0.3364(17) 0.5058(17) 0.378(5) 0.011(9) Uiso 1 1 d . . .


_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 S1 2.6922(10) 2 ?
Bi1 S1 2.6922(10) 3 ?
Bi1 S1 2.6922(10) . ?
Bi2 S2 2.6730(10) 3_665 ?
Bi2 S2 2.6730(10) . ?
Bi2 S2 2.6730(10) 2_655 ?
Bi3 S3 2.6723(9) . ?
Bi3 S3 2.6723(10) 2_665 ?
Bi3 S3 2.6723(10) 3_565 ?
S1 C1 1.740(3) . ?
S2 C8 1.725(3) . ?
S3 C15 1.734(3) . ?
N1 N2 1.373(4) . ?
N1 C1 1.339(4) . ?
N1 C2 1.438(5) . ?
N2 N3 1.292(4) . ?
N3 N4 1.366(4) . ?
N4 C1 1.316(5) . ?
N5 N6 1.369(4) . ?
N5 C8 1.348(4) . ?
N5 C9 1.431(5) . ?
N6 N7 1.291(5) . ?
N7 N8 1.362(4) . ?
N8 C8 1.334(5) . ?
N9 N10 1.366(4) . ?
N9 C15 1.335(4) . ?
N9 C16 1.437(5) . ?
N10 N11 1.299(4) . ?
N11 N12 1.364(4) . ?
N12 C15 1.329(4) . ?
C2 C3 1.376(5) . ?
C2 C7 1.384(5) . ?
C3 H3 0.83(4) . ?
C3 C4 1.390(5) . ?
C4 H4 1.01(5) . ?
C4 C5 1.396(6) . ?
C5 H5 1.01(5) . ?
C5 C6 1.372(7) . ?
C6 H6 0.87(5) . ?
C6 C7 1.397(6) . ?
C7 H7 0.85(4) . ?
C9 C10 1.382(5) . ?
C9 C14 1.388(5) . ?
C10 H10 0.87(4) . ?
C10 C11 1.387(5) . ?
C11 H11 0.93(4) . ?
C11 C12 1.390(6) . ?
C12 H12 0.82(6) . ?
C12 C13 1.379(7) . ?
C13 H13 0.89(5) . ?
C13 C14 1.385(6) . ?
C14 H14 0.79(5) . ?
C16 C17 1.399(6) . ?
C16 C21 1.374(5) . ?
C17 H17 0.72(4) . ?
C17 C18 1.378(6) . ?
C18 H18 0.89(5) . ?
C18 C19 1.379(7) . ?
C19 H19 0.80(5) . ?
C19 C20 1.391(6) . ?
C20 H20 0.83(4) . ?
C20 C21 1.393(5) . ?
C21 H21 1.06(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
S1 Bi1 S1 88.12(3) 3 2 ?
S1 Bi1 S1 88.12(3) . 2 ?
S1 Bi1 S1 88.11(3) . 3 ?
S2 Bi2 S2 87.80(3) . 3_665 ?
S2 Bi2 S2 87.80(3) 2_655 3_665 ?
S2 Bi2 S2 87.80(3) 2_655 . ?
S3 Bi3 S3 87.34(3) 2_665 . ?
S3 Bi3 S3 87.34(3) 3_565 . ?
S3 Bi3 S3 87.34(3) 3_565 2_665 ?
C1 S1 Bi1 86.84(12) . . ?
C8 S2 Bi2 88.06(12) . . ?
C15 S3 Bi3 87.92(11) . . ?
N2 N1 C2 123.2(3) . . ?
C1 N1 N2 107.7(3) . . ?
C1 N1 C2 129.0(3) . . ?
N3 N2 N1 106.4(3) . . ?
N2 N3 N4 110.6(3) . . ?
C1 N4 N3 106.3(3) . . ?
N6 N5 C9 122.6(3) . . ?
C8 N5 N6 108.2(3) . . ?
C8 N5 C9 129.1(3) . . ?
N7 N6 N5 106.5(3) . . ?
N6 N7 N8 111.0(3) . . ?
C8 N8 N7 106.3(3) . . ?
N10 N9 C16 123.0(3) . . ?
C15 N9 N10 108.8(3) . . ?
C15 N9 C16 128.2(3) . . ?
N11 N10 N9 105.6(3) . . ?
N10 N11 N12 111.3(3) . . ?
C15 N12 N11 105.6(3) . . ?
N1 C1 S1 126.8(3) . . ?
N4 C1 S1 124.0(3) . . ?
N4 C1 N1 108.9(3) . . ?
C3 C2 N1 118.7(3) . . ?
C3 C2 C7 122.5(3) . . ?
C7 C2 N1 118.8(3) . . ?
C2 C3 H3 118(3) . . ?
C2 C3 C4 118.8(3) . . ?
C4 C3 H3 123(3) . . ?
C3 C4 H4 121(2) . . ?
C3 C4 C5 119.9(4) . . ?
C5 C4 H4 119(2) . . ?
C4 C5 H5 121(3) . . ?
C6 C5 C4 120.1(4) . . ?
C6 C5 H5 119(3) . . ?
C5 C6 H6 118(3) . . ?
C5 C6 C7 120.8(4) . . ?
C7 C6 H6 121(3) . . ?
C2 C7 C6 117.9(4) . . ?
C2 C7 H7 117(2) . . ?
C6 C7 H7 125(2) . . ?
N5 C8 S2 127.1(3) . . ?
N8 C8 S2 124.7(3) . . ?
N8 C8 N5 107.9(3) . . ?
C10 C9 N5 118.5(3) . . ?
C10 C9 C14 121.8(4) . . ?
C14 C9 N5 119.7(4) . . ?
C9 C10 H10 119(3) . . ?
C9 C10 C11 119.4(3) . . ?
C11 C10 H10 121(3) . . ?
C10 C11 H11 121(2) . . ?
C10 C11 C12 119.3(4) . . ?
C12 C11 H11 119(2) . . ?
C11 C12 H12 124(4) . . ?
C13 C12 C11 120.5(4) . . ?
C13 C12 H12 114(4) . . ?
C12 C13 H13 118(3) . . ?
C12 C13 C14 120.9(4) . . ?
C14 C13 H13 121(3) . . ?
C9 C14 H14 129(3) . . ?
C13 C14 C9 118.1(4) . . ?
C13 C14 H14 112(3) . . ?
N9 C15 S3 127.3(3) . . ?
N12 C15 S3 123.9(2) . . ?
N12 C15 N9 108.6(3) . . ?
C17 C16 N9 119.6(4) . . ?
C21 C16 N9 118.3(3) . . ?
C21 C16 C17 122.1(4) . . ?
C16 C17 H17 125(3) . . ?
C18 C17 C16 118.4(4) . . ?
C18 C17 H17 115(3) . . ?
C17 C18 H18 121(3) . . ?
C17 C18 C19 120.6(4) . . ?
C19 C18 H18 118(3) . . ?
C18 C19 H19 125(4) . . ?
C18 C19 C20 120.4(4) . . ?
C20 C19 H19 114(4) . . ?
C19 C20 H20 122(3) . . ?
C19 C20 C21 119.9(4) . . ?
C21 C20 H20 118(3) . . ?
C16 C21 C20 118.6(3) . . ?
C16 C21 H21 116(2) . . ?
C20 C21 H21 125(2) . . ?



#===END 


_database_code_depnum_ccdc_archive 'CCDC 981811'
