# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound1
_database_code_depnum_ccdc_archive 'CCDC 1050429'
_audit_update_record             
;
2015-04-02 deposited with the CCDC.
2015-04-29 downloaded from the CCDC.
;
_audit_creation_date             2015-03-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Bi3 I11, 2(C24 H30 N2 Na O6), C2 H3 N'
_chemical_formula_sum            'C50 H63 Bi3 I11 N5 Na2 O12'
_chemical_formula_weight         2994.87
_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 0.0033 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'
I I -0.4742 1.8119 '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'
Na Na 0.0362 0.0249 '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'

_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.
;
_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                   14.0239(7)
_cell_length_b                   14.4683(7)
_cell_length_c                   21.9043(15)
_cell_angle_alpha                100.800(6)
_cell_angle_beta                 101.549(6)
_cell_angle_gamma                109.797(4)
_cell_volume                     3937.0(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1922
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.11
_cell_measurement_theta_min      1.59
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.063
_exptl_absorpt_correction_T_max  0.0582
_exptl_absorpt_correction_T_min  0.0119
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.526
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2696
_exptl_crystal_size_max          0.81
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1308
_diffrn_reflns_av_unetI/netI     0.1171
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            46317
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.804
_diffrn_reflns_theta_min         1.557
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Stoe IPDS-II'
_diffrn_measurement_method       'area detetor, ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9549
_reflns_number_total             16642
_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       ?
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_refine_diff_density_max         2.202
_refine_diff_density_min         -3.315
_refine_diff_density_rms         0.371
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.858
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     753
_refine_ls_number_reflns         16642
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0469
_refine_ls_restrained_S_all      0.858
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0400P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.1013
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C24(H24A,H24B), C11(H11A,H11B), C21(H21A,H21B), C33(H33A,
 H33B), C32(H32A,H32B), C14(H14A,H14B), C22(H22A,H22B), C3(H3A,H3B), C1(H1A,
 H1B), C23(H23A,H23B), C13(H13A,H13B), C12(H12A,H12B), C2(H2A,H2B), C4(H4A,H4B),
  C31(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
 C29(H29), C39(H39), C18(H18), C36(H36), C37(H37), C9(H9), C16(H16), C26(H26),
 C8(H8), C38(H38), C17(H17), C19(H19), C7(H7), C28(H28), C27(H27), C6(H6)
2.c Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C46(H46A,H46B,H46C), C42(H42A,H42B,H42C), C50(H50A,H50B,
 H50C), C44(H44A,H44B,H44C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 0.41622(3) 0.35141(3) 0.81273(2) 0.03593(10) Uani 1 1 d . . . . .
Bi3 Bi 0.88308(4) 0.54169(3) 1.22692(2) 0.03811(11) Uani 1 1 d . . . . .
Bi2 Bi 0.64777(3) 0.44748(3) 1.01690(2) 0.03444(10) Uani 1 1 d . . . . .
I6 I 0.82315(6) 0.46832(5) 0.96516(4) 0.04347(18) Uani 1 1 d . . . . .
I1 I 0.33932(6) 0.46363(5) 0.72844(4) 0.04200(18) Uani 1 1 d . . . . .
I11 I 0.89987(7) 0.42387(5) 1.31809(4) 0.04535(18) Uani 1 1 d . . . . .
I3 I 0.59602(7) 0.36704(6) 0.76375(4) 0.0490(2) Uani 1 1 d . . . . .
I5 I 0.49961(6) 0.24559(5) 0.91982(4) 0.04090(17) Uani 1 1 d . . . . .
I7 I 0.78516(6) 0.66121(5) 1.12294(4) 0.03677(16) Uani 1 1 d . . . . .
I4 I 0.56121(6) 0.56704(5) 0.92524(4) 0.03565(16) Uani 1 1 d . . . . .
I8 I 0.69916(6) 0.33757(5) 1.11331(4) 0.04162(18) Uani 1 1 d . . . . .
I9 I 1.03710(6) 0.50571(5) 1.16792(4) 0.04367(18) Uani 1 1 d . . . . .
I2 I 0.28038(7) 0.15229(5) 0.72246(4) 0.04311(18) Uani 1 1 d . . . . .
I10 I 1.03732(8) 0.73320(5) 1.31895(4) 0.0533(2) Uani 1 1 d . . . . .
Na2 Na 0.7810(4) 0.9981(3) 0.9048(2) 0.0423(10) Uani 1 1 d . . . . .
Na1 Na 0.7649(4) 0.6381(3) 0.5520(2) 0.0437(10) Uani 1 1 d . . . . .
O7 O 0.9067(6) 1.1431(5) 1.0134(4) 0.0386(17) Uani 1 1 d . . . . .
O11 O 0.7404(6) 0.8065(5) 0.8912(4) 0.0379(17) Uani 1 1 d . . . . .
O9 O 0.6713(6) 1.0375(5) 0.7988(4) 0.0404(18) Uani 1 1 d . . . . .
O12 O 0.8492(6) 0.9534(5) 1.0073(4) 0.0395(18) Uani 1 1 d . . . . .
O5 O 0.8535(7) 0.6617(5) 0.6687(4) 0.0439(19) Uani 1 1 d . . . . .
O6 O 0.9462(7) 0.8191(5) 0.6200(4) 0.0446(19) Uani 1 1 d . . . . .
O8 O 0.8315(7) 1.1820(5) 0.9005(4) 0.0446(19) Uani 1 1 d . . . . .
O2 O 0.6633(6) 0.6349(5) 0.4422(4) 0.0439(19) Uani 1 1 d . . . . .
O4 O 0.7110(6) 0.4745(5) 0.5974(4) 0.0407(18) Uani 1 1 d . . . . .
O1 O 0.8465(7) 0.8064(5) 0.5046(4) 0.0456(19) Uani 1 1 d . . . . .
O3 O 0.6151(7) 0.4614(6) 0.4810(4) 0.046(2) Uani 1 1 d . . . . .
O10 O 0.6304(7) 0.8485(5) 0.7897(4) 0.046(2) Uani 1 1 d . . . . .
C34 C 0.8212(9) 0.8459(7) 1.0022(6) 0.039(3) Uani 1 1 d . . . . .
H34A H 0.7499 0.8151 1.0077 0.047 Uiso 1 1 calc R . . . .
H34B H 0.8727 0.8364 1.0360 0.047 Uiso 1 1 calc R . . . .
C40 C 0.8772(9) 1.1176(8) 1.0662(5) 0.036(2) Uani 1 1 d . . . . .
C24 C 0.6972(10) 1.1445(7) 0.8072(6) 0.044(3) Uani 1 1 d . . . . .
H24A H 0.6574 1.1686 0.8346 0.053 Uiso 1 1 calc R . . . .
H24B H 0.6786 1.1579 0.7647 0.053 Uiso 1 1 calc R . . . .
C29 C 0.4427(10) 0.7993(8) 0.7415(6) 0.043(3) Uani 1 1 d . . . . .
H29 H 0.4278 0.7293 0.7389 0.052 Uiso 1 1 calc R . . . .
N1 N 0.8977(9) 0.5911(7) 0.5164(6) 0.053(3) Uani 1 1 d . . . . .
C39 C 0.8750(9) 1.1845(8) 1.1187(6) 0.041(3) Uani 1 1 d . . . . .
H39 H 0.8999 1.2557 1.1224 0.049 Uiso 1 1 calc R . . . .
N2 N 0.6812(9) 0.7444(8) 0.6027(6) 0.058(3) Uani 1 1 d . . . . .
C11 C 0.7706(10) 0.4872(8) 0.6602(6) 0.043(3) Uani 1 1 d . . . . .
H11A H 0.8372 0.4782 0.6590 0.051 Uiso 1 1 calc R . . . .
H11B H 0.7302 0.4362 0.6797 0.051 Uiso 1 1 calc R . . . .
N3 N 0.9079(9) 0.9975(7) 0.8435(6) 0.055(3) Uani 1 1 d . . . . .
C18 C 1.1199(12) 0.9259(8) 0.4977(7) 0.054(3) Uani 1 1 d . . . . .
H18 H 1.1581 0.9505 0.4688 0.065 Uiso 1 1 calc R . . . .
C35 C 0.8433(9) 1.0120(7) 1.0629(6) 0.037(2) Uani 1 1 d . . . . .
C21 C 0.9282(9) 1.2468(7) 1.0111(6) 0.042(3) Uani 1 1 d . . . . .
H21A H 0.9960 1.2940 1.0434 0.050 Uiso 1 1 calc R . . . .
H21B H 0.8711 1.2675 1.0206 0.050 Uiso 1 1 calc R . . . .
C36 C 0.8073(9) 0.9772(8) 1.1114(6) 0.039(2) Uani 1 1 d . . . . .
H36 H 0.7837 0.9063 1.1086 0.047 Uiso 1 1 calc R . . . .
C25 C 0.5668(10) 0.9746(8) 0.7721(6) 0.042(3) Uani 1 1 d . . . . .
N5 N 0.3859(10) 0.0466(8) 0.4864(7) 0.059(3) Uani 1 1 d . . . . .
C33 C 0.8231(9) 0.7978(7) 0.9370(6) 0.041(3) Uani 1 1 d . . . . .
H33A H 0.8924 0.8331 0.9301 0.049 Uiso 1 1 calc R . . . .
H33B H 0.8112 0.7250 0.9321 0.049 Uiso 1 1 calc R . . . .
C37 C 0.8055(10) 1.0449(9) 1.1643(6) 0.046(3) Uani 1 1 d . . . . .
H37 H 0.7835 1.0212 1.1988 0.055 Uiso 1 1 calc R . . . .
C32 C 0.7147(10) 0.7461(8) 0.8280(6) 0.043(3) Uani 1 1 d . . . . .
H32A H 0.7077 0.6757 0.8280 0.051 Uiso 1 1 calc R . . . .
H32B H 0.7705 0.7749 0.8074 0.051 Uiso 1 1 calc R . . . .
C14 C 0.9959(10) 0.8108(8) 0.6784(6) 0.043(3) Uani 1 1 d . . . . .
H14A H 1.0448 0.8794 0.7069 0.051 Uiso 1 1 calc R . . . .
H14B H 1.0377 0.7688 0.6712 0.051 Uiso 1 1 calc R . . . .
C5 C 0.6326(10) 0.3758(8) 0.4887(7) 0.049(3) Uani 1 1 d . . . . .
C47 C 0.5391(11) 0.9722(8) 0.9244(6) 0.044(3) Uani 1 1 d . . . . .
N4 N 0.6275(10) 0.9893(8) 0.9377(6) 0.057(3) Uani 1 1 d . . . . .
C10 C 0.6848(9) 0.3837(8) 0.5509(6) 0.041(3) Uani 1 1 d . . . . .
C20 C 0.9543(10) 0.8497(8) 0.5178(6) 0.044(3) Uani 1 1 d . . . . .
C43 C 0.6894(10) 0.8234(9) 0.6261(6) 0.049(3) Uani 1 1 d . . . . .
C22 C 0.9339(10) 1.2492(8) 0.9444(7) 0.047(3) Uani 1 1 d . . . . .
H22A H 0.9516 1.3197 0.9403 0.057 Uiso 1 1 calc R . . . .
H22B H 0.9891 1.2258 0.9343 0.057 Uiso 1 1 calc R . . . .
C3 C 0.5589(10) 0.5631(8) 0.4227(6) 0.045(3) Uani 1 1 d . . . . .
H3A H 0.5209 0.5655 0.3801 0.054 Uiso 1 1 calc R . . . .
H3B H 0.5217 0.5783 0.4547 0.054 Uiso 1 1 calc R . . . .
C9 C 0.7076(11) 0.3011(9) 0.5662(7) 0.053(3) Uani 1 1 d . . . . .
H9 H 0.7415 0.3053 0.6093 0.064 Uiso 1 1 calc R . . . .
C16 C 1.1185(10) 0.8965(8) 0.6012(6) 0.043(3) Uani 1 1 d . . . . .
H16 H 1.1562 0.9001 0.6433 0.052 Uiso 1 1 calc R . . . .
C48 C 0.4267(10) 0.9510(9) 0.9052(7) 0.051(3) Uani 1 1 d . . . . .
H48A H 0.3933 0.9015 0.8623 0.077 Uiso 1 1 calc GR . . . .
H48B H 0.4168 1.0144 0.9035 0.077 Uiso 1 1 calc GR . . . .
H48C H 0.3941 0.9227 0.9368 0.077 Uiso 1 1 calc GR . . . .
C26 C 0.4845(10) 1.0028(9) 0.7503(5) 0.042(3) Uani 1 1 d . . . . .
H26 H 0.4980 1.0728 0.7536 0.050 Uiso 1 1 calc R . . . .
C1 C 0.7884(11) 0.7921(8) 0.4399(6) 0.047(3) Uani 1 1 d . . . . .
H1A H 0.8128 0.7536 0.4085 0.056 Uiso 1 1 calc R . . . .
H1B H 0.7981 0.8589 0.4313 0.056 Uiso 1 1 calc R . . . .
C23 C 0.8116(10) 1.1979(8) 0.8388(6) 0.042(3) Uani 1 1 d . . . . .
H23A H 0.8513 1.1706 0.8129 0.050 Uiso 1 1 calc R . . . .
H23B H 0.8339 1.2719 0.8426 0.050 Uiso 1 1 calc R . . . .
C46 C 1.0063(13) 1.0595(10) 0.7621(8) 0.062(4) Uani 1 1 d . . . . .
H46A H 0.9679 1.0140 0.7183 0.092 Uiso 1 1 calc GR . . . .
H46B H 1.0780 1.0607 0.7741 0.092 Uiso 1 1 calc GR . . . .
H46C H 1.0102 1.1287 0.7631 0.092 Uiso 1 1 calc GR . . . .
C30 C 0.5444(10) 0.8693(8) 0.7677(6) 0.041(3) Uani 1 1 d . . . . .
C13 C 0.9140(10) 0.7618(8) 0.7099(6) 0.048(3) Uani 1 1 d . . . . .
H13A H 0.9480 0.7594 0.7535 0.058 Uiso 1 1 calc R . . . .
H13B H 0.8685 0.8007 0.7145 0.058 Uiso 1 1 calc R . . . .
C8 C 0.6782(10) 0.2131(8) 0.5153(8) 0.057(4) Uani 1 1 d . . . . .
H8 H 0.6930 0.1566 0.5240 0.069 Uiso 1 1 calc R . . . .
C41 C 0.9756(11) 0.6143(8) 0.5047(6) 0.046(3) Uani 1 1 d . . . . .
C45 C 0.9521(10) 1.0234(8) 0.8070(6) 0.044(3) Uani 1 1 d . . . . .
C12 C 0.7944(11) 0.5947(9) 0.6996(6) 0.050(3) Uani 1 1 d . . . . .
H12A H 0.7280 0.6044 0.7002 0.060 Uiso 1 1 calc R . . . .
H12B H 0.8359 0.6076 0.7448 0.060 Uiso 1 1 calc R . . . .
C2 C 0.6721(10) 0.7319(8) 0.4336(6) 0.046(3) Uani 1 1 d . . . . .
H2A H 0.6492 0.7682 0.4670 0.055 Uiso 1 1 calc R . . . .
H2B H 0.6272 0.7239 0.3903 0.055 Uiso 1 1 calc R . . . .
C4 C 0.5618(10) 0.4599(8) 0.4177(6) 0.047(3) Uani 1 1 d . . . . .
H4A H 0.4891 0.4067 0.4030 0.056 Uiso 1 1 calc R . . . .
H4B H 0.6002 0.4450 0.3864 0.056 Uiso 1 1 calc R . . . .
C38 C 0.8357(9) 1.1470(8) 1.1669(6) 0.043(3) Uani 1 1 d . . . . .
H38 H 0.8297 1.1925 1.2019 0.052 Uiso 1 1 calc R . . . .
C17 C 1.1724(11) 0.9318(8) 0.5578(7) 0.051(3) Uani 1 1 d . . . . .
H17 H 1.2475 0.9605 0.5710 0.061 Uiso 1 1 calc R . . . .
C15 C 1.0085(10) 0.8559(7) 0.5817(6) 0.041(3) Uani 1 1 d . . . . .
C31 C 0.6140(10) 0.7454(8) 0.7924(6) 0.046(3) Uani 1 1 d . . . . .
H31A H 0.5896 0.6991 0.7480 0.055 Uiso 1 1 calc R . . . .
H31B H 0.5595 0.7209 0.8147 0.055 Uiso 1 1 calc R . . . .
C42 C 1.0768(11) 0.6469(9) 0.4917(6) 0.052(3) Uani 1 1 d . . . . .
H42A H 1.0718 0.6021 0.4506 0.078 Uiso 1 1 calc GR . . . .
H42B H 1.1299 0.6436 0.5269 0.078 Uiso 1 1 calc GR . . . .
H42C H 1.0974 0.7174 0.4886 0.078 Uiso 1 1 calc GR . . . .
C49 C 0.4370(12) 0.0744(9) 0.5383(8) 0.054(4) Uani 1 1 d . . . . .
C19 C 1.0108(10) 0.8843(8) 0.4779(6) 0.044(3) Uani 1 1 d . . . . .
H19 H 0.9748 0.8799 0.4352 0.053 Uiso 1 1 calc R . . . .
C50 C 0.5044(13) 0.1076(10) 0.6052(7) 0.063(4) Uani 1 1 d . . . . .
H50A H 0.5543 0.0737 0.6083 0.095 Uiso 1 1 calc GR . . . .
H50B H 0.4604 0.0896 0.6341 0.095 Uiso 1 1 calc GR . . . .
H50C H 0.5437 0.1819 0.6179 0.095 Uiso 1 1 calc GR . . . .
C7 C 0.6282(12) 0.2070(9) 0.4527(8) 0.060(4) Uani 1 1 d . . . . .
H7 H 0.6094 0.1469 0.4188 0.072 Uiso 1 1 calc R . . . .
C44 C 0.6999(15) 0.9269(10) 0.6571(8) 0.073(5) Uani 1 1 d . . . . .
H44A H 0.6352 0.9362 0.6387 0.109 Uiso 1 1 calc GR . . . .
H44B H 0.7603 0.9772 0.6494 0.109 Uiso 1 1 calc GR . . . .
H44C H 0.7112 0.9363 0.7038 0.109 Uiso 1 1 calc GR . . . .
C28 C 0.3598(11) 0.8288(9) 0.7184(6) 0.052(3) Uani 1 1 d . . . . .
H28 H 0.2896 0.7791 0.6997 0.062 Uiso 1 1 calc R . . . .
C27 C 0.3810(11) 0.9293(9) 0.7231(6) 0.051(3) Uani 1 1 d . . . . .
H27 H 0.3251 0.9498 0.7079 0.062 Uiso 1 1 calc R . . . .
C6 C 0.6052(11) 0.2888(9) 0.4393(7) 0.053(3) Uani 1 1 d . . . . .
H6 H 0.5707 0.2846 0.3963 0.063 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
Bi1 I1 2.9531(8) . ?
Bi1 I3 2.8893(9) . ?
Bi1 I5 3.2670(9) . ?
Bi1 I7 3.3669(8) 2_667 ?
Bi1 I4 3.2797(9) . ?
Bi1 I2 2.9116(9) . ?
Bi3 I11 2.8824(9) . ?
Bi3 I8 3.3291(10) . ?
Bi3 I9 2.8695(8) . ?
Bi3 I10 2.9190(10) . ?
Bi2 I6 2.8577(8) . ?
Bi2 I5 3.0270(9) . ?
Bi2 I7 3.1860(9) . ?
Bi2 I4 3.2007(8) . ?
Bi2 I4 3.3778(8) 2_667 ?
Bi2 I8 2.9888(9) . ?
I7 Bi1 3.3669(8) 2_667 ?
I4 Bi2 3.3777(8) 2_667 ?
Na2 O7 2.666(9) . ?
Na2 O11 2.579(7) . ?
Na2 O9 2.782(9) . ?
Na2 O12 2.545(9) . ?
Na2 O8 2.536(8) . ?
Na2 O10 2.868(10) . ?
Na2 N3 2.436(11) . ?
Na2 N4 2.374(11) . ?
Na1 O5 2.512(9) . ?
Na1 O6 2.837(9) . ?
Na1 O2 2.521(9) . ?
Na1 O4 2.673(8) . ?
Na1 O1 2.802(9) . ?
Na1 O3 2.633(10) . ?
Na1 N1 2.403(10) . ?
Na1 N2 2.466(10) . ?
O7 C40 1.376(13) . ?
O7 C21 1.440(11) . ?
O11 C33 1.430(14) . ?
O11 C32 1.395(13) . ?
O9 C24 1.430(11) . ?
O9 C25 1.369(14) . ?
O12 C34 1.445(11) . ?
O12 C35 1.383(12) . ?
O5 C13 1.416(14) . ?
O5 C12 1.418(14) . ?
O6 C14 1.376(14) . ?
O6 C15 1.378(14) . ?
O8 C22 1.444(15) . ?
O8 C23 1.402(14) . ?
O2 C3 1.398(14) . ?
O2 C2 1.418(12) . ?
O4 C11 1.402(14) . ?
O4 C10 1.385(13) . ?
O1 C20 1.370(15) . ?
O1 C1 1.424(15) . ?
O3 C5 1.374(13) . ?
O3 C4 1.430(15) . ?
O10 C30 1.359(14) . ?
O10 C31 1.445(12) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C33 1.477(16) . ?
C40 C39 1.371(15) . ?
C40 C35 1.421(14) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C23 1.471(17) . ?
C29 H29 0.9500 . ?
C29 C30 1.366(17) . ?
C29 C28 1.404(17) . ?
N1 C41 1.127(15) . ?
C39 H39 0.9500 . ?
C39 C38 1.398(16) . ?
N2 C43 1.118(14) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.518(15) . ?
N3 C45 1.149(15) . ?
C18 H18 0.9500 . ?
C18 C17 1.347(19) . ?
C18 C19 1.380(18) . ?
C35 C36 1.370(15) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.487(16) . ?
C36 H36 0.9500 . ?
C36 C37 1.382(16) . ?
C25 C26 1.378(16) . ?
C25 C30 1.427(14) . ?
N5 C49 1.129(18) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C37 H37 0.9500 . ?
C37 C38 1.378(15) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C31 1.465(17) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C13 1.500(17) . ?
C5 C10 1.375(18) . ?
C5 C6 1.378(17) . ?
C47 N4 1.142(16) . ?
C47 C48 1.455(17) . ?
C10 C9 1.417(15) . ?
C20 C15 1.423(17) . ?
C20 C19 1.348(16) . ?
C43 C44 1.467(16) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.491(14) . ?
C9 H9 0.9500 . ?
C9 C8 1.401(18) . ?
C16 H16 0.9500 . ?
C16 C17 1.393(17) . ?
C16 C15 1.391(17) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C26 H26 0.9500 . ?
C26 C27 1.401(18) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.529(18) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C46 C45 1.428(17) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C8 H8 0.9500 . ?
C8 C7 1.38(2) . ?
C41 C42 1.440(18) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C38 H38 0.9500 . ?
C17 H17 0.9500 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C49 C50 1.46(2) . ?
C19 H19 0.9500 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C7 H7 0.9500 . ?
C7 C6 1.394(17) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C28 H28 0.9500 . ?
C28 C27 1.361(16) . ?
C27 H27 0.9500 . ?
C6 H6 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
I1 Bi1 I5 173.44(2) . . ?
I1 Bi1 I7 87.68(2) . 2_667 ?
I1 Bi1 I4 90.25(2) . . ?
I3 Bi1 I1 93.83(2) . . ?
I3 Bi1 I5 90.22(2) . . ?
I3 Bi1 I7 177.23(3) . 2_667 ?
I3 Bi1 I4 89.49(2) . . ?
I3 Bi1 I2 94.32(3) . . ?
I5 Bi1 I7 88.07(2) . 2_667 ?
I5 Bi1 I4 84.62(2) . . ?
I4 Bi1 I7 88.178(19) . 2_667 ?
I2 Bi1 I1 93.35(3) . . ?
I2 Bi1 I5 91.48(2) . . ?
I2 Bi1 I7 87.90(2) . 2_667 ?
I2 Bi1 I4 174.56(3) . . ?
I11 Bi3 I8 92.02(2) . . ?
I11 Bi3 I10 93.50(3) . . ?
I9 Bi3 I11 96.36(2) . . ?
I9 Bi3 I8 87.96(2) . . ?
I9 Bi3 I10 93.18(3) . . ?
I10 Bi3 I8 174.21(2) . . ?
I6 Bi2 I5 95.71(2) . . ?
I6 Bi2 I7 89.46(2) . . ?
I6 Bi2 I4 176.93(2) . 2_667 ?
I6 Bi2 I4 91.95(2) . . ?
I6 Bi2 I8 97.96(2) . . ?
I5 Bi2 I7 174.71(2) . . ?
I5 Bi2 I4 90.04(2) . . ?
I5 Bi2 I4 85.23(2) . 2_667 ?
I7 Bi2 I4 89.55(2) . 2_667 ?
I7 Bi2 I4 88.66(2) . . ?
I4 Bi2 I4 85.12(2) . 2_667 ?
I8 Bi2 I5 90.27(2) . . ?
I8 Bi2 I7 90.13(2) . . ?
I8 Bi2 I4 84.95(2) . 2_667 ?
I8 Bi2 I4 170.00(2) . . ?
Bi2 I5 Bi1 94.17(2) . . ?
Bi2 I7 Bi1 92.01(2) . 2_667 ?
Bi1 I4 Bi2 90.19(2) . 2_667 ?
Bi2 I4 Bi1 90.746(19) . . ?
Bi2 I4 Bi2 94.88(2) . 2_667 ?
Bi2 I8 Bi3 96.98(2) . . ?
O7 Na2 O9 123.3(2) . . ?
O7 Na2 O10 174.7(3) . . ?
O11 Na2 O7 122.9(3) . . ?
O11 Na2 O9 113.7(3) . . ?
O11 Na2 O10 59.9(2) . . ?
O9 Na2 O10 53.8(2) . . ?
O12 Na2 O7 58.6(2) . . ?
O12 Na2 O11 64.8(2) . . ?
O12 Na2 O9 169.4(3) . . ?
O12 Na2 O10 123.3(3) . . ?
O8 Na2 O7 63.1(3) . . ?
O8 Na2 O11 169.9(3) . . ?
O8 Na2 O9 61.5(3) . . ?
O8 Na2 O12 121.7(3) . . ?
O8 Na2 O10 114.8(3) . . ?
N3 Na2 O7 100.4(4) . . ?
N3 Na2 O11 86.9(3) . . ?
N3 Na2 O9 85.1(4) . . ?
N3 Na2 O12 105.1(4) . . ?
N3 Na2 O8 83.9(3) . . ?
N3 Na2 O10 84.0(3) . . ?
N4 Na2 O7 91.8(4) . . ?
N4 Na2 O11 93.4(3) . . ?
N4 Na2 O9 81.3(4) . . ?
N4 Na2 O12 88.3(4) . . ?
N4 Na2 O8 94.5(3) . . ?
N4 Na2 O10 83.4(4) . . ?
N4 Na2 N3 165.3(5) . . ?
O5 Na1 O6 61.1(3) . . ?
O5 Na1 O2 170.5(3) . . ?
O5 Na1 O4 62.6(3) . . ?
O5 Na1 O1 115.1(3) . . ?
O5 Na1 O3 120.4(3) . . ?
O2 Na1 O6 116.4(3) . . ?
O2 Na1 O4 121.3(3) . . ?
O2 Na1 O1 62.3(3) . . ?
O2 Na1 O3 63.5(3) . . ?
O4 Na1 O6 122.2(3) . . ?
O4 Na1 O1 172.5(3) . . ?
O1 Na1 O6 54.3(3) . . ?
O3 Na1 O6 171.8(3) . . ?
O3 Na1 O4 58.0(3) . . ?
O3 Na1 O1 124.3(3) . . ?
N1 Na1 O5 92.1(4) . . ?
N1 Na1 O6 80.4(3) . . ?
N1 Na1 O2 96.5(4) . . ?
N1 Na1 O4 89.7(3) . . ?
N1 Na1 O1 83.2(3) . . ?
N1 Na1 O3 91.4(3) . . ?
N1 Na1 N2 160.0(4) . . ?
N2 Na1 O5 81.6(3) . . ?
N2 Na1 O6 79.9(3) . . ?
N2 Na1 O2 89.0(3) . . ?
N2 Na1 O4 103.9(3) . . ?
N2 Na1 O1 82.4(3) . . ?
N2 Na1 O3 108.2(4) . . ?
C40 O7 Na2 110.1(6) . . ?
C40 O7 C21 116.7(8) . . ?
C21 O7 Na2 115.9(6) . . ?
C33 O11 Na2 108.2(6) . . ?
C32 O11 Na2 116.1(6) . . ?
C32 O11 C33 115.1(7) . . ?
C24 O9 Na2 112.3(7) . . ?
C25 O9 Na2 116.7(6) . . ?
C25 O9 C24 116.4(8) . . ?
C34 O12 Na2 116.4(6) . . ?
C35 O12 Na2 113.6(5) . . ?
C35 O12 C34 116.3(8) . . ?
C13 O5 Na1 119.3(7) . . ?
C13 O5 C12 113.3(9) . . ?
C12 O5 Na1 115.9(8) . . ?
C14 O6 Na1 111.0(6) . . ?
C14 O6 C15 117.3(9) . . ?
C15 O6 Na1 113.5(7) . . ?
C22 O8 Na2 112.8(6) . . ?
C23 O8 Na2 116.8(6) . . ?
C23 O8 C22 114.8(9) . . ?
C3 O2 Na1 112.4(7) . . ?
C3 O2 C2 113.4(8) . . ?
C2 O2 Na1 115.3(7) . . ?
C11 O4 Na1 115.9(6) . . ?
C10 O4 Na1 113.1(6) . . ?
C10 O4 C11 117.9(8) . . ?
C20 O1 Na1 116.3(6) . . ?
C20 O1 C1 115.6(9) . . ?
C1 O1 Na1 112.8(6) . . ?
C5 O3 Na1 116.0(8) . . ?
C5 O3 C4 118.3(9) . . ?
C4 O3 Na1 115.7(6) . . ?
C30 O10 Na2 113.9(6) . . ?
C30 O10 C31 118.3(9) . . ?
C31 O10 Na2 112.1(7) . . ?
O12 C34 H34A 110.4 . . ?
O12 C34 H34B 110.4 . . ?
O12 C34 C33 106.6(8) . . ?
H34A C34 H34B 108.6 . . ?
C33 C34 H34A 110.4 . . ?
C33 C34 H34B 110.4 . . ?
O7 C40 C35 115.2(9) . . ?
C39 C40 O7 125.4(9) . . ?
C39 C40 C35 119.4(10) . . ?
O9 C24 H24A 110.2 . . ?
O9 C24 H24B 110.2 . . ?
O9 C24 C23 107.5(9) . . ?
H24A C24 H24B 108.5 . . ?
C23 C24 H24A 110.2 . . ?
C23 C24 H24B 110.2 . . ?
C30 C29 H29 119.3 . . ?
C30 C29 C28 121.3(10) . . ?
C28 C29 H29 119.3 . . ?
C41 N1 Na1 149.4(9) . . ?
C40 C39 H39 120.3 . . ?
C40 C39 C38 119.4(10) . . ?
C38 C39 H39 120.3 . . ?
C43 N2 Na1 146.4(10) . . ?
O4 C11 H11A 110.3 . . ?
O4 C11 H11B 110.3 . . ?
O4 C11 C12 107.1(9) . . ?
H11A C11 H11B 108.6 . . ?
C12 C11 H11A 110.3 . . ?
C12 C11 H11B 110.3 . . ?
C45 N3 Na2 153.1(9) . . ?
C17 C18 H18 120.0 . . ?
C17 C18 C19 120.1(12) . . ?
C19 C18 H18 120.0 . . ?
O12 C35 C40 113.2(9) . . ?
C36 C35 O12 126.4(9) . . ?
C36 C35 C40 120.3(9) . . ?
O7 C21 H21A 110.4 . . ?
O7 C21 H21B 110.4 . . ?
O7 C21 C22 106.4(8) . . ?
H21A C21 H21B 108.6 . . ?
C22 C21 H21A 110.4 . . ?
C22 C21 H21B 110.4 . . ?
C35 C36 H36 119.9 . . ?
C35 C36 C37 120.1(10) . . ?
C37 C36 H36 119.9 . . ?
O9 C25 C26 127.0(10) . . ?
O9 C25 C30 114.2(9) . . ?
C26 C25 C30 118.8(11) . . ?
O11 C33 C34 107.0(8) . . ?
O11 C33 H33A 110.3 . . ?
O11 C33 H33B 110.3 . . ?
C34 C33 H33A 110.3 . . ?
C34 C33 H33B 110.3 . . ?
H33A C33 H33B 108.6 . . ?
C36 C37 H37 120.1 . . ?
C38 C37 C36 119.7(11) . . ?
C38 C37 H37 120.1 . . ?
O11 C32 H32A 110.3 . . ?
O11 C32 H32B 110.3 . . ?
O11 C32 C31 107.1(8) . . ?
H32A C32 H32B 108.5 . . ?
C31 C32 H32A 110.3 . . ?
C31 C32 H32B 110.3 . . ?
O6 C14 H14A 109.9 . . ?
O6 C14 H14B 109.9 . . ?
O6 C14 C13 109.0(10) . . ?
H14A C14 H14B 108.3 . . ?
C13 C14 H14A 109.9 . . ?
C13 C14 H14B 109.9 . . ?
O3 C5 C10 114.6(10) . . ?
O3 C5 C6 124.8(13) . . ?
C10 C5 C6 120.6(11) . . ?
N4 C47 C48 177.9(14) . . ?
C47 N4 Na2 149.5(11) . . ?
O4 C10 C9 122.3(11) . . ?
C5 C10 O4 116.8(9) . . ?
C5 C10 C9 120.8(10) . . ?
O1 C20 C15 113.2(10) . . ?
C19 C20 O1 127.6(12) . . ?
C19 C20 C15 119.2(12) . . ?
N2 C43 C44 179.7(16) . . ?
O8 C22 C21 107.2(9) . . ?
O8 C22 H22A 110.3 . . ?
O8 C22 H22B 110.3 . . ?
C21 C22 H22A 110.3 . . ?
C21 C22 H22B 110.3 . . ?
H22A C22 H22B 108.5 . . ?
O2 C3 H3A 110.1 . . ?
O2 C3 H3B 110.1 . . ?
O2 C3 C4 108.0(9) . . ?
H3A C3 H3B 108.4 . . ?
C4 C3 H3A 110.1 . . ?
C4 C3 H3B 110.1 . . ?
C10 C9 H9 121.2 . . ?
C8 C9 C10 117.6(14) . . ?
C8 C9 H9 121.2 . . ?
C17 C16 H16 120.6 . . ?
C15 C16 H16 120.6 . . ?
C15 C16 C17 118.8(12) . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C25 C26 H26 119.7 . . ?
C25 C26 C27 120.6(10) . . ?
C27 C26 H26 119.7 . . ?
O1 C1 H1A 110.4 . . ?
O1 C1 H1B 110.4 . . ?
O1 C1 C2 106.8(10) . . ?
H1A C1 H1B 108.6 . . ?
C2 C1 H1A 110.4 . . ?
C2 C1 H1B 110.4 . . ?
O8 C23 C24 107.4(9) . . ?
O8 C23 H23A 110.2 . . ?
O8 C23 H23B 110.2 . . ?
C24 C23 H23A 110.2 . . ?
C24 C23 H23B 110.2 . . ?
H23A C23 H23B 108.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
O10 C30 C29 125.9(9) . . ?
O10 C30 C25 114.7(10) . . ?
C29 C30 C25 119.4(11) . . ?
O5 C13 C14 106.0(9) . . ?
O5 C13 H13A 110.5 . . ?
O5 C13 H13B 110.5 . . ?
C14 C13 H13A 110.5 . . ?
C14 C13 H13B 110.5 . . ?
H13A C13 H13B 108.7 . . ?
C9 C8 H8 119.5 . . ?
C7 C8 C9 121.0(12) . . ?
C7 C8 H8 119.5 . . ?
N1 C41 C42 178.0(14) . . ?
N3 C45 C46 177.5(11) . . ?
O5 C12 C11 106.1(9) . . ?
O5 C12 H12A 110.5 . . ?
O5 C12 H12B 110.5 . . ?
C11 C12 H12A 110.5 . . ?
C11 C12 H12B 110.5 . . ?
H12A C12 H12B 108.7 . . ?
O2 C2 C1 107.1(9) . . ?
O2 C2 H2A 110.3 . . ?
O2 C2 H2B 110.3 . . ?
C1 C2 H2A 110.3 . . ?
C1 C2 H2B 110.3 . . ?
H2A C2 H2B 108.5 . . ?
O3 C4 C3 106.9(9) . . ?
O3 C4 H4A 110.3 . . ?
O3 C4 H4B 110.3 . . ?
C3 C4 H4A 110.3 . . ?
C3 C4 H4B 110.3 . . ?
H4A C4 H4B 108.6 . . ?
C39 C38 H38 119.5 . . ?
C37 C38 C39 121.0(10) . . ?
C37 C38 H38 119.5 . . ?
C18 C17 C16 121.2(13) . . ?
C18 C17 H17 119.4 . . ?
C16 C17 H17 119.4 . . ?
O6 C15 C20 116.3(11) . . ?
O6 C15 C16 124.5(11) . . ?
C16 C15 C20 119.2(11) . . ?
O10 C31 C32 108.1(9) . . ?
O10 C31 H31A 110.1 . . ?
O10 C31 H31B 110.1 . . ?
C32 C31 H31A 110.1 . . ?
C32 C31 H31B 110.1 . . ?
H31A C31 H31B 108.4 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N5 C49 C50 178.1(13) . . ?
C18 C19 H19 119.3 . . ?
C20 C19 C18 121.5(12) . . ?
C20 C19 H19 119.3 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C8 C7 H7 119.9 . . ?
C8 C7 C6 120.1(12) . . ?
C6 C7 H7 119.9 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C29 C28 H28 120.3 . . ?
C27 C28 C29 119.3(13) . . ?
C27 C28 H28 120.3 . . ?
C26 C27 H27 119.7 . . ?
C28 C27 C26 120.6(11) . . ?
C28 C27 H27 119.7 . . ?
C5 C6 C7 119.8(14) . . ?
C5 C6 H6 120.1 . . ?
C7 C6 H6 120.1 . . ?

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
Na2 O7 C40 C39 -140.3(10) . . . . ?
Na2 O7 C40 C35 37.4(10) . . . . ?
Na2 O7 C21 C22 -35.3(10) . . . . ?
Na2 O11 C33 C34 61.8(8) . . . . ?
Na2 O11 C32 C31 -65.7(10) . . . . ?
Na2 O9 C24 C23 39.5(10) . . . . ?
Na2 O9 C25 C26 138.9(10) . . . . ?
Na2 O9 C25 C30 -40.7(11) . . . . ?
Na2 O12 C34 C33 36.4(10) . . . . ?
Na2 O12 C35 C40 -43.8(10) . . . . ?
Na2 O12 C35 C36 134.9(10) . . . . ?
Na2 O8 C22 C21 -61.6(8) . . . . ?
Na2 O8 C23 C24 59.7(9) . . . . ?
Na2 O10 C30 C29 -141.7(10) . . . . ?
Na2 O10 C30 C25 39.7(11) . . . . ?
Na2 O10 C31 C32 -34.4(10) . . . . ?
Na1 O5 C13 C14 -56.4(10) . . . . ?
Na1 O5 C12 C11 58.3(10) . . . . ?
Na1 O6 C14 C13 -42.7(9) . . . . ?
Na1 O6 C15 C20 39.4(9) . . . . ?
Na1 O6 C15 C16 -139.8(8) . . . . ?
Na1 O2 C3 C4 -61.6(10) . . . . ?
Na1 O2 C2 C1 62.9(10) . . . . ?
Na1 O4 C11 C12 37.4(10) . . . . ?
Na1 O4 C10 C5 -35.9(12) . . . . ?
Na1 O4 C10 C9 145.8(9) . . . . ?
Na1 O1 C20 C15 -40.3(9) . . . . ?
Na1 O1 C20 C19 139.1(9) . . . . ?
Na1 O1 C1 C2 36.1(8) . . . . ?
Na1 O3 C5 C10 35.5(12) . . . . ?
Na1 O3 C5 C6 -142.0(11) . . . . ?
Na1 O3 C4 C3 -32.7(10) . . . . ?
O7 C40 C39 C38 175.2(10) . . . . ?
O7 C40 C35 O12 1.9(13) . . . . ?
O7 C40 C35 C36 -176.9(10) . . . . ?
O7 C21 C22 O8 62.3(10) . . . . ?
O11 C32 C31 O10 64.0(11) . . . . ?
O9 C24 C23 O8 -64.0(11) . . . . ?
O9 C25 C26 C27 179.3(11) . . . . ?
O9 C25 C30 O10 -1.0(14) . . . . ?
O9 C25 C30 C29 -179.7(10) . . . . ?
O12 C34 C33 O11 -65.4(10) . . . . ?
O12 C35 C36 C37 -179.7(11) . . . . ?
O6 C14 C13 O5 64.2(11) . . . . ?
O2 C3 C4 O3 61.3(11) . . . . ?
O4 C11 C12 O5 -60.9(12) . . . . ?
O4 C10 C9 C8 -179.6(10) . . . . ?
O1 C20 C15 O6 -0.5(11) . . . . ?
O1 C20 C15 C16 178.8(8) . . . . ?
O1 C20 C19 C18 -179.7(9) . . . . ?
O1 C1 C2 O2 -63.9(10) . . . . ?
O3 C5 C10 O4 1.2(15) . . . . ?
O3 C5 C10 C9 179.5(10) . . . . ?
O3 C5 C6 C7 179.1(11) . . . . ?
C34 O12 C35 C40 176.9(9) . . . . ?
C34 O12 C35 C36 -4.4(16) . . . . ?
C40 O7 C21 C22 -167.5(9) . . . . ?
C40 C39 C38 C37 4.1(18) . . . . ?
C40 C35 C36 C37 -1.0(17) . . . . ?
C24 O9 C25 C26 2.5(16) . . . . ?
C24 O9 C25 C30 -177.1(9) . . . . ?
C29 C28 C27 C26 0.4(18) . . . . ?
C39 C40 C35 O12 179.7(10) . . . . ?
C39 C40 C35 C36 0.9(16) . . . . ?
C11 O4 C10 C5 -175.7(10) . . . . ?
C11 O4 C10 C9 6.0(15) . . . . ?
C35 O12 C34 C33 174.5(9) . . . . ?
C35 C40 C39 C38 -2.4(17) . . . . ?
C35 C36 C37 C38 2.7(18) . . . . ?
C21 O7 C40 C39 -5.5(15) . . . . ?
C21 O7 C40 C35 172.2(9) . . . . ?
C36 C37 C38 C39 -4.3(18) . . . . ?
C25 O9 C24 C23 177.8(9) . . . . ?
C25 C26 C27 C28 0.6(18) . . . . ?
C33 O11 C32 C31 166.4(9) . . . . ?
C32 O11 C33 C34 -166.5(8) . . . . ?
C14 O6 C15 C20 171.0(8) . . . . ?
C14 O6 C15 C16 -8.2(13) . . . . ?
C5 O3 C4 C3 -176.9(9) . . . . ?
C5 C10 C9 C8 2.2(17) . . . . ?
C10 O4 C11 C12 176.1(9) . . . . ?
C10 C5 C6 C7 1.6(19) . . . . ?
C10 C9 C8 C7 -0.5(18) . . . . ?
C20 O1 C1 C2 173.3(7) . . . . ?
C22 O8 C23 C24 -165.0(7) . . . . ?
C3 O2 C2 C1 -165.6(9) . . . . ?
C9 C8 C7 C6 -0.6(19) . . . . ?
C26 C25 C30 O10 179.4(10) . . . . ?
C26 C25 C30 C29 0.6(16) . . . . ?
C1 O1 C20 C15 -176.0(8) . . . . ?
C1 O1 C20 C19 3.4(14) . . . . ?
C23 O8 C22 C21 161.2(8) . . . . ?
C30 O10 C31 C32 -170.1(9) . . . . ?
C30 C29 C28 C27 -1.0(18) . . . . ?
C30 C25 C26 C27 -1.2(16) . . . . ?
C13 O5 C12 C11 -158.5(10) . . . . ?
C8 C7 C6 C5 0.0(19) . . . . ?
C12 O5 C13 C14 161.8(9) . . . . ?
C2 O2 C3 C4 165.5(9) . . . . ?
C4 O3 C5 C10 179.6(10) . . . . ?
C4 O3 C5 C6 2.0(17) . . . . ?
C17 C18 C19 C20 0.7(15) . . . . ?
C17 C16 C15 O6 -179.6(9) . . . . ?
C17 C16 C15 C20 1.2(14) . . . . ?
C15 O6 C14 C13 -175.5(8) . . . . ?
C15 C20 C19 C18 -0.3(15) . . . . ?
C15 C16 C17 C18 -0.9(15) . . . . ?
C31 O10 C30 C29 -6.7(16) . . . . ?
C31 O10 C30 C25 174.6(9) . . . . ?
C19 C18 C17 C16 -0.1(15) . . . . ?
C19 C20 C15 O6 -179.9(8) . . . . ?
C19 C20 C15 C16 -0.7(14) . . . . ?
C28 C29 C30 O10 -178.2(11) . . . . ?
C28 C29 C30 C25 0.4(17) . . . . ?
C6 C5 C10 O4 178.9(10) . . . . ?
C6 C5 C10 C9 -2.8(18) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound2
_database_code_depnum_ccdc_archive 'CCDC 1050430'
_audit_update_record             
;
2015-04-02 deposited with the CCDC.
2015-04-29 downloaded from the CCDC.
;
_audit_creation_date             2015-03-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Bi8 I28, 4(C24 H30 N2 Na O6), 6(C2 H3 N)'
_chemical_formula_sum            'C108 H138 Bi8 I28 N14 Na4 O24'
_chemical_formula_weight         7333.32
_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 0.0033 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'
I I -0.4742 1.8119 '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'
Na Na 0.0362 0.0249 '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'

_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.
;
_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                   13.7807(6)
_cell_length_b                   14.9735(7)
_cell_length_c                   23.0161(9)
_cell_angle_alpha                85.620(3)
_cell_angle_beta                 88.702(3)
_cell_angle_gamma                74.572(3)
_cell_volume                     4564.7(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    3389
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      1.48
_shelx_estimated_absorpt_T_max   0.952
_shelx_estimated_absorpt_T_min   0.212
_exptl_absorpt_coefficient_mu    12.480
_exptl_absorpt_correction_T_max  0.4112
_exptl_absorpt_correction_T_min  0.1531
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.668
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3268
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.004
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1285
_diffrn_reflns_av_unetI/netI     0.1544
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            49426
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.790
_diffrn_reflns_theta_min         1.415
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Stoe IPDS-II'
_diffrn_measurement_method       'area detetor, ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9545
_reflns_number_total             19279
_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       ?
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_refine_diff_density_max         3.118
_refine_diff_density_min         -4.478
_refine_diff_density_rms         0.370
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.832
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     845
_refine_ls_number_reflns         19279
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.1203
_refine_ls_R_factor_gt           0.0594
_refine_ls_restrained_S_all      0.831
_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)+(0.0500P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1390
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C34) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C21)
\\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C27) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C34(H34A,H34B), C21(H21A,H21B), C19(H19A,H19B), C22(H22A,
 H22B), C32(H32A,H32B), C31(H31A,H31B), C33(H33A,H33B), C23(H23A,H23B), C7(H7A,
 H7B), C18(H18A,H18B), C20(H20A,H20B), C17(H17A,H17B), C10(H10A,H10B), C8(H8A,
 H8B), C9(H9A,H9B)
3.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C39(H39), C2(H2), C37(H37), C14(H14), C26(H26), C38(H38), C29(H29),
 C36(H36), C15(H15), C3(H3), C5(H5), C12(H12), C13(H13), C4(H4), C28(H28)
3.c Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C46(H46A,H46B,H46C), C44(H44A,H44B,
 H44C), C42(H42A,H42B,H42C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Bi2 Bi 0.22582(5) 0.50827(4) 0.38638(3) 0.02352(15) Uani 1 1 d . . . . .
Bi3 Bi 0.07883(5) 0.58362(4) 0.56205(3) 0.02503(15) Uani 1 1 d . . . . .
Bi4 Bi -0.07068(5) 0.66218(4) 0.73677(3) 0.02719(15) Uani 1 1 d . . . . .
Bi1 Bi 0.37742(5) 0.41601(4) 0.20698(3) 0.02560(15) Uani 1 1 d . . . . .
I11 I 0.01174(8) 0.46560(7) 0.66580(5) 0.0252(2) Uani 1 1 d . . . . .
I8 I 0.15290(8) 0.39625(7) 0.49461(5) 0.0250(2) Uani 1 1 d . . . . .
I5 I 0.29884(8) 0.32110(7) 0.33356(5) 0.0262(2) Uani 1 1 d . . . . .
I4 I 0.26683(8) 0.61095(7) 0.27612(5) 0.0289(3) Uani 1 1 d . . . . .
I7 I 0.11950(8) 0.68952(7) 0.44850(5) 0.0273(2) Uani 1 1 d . . . . .
I10 I -0.01513(9) 0.76392(7) 0.61188(5) 0.0328(3) Uani 1 1 d . . . . .
I9 I 0.27275(9) 0.55764(9) 0.61124(5) 0.0361(3) Uani 1 1 d . . . . .
I14 I -0.13586(9) 0.56292(8) 0.83841(5) 0.0360(3) Uani 1 1 d . . . . .
I6 I 0.41589(8) 0.50042(8) 0.43595(5) 0.0313(3) Uani 1 1 d . . . . .
I12 I 0.12509(9) 0.64222(8) 0.78221(6) 0.0378(3) Uani 1 1 d . . . . .
I2 I 0.46077(9) 0.22883(8) 0.17364(6) 0.0372(3) Uani 1 1 d . . . . .
I13 I -0.16586(10) 0.84476(8) 0.77043(6) 0.0424(3) Uani 1 1 d . . . . .
I3 I 0.56329(8) 0.44615(8) 0.24343(5) 0.0341(3) Uani 1 1 d . . . . .
I1 I 0.38521(9) 0.50153(8) 0.09231(5) 0.0362(3) Uani 1 1 d . . . . .
Na2 Na 0.2960(5) 0.9820(4) 0.5856(3) 0.0308(15) Uani 1 1 d . . . . .
Na1 Na 0.0842(5) 1.1966(4) 0.9605(3) 0.0369(17) Uani 1 1 d . . . . .
O9 O 0.1949(9) 1.1156(7) 0.6578(5) 0.031(3) Uani 1 1 d . . . . .
O7 O 0.3551(8) 1.0208(7) 0.4802(5) 0.028(3) Uani 1 1 d . . . . .
O10 O 0.2075(8) 0.9490(7) 0.6905(5) 0.032(3) Uani 1 1 d . . . . .
O2 O 0.2515(9) 1.2180(8) 0.9891(5) 0.035(3) Uani 1 1 d . . . . .
O5 O -0.1176(9) 1.2116(8) 0.9579(5) 0.034(3) Uani 1 1 d . . . . .
O12 O 0.3839(8) 0.8517(7) 0.5122(5) 0.029(3) Uani 1 1 d . . . . .
O8 O 0.2920(8) 1.1540(7) 0.5565(5) 0.028(3) Uani 1 1 d . . . . .
O1 O 0.1877(9) 1.2812(8) 0.8846(5) 0.035(3) Uani 1 1 d . . . . .
O11 O 0.3231(8) 0.8147(7) 0.6234(5) 0.031(3) Uani 1 1 d . . . . .
C24 C 0.1954(13) 1.2085(10) 0.6378(8) 0.029(4) Uani 1 1 d . . . . .
H24A H 0.1890 1.2475 0.6712 0.035 Uiso 1 1 calc R . . . .
H24B H 0.1379 1.2360 0.6112 0.035 Uiso 1 1 calc R . . . .
O6 O -0.0067(9) 1.2809(8) 0.8708(5) 0.038(3) Uani 1 1 d . . . . .
O4 O -0.0254(10) 1.1142(9) 1.0440(6) 0.042(3) Uani 1 1 d . . . . .
N3 N 0.4396(13) 0.9774(11) 0.6489(9) 0.047(4) Uani 1 1 d . . . . .
C34 C 0.3912(12) 0.7581(10) 0.5347(7) 0.028(4) Uani 1 1 d . U . . .
H34A H 0.4468 0.7139 0.5155 0.033 Uiso 1 1 calc R . . . .
H34B H 0.3276 0.7414 0.5282 0.033 Uiso 1 1 calc R . . . .
C21 C 0.3503(13) 1.1181(11) 0.4637(7) 0.032(4) Uani 1 1 d . U . . .
H21A H 0.2828 1.1513 0.4483 0.038 Uiso 1 1 calc R . . . .
H21B H 0.4011 1.1228 0.4333 0.038 Uiso 1 1 calc R . . . .
C16 C -0.1703(12) 1.2225(10) 1.0101(7) 0.024(3) Uani 1 1 d . U . . .
O3 O 0.1829(11) 1.0745(11) 1.0337(7) 0.064(4) Uani 1 1 d . U . . .
C19 C 0.0527(14) 1.2849(12) 0.8204(8) 0.036(4) Uani 1 1 d . . . . .
H19A H 0.0102 1.3212 0.7881 0.043 Uiso 1 1 calc R . . . .
H19B H 0.0831 1.2214 0.8083 0.043 Uiso 1 1 calc R . . . .
C27 C -0.0561(13) 1.1470(11) 0.7223(7) 0.031(4) Uani 1 1 d . U . . .
H27 H -0.1159 1.1946 0.7283 0.037 Uiso 1 1 calc R . . . .
N4 N 0.1258(13) 1.0012(11) 0.5531(7) 0.043(4) Uani 1 1 d . . . . .
C45 C 0.4810(14) 0.9908(12) 0.6900(9) 0.036(4) Uani 1 1 d . . . . .
C1 C 0.2608(12) 1.3146(12) 0.9036(7) 0.028(4) Uani 1 1 d . . . . .
C48 C -0.0629(12) 1.0371(12) 0.5822(9) 0.037(4) Uani 1 1 d . . . . .
H48A H -0.1004 1.0941 0.5604 0.055 Uiso 1 1 calc GR . . . .
H48B H -0.0699 1.0453 0.6241 0.055 Uiso 1 1 calc GR . . . .
H48C H -0.0896 0.9853 0.5731 0.055 Uiso 1 1 calc GR . . . .
C39 C 0.3007(12) 0.9985(12) 0.3818(8) 0.034(4) Uani 1 1 d . . . . .
H39 H 0.2872 1.0627 0.3697 0.040 Uiso 1 1 calc R . . . .
C2 C 0.3019(15) 1.3820(12) 0.8755(8) 0.041(5) Uani 1 1 d . . . . .
H2 H 0.2779 1.4084 0.8380 0.049 Uiso 1 1 calc R . . . .
C22 C 0.3708(13) 1.1583(11) 0.5168(8) 0.036(4) Uani 1 1 d . . . . .
H22A H 0.4364 1.1226 0.5336 0.043 Uiso 1 1 calc R . . . .
H22B H 0.3727 1.2236 0.5080 0.043 Uiso 1 1 calc R . . . .
C32 C 0.3165(14) 0.7963(12) 0.6835(8) 0.037(4) Uani 1 1 d . U . . .
H32A H 0.3695 0.8157 0.7036 0.045 Uiso 1 1 calc R . . . .
H32B H 0.3257 0.7290 0.6930 0.045 Uiso 1 1 calc R . . . .
C30 C 0.1160(11) 1.0078(10) 0.7034(7) 0.023(3) Uani 1 1 d . . . . .
C6 C 0.2945(13) 1.2804(12) 0.9612(8) 0.035(4) Uani 1 1 d . . . . .
N1 N 0.0125(13) 1.3378(11) 1.0091(8) 0.050(5) Uani 1 1 d . . . . .
C40 C 0.3362(12) 0.9692(11) 0.4377(8) 0.029(4) Uani 1 1 d . . . . .
C37 C 0.3010(13) 0.8466(13) 0.3616(7) 0.033(4) Uani 1 1 d . . . . .
H37 H 0.2893 0.8046 0.3353 0.040 Uiso 1 1 calc R . . . .
C14 C -0.3046(14) 1.2828(12) 1.0728(9) 0.040(5) Uani 1 1 d . . . . .
H14 H -0.3691 1.3238 1.0785 0.048 Uiso 1 1 calc R . . . .
C31 C 0.2111(13) 0.8515(11) 0.7034(8) 0.033(4) Uani 1 1 d . U . . .
H31A H 0.1578 0.8348 0.6820 0.040 Uiso 1 1 calc R . . . .
H31B H 0.2018 0.8383 0.7457 0.040 Uiso 1 1 calc R . . . .
C26 C 0.0234(13) 1.1694(12) 0.6947(8) 0.034(4) Uani 1 1 d . . . . .
H26 H 0.0181 1.2326 0.6825 0.041 Uiso 1 1 calc R . . . .
C38 C 0.2844(13) 0.9398(12) 0.3440(8) 0.036(4) Uani 1 1 d . . . . .
H38 H 0.2617 0.9621 0.3056 0.043 Uiso 1 1 calc R . . . .
C11 C -0.1183(13) 1.1687(11) 1.0570(7) 0.033(4) Uani 1 1 d . . . . .
C33 C 0.4114(13) 0.7560(11) 0.5993(8) 0.037(4) Uani 1 1 d . . . . .
H33A H 0.4241 0.6919 0.6175 0.044 Uiso 1 1 calc R . . . .
H33B H 0.4708 0.7794 0.6058 0.044 Uiso 1 1 calc R . . . .
C47 C 0.0395(14) 1.0177(11) 0.5665(8) 0.036(4) Uani 1 1 d . . . . .
C23 C 0.2918(12) 1.2047(10) 0.6066(7) 0.027(4) Uani 1 1 d . . . . .
H23A H 0.2970 1.2682 0.5948 0.032 Uiso 1 1 calc R . . . .
H23B H 0.3495 1.1731 0.6322 0.032 Uiso 1 1 calc R . . . .
C29 C 0.0383(12) 0.9866(11) 0.7329(7) 0.029(4) Uani 1 1 d . . . . .
H29 H 0.0443 0.9244 0.7476 0.035 Uiso 1 1 calc R . . . .
N2 N 0.1486(14) 1.0702(12) 0.8954(9) 0.061(5) Uani 1 1 d . . . . .
C36 C 0.3349(14) 0.8144(12) 0.4180(8) 0.036(4) Uani 1 1 d . . . . .
H36 H 0.3461 0.7502 0.4295 0.044 Uiso 1 1 calc R . . . .
C7 C 0.2919(13) 1.1701(13) 1.0440(7) 0.033(4) Uani 1 1 d . . . . .
H7A H 0.3552 1.1222 1.0371 0.040 Uiso 1 1 calc R . . . .
H7B H 0.3069 1.2148 1.0697 0.040 Uiso 1 1 calc R . . . .
C15 C -0.2647(13) 1.2797(13) 1.0175(9) 0.042(5) Uani 1 1 d . . . . .
H15 H -0.3013 1.3161 0.9855 0.051 Uiso 1 1 calc R . . . .
C3 C 0.3748(16) 1.4104(13) 0.9005(9) 0.047(5) Uani 1 1 d . . . . .
H3 H 0.4017 1.4561 0.8802 0.057 Uiso 1 1 calc R . . . .
C35 C 0.3527(12) 0.8723(11) 0.4572(7) 0.029(4) Uani 1 1 d . . . . .
C50 C 0.4694(19) 1.3194(13) 0.6778(10) 0.059(7) Uani 1 1 d . . . . .
H50A H 0.4871 1.2824 0.6439 0.089 Uiso 1 1 calc GR . . . .
H50B H 0.5310 1.3216 0.6974 0.089 Uiso 1 1 calc GR . . . .
H50C H 0.4311 1.3826 0.6649 0.089 Uiso 1 1 calc GR . . . .
C43 C 0.2072(15) 1.0541(12) 0.8595(11) 0.050(6) Uani 1 1 d . . . . .
C5 C 0.3694(16) 1.3095(13) 0.9851(9) 0.046(5) Uani 1 1 d . . . . .
H5 H 0.3938 1.2852 1.0229 0.055 Uiso 1 1 calc R . . . .
N7 N 0.7078(14) 1.1178(15) 0.8085(9) 0.068(6) Uani 1 1 d . . . . .
C25 C 0.1108(12) 1.1037(12) 0.6839(7) 0.029(4) Uani 1 1 d . . . . .
C49 C 0.4089(16) 1.2776(15) 0.7177(10) 0.048(6) Uani 1 1 d . . . . .
C18 C -0.0944(14) 1.2508(14) 0.8592(8) 0.043(5) Uani 1 1 d . . . . .
H18A H -0.0741 1.1839 0.8524 0.051 Uiso 1 1 calc R . . . .
H18B H -0.1277 1.2853 0.8234 0.051 Uiso 1 1 calc R . . . .
C12 C -0.1642(15) 1.1718(14) 1.1125(8) 0.042(5) Uani 1 1 d . . . . .
H12 H -0.1310 1.1336 1.1449 0.050 Uiso 1 1 calc R . . . .
C20 C 0.1340(14) 1.3302(13) 0.8335(7) 0.039(5) Uani 1 1 d . . . . .
H20A H 0.1808 1.3274 0.8000 0.046 Uiso 1 1 calc R . . . .
H20B H 0.1041 1.3962 0.8406 0.046 Uiso 1 1 calc R . . . .
N6 N 0.3642(16) 1.2401(16) 0.7488(10) 0.071(6) Uani 1 1 d . . . . .
C17 C -0.1667(15) 1.2665(13) 0.9087(8) 0.042(5) Uani 1 1 d . . . . .
H17A H -0.1863 1.3330 0.9167 0.050 Uiso 1 1 calc R . . . .
H17B H -0.2281 1.2480 0.8995 0.050 Uiso 1 1 calc R . . . .
C51 C 0.6431(18) 1.1648(16) 0.8278(10) 0.058(6) Uani 1 1 d . . . . .
C10 C 0.0351(16) 1.0571(14) 1.0894(10) 0.055(6) Uani 1 1 d . . . . .
H10A H 0.0017 1.0101 1.1063 0.065 Uiso 1 1 calc R . . . .
H10B H 0.0453 1.0954 1.1207 0.065 Uiso 1 1 calc R . . . .
N5 N 0.4744(18) 1.0311(16) 0.9119(11) 0.081(7) Uani 1 1 d . . . . .
C13 C -0.2577(14) 1.2314(14) 1.1186(9) 0.043(5) Uani 1 1 d . . . . .
H13 H -0.2892 1.2359 1.1558 0.051 Uiso 1 1 calc R . . . .
C4 C 0.4104(18) 1.3750(15) 0.9541(9) 0.054(6) Uani 1 1 d . . . . .
H4 H 0.4632 1.3946 0.9707 0.065 Uiso 1 1 calc R . . . .
C28 C -0.0517(13) 1.0556(13) 0.7421(7) 0.035(4) Uani 1 1 d . . . . .
H28 H -0.1077 1.0403 0.7612 0.042 Uiso 1 1 calc R . . . .
C41 C -0.0514(17) 1.3961(15) 1.0236(9) 0.047(5) Uani 1 1 d . . . . .
C8 C 0.2203(18) 1.1278(16) 1.0713(10) 0.056(6) Uani 1 1 d . U . . .
H8A H 0.1634 1.1768 1.0855 0.068 Uiso 1 1 calc R . . . .
H8B H 0.2519 1.0872 1.1054 0.068 Uiso 1 1 calc R . . . .
C9 C 0.1316(15) 1.0114(14) 1.0635(10) 0.048(5) Uani 1 1 d . U . . .
H9A H 0.1760 0.9738 1.0946 0.058 Uiso 1 1 calc R . . . .
H9B H 0.1202 0.9684 1.0354 0.058 Uiso 1 1 calc R . . . .
C46 C 0.5310(14) 1.0027(15) 0.7398(9) 0.047(5) Uani 1 1 d . . . . .
H46A H 0.5546 1.0589 0.7335 0.071 Uiso 1 1 calc GR . . . .
H46B H 0.5887 0.9488 0.7477 0.071 Uiso 1 1 calc GR . . . .
H46C H 0.4847 1.0089 0.7731 0.071 Uiso 1 1 calc GR . . . .
C44 C 0.2845(15) 1.0389(17) 0.8151(11) 0.064(7) Uani 1 1 d . . . . .
H44A H 0.2534 1.0417 0.7769 0.096 Uiso 1 1 calc GR . . . .
H44B H 0.3317 0.9777 0.8231 0.096 Uiso 1 1 calc GR . . . .
H44C H 0.3207 1.0870 0.8152 0.096 Uiso 1 1 calc GR . . . .
C53 C 0.4360(19) 0.981(2) 0.9398(12) 0.070(8) Uani 1 1 d . . . . .
C42 C -0.1327(19) 1.4718(14) 1.0438(11) 0.070(7) Uani 1 1 d . . . . .
H42A H -0.1784 1.4995 1.0114 0.105 Uiso 1 1 calc GR . . . .
H42B H -0.1043 1.5192 1.0584 0.105 Uiso 1 1 calc GR . . . .
H42C H -0.1700 1.4475 1.0752 0.105 Uiso 1 1 calc GR . . . .
C52 C 0.5532(19) 1.229(2) 0.8562(14) 0.089(10) Uani 1 1 d . . . . .
H52A H 0.5056 1.2627 0.8260 0.134 Uiso 1 1 calc GR . . . .
H52B H 0.5759 1.2730 0.8781 0.134 Uiso 1 1 calc GR . . . .
H52C H 0.5200 1.1918 0.8828 0.134 Uiso 1 1 calc GR . . . .
C54 C 0.385(2) 0.9159(19) 0.9714(13) 0.075(8) Uani 1 1 d . . . . .
H54A H 0.3201 0.9210 0.9526 0.112 Uiso 1 1 calc GR . . . .
H54B H 0.3730 0.9317 1.0119 0.112 Uiso 1 1 calc GR . . . .
H54C H 0.4272 0.8522 0.9703 0.112 Uiso 1 1 calc GR . . . .


_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
Bi2 I11 3.4261(13) 2_566 ?
Bi2 I8 3.1895(13) . ?
Bi2 I5 3.0512(12) . ?
Bi2 I4 2.9876(13) . ?
Bi2 I7 3.1526(11) . ?
Bi2 I6 2.8508(13) . ?
Bi3 I11 3.1312(13) . ?
Bi3 I8 3.2238(12) . ?
Bi3 I8 3.4068(13) 2_566 ?
Bi3 I7 3.0712(13) . ?
Bi3 I10 2.9709(12) . ?
Bi3 I9 2.8445(13) . ?
Bi4 I11 3.3903(12) . ?
Bi4 I10 3.3201(14) . ?
Bi4 I14 2.9278(14) . ?
Bi4 I12 2.8482(13) . ?
Bi4 I13 2.8573(13) . ?
Bi1 I5 3.4240(13) . ?
Bi1 I4 3.4070(12) . ?
Bi1 I2 2.8878(12) . ?
Bi1 I3 2.8702(14) . ?
Bi1 I1 2.8566(13) . ?
I11 Bi2 3.4261(13) 2_566 ?
I8 Bi3 3.4067(13) 2_566 ?
Na2 O9 2.760(12) . ?
Na2 O7 2.615(13) . ?
Na2 O10 2.750(14) . ?
Na2 O12 2.700(12) . ?
Na2 O8 2.597(12) . ?
Na2 O11 2.521(12) . ?
Na2 N3 2.47(2) . ?
Na2 N4 2.414(18) . ?
Na1 O2 2.519(14) . ?
Na1 O5 2.732(14) . ?
Na1 O1 2.683(15) . ?
Na1 O6 2.509(14) . ?
Na1 O4 2.827(16) . ?
Na1 O3 2.518(16) . ?
Na1 N1 2.429(16) . ?
Na1 N2 2.468(18) . ?
O9 C24 1.434(18) . ?
O9 C25 1.341(19) . ?
O7 C21 1.463(19) . ?
O7 C40 1.361(19) . ?
O10 C30 1.373(16) . ?
O10 C31 1.455(19) . ?
O2 C6 1.35(2) . ?
O2 C7 1.450(19) . ?
O5 C16 1.387(19) . ?
O5 C17 1.42(2) . ?
O12 C34 1.436(18) . ?
O12 C35 1.332(19) . ?
O8 C22 1.41(2) . ?
O8 C23 1.428(19) . ?
O1 C1 1.33(2) . ?
O1 C20 1.445(19) . ?
O11 C32 1.39(2) . ?
O11 C33 1.428(18) . ?
C24 C23 1.48(2) . ?
O6 C19 1.41(2) . ?
O6 C18 1.44(2) . ?
O4 C11 1.36(2) . ?
O4 C10 1.43(2) . ?
N3 C45 1.17(2) . ?
C34 C33 1.52(2) . ?
C21 C22 1.47(2) . ?
C16 C11 1.39(2) . ?
C16 C15 1.37(2) . ?
O3 C8 1.41(3) . ?
O3 C9 1.45(2) . ?
C19 C20 1.50(3) . ?
C27 C26 1.36(3) . ?
C27 C28 1.40(2) . ?
N4 C47 1.19(2) . ?
C45 C46 1.40(3) . ?
C1 C2 1.40(3) . ?
C1 C6 1.42(2) . ?
C48 C47 1.41(2) . ?
C39 C40 1.38(2) . ?
C39 C38 1.35(2) . ?
C2 C3 1.35(3) . ?
C32 C31 1.55(2) . ?
C30 C29 1.35(2) . ?
C30 C25 1.45(2) . ?
C6 C5 1.36(3) . ?
N1 C41 1.13(2) . ?
C40 C35 1.44(2) . ?
C37 C38 1.38(2) . ?
C37 C36 1.40(2) . ?
C14 C15 1.37(3) . ?
C14 C13 1.33(3) . ?
C26 C25 1.37(2) . ?
C11 C12 1.41(2) . ?
C29 C28 1.41(2) . ?
N2 C43 1.14(3) . ?
C36 C35 1.37(2) . ?
C7 C8 1.42(3) . ?
C3 C4 1.35(3) . ?
C50 C49 1.44(3) . ?
C43 C44 1.44(3) . ?
C5 C4 1.40(3) . ?
N7 C51 1.09(3) . ?
C49 N6 1.15(3) . ?
C18 C17 1.49(3) . ?
C12 C13 1.37(3) . ?
C51 C52 1.52(3) . ?
C10 C9 1.46(3) . ?
N5 C53 1.17(4) . ?
C41 C42 1.46(3) . ?
C53 C54 1.49(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
I8 Bi2 I11 84.39(3) . 2_566 ?
I5 Bi2 I11 90.56(3) . 2_566 ?
I5 Bi2 I8 86.06(3) . . ?
I5 Bi2 I7 170.42(4) . . ?
I4 Bi2 I11 87.34(3) . 2_566 ?
I4 Bi2 I8 171.51(4) . . ?
I4 Bi2 I5 92.12(3) . . ?
I4 Bi2 I7 94.45(3) . . ?
I7 Bi2 I11 82.80(3) . 2_566 ?
I7 Bi2 I8 86.42(3) . . ?
I6 Bi2 I11 174.82(4) . 2_566 ?
I6 Bi2 I8 94.91(4) . . ?
I6 Bi2 I5 94.52(3) . . ?
I6 Bi2 I4 93.51(4) . . ?
I6 Bi2 I7 92.03(4) . . ?
I11 Bi3 I8 88.28(3) . . ?
I11 Bi3 I8 85.60(3) . 2_566 ?
I8 Bi3 I8 86.29(3) . 2_566 ?
I7 Bi3 I11 170.60(4) . . ?
I7 Bi3 I8 85.89(3) . 2_566 ?
I7 Bi3 I8 87.20(3) . . ?
I10 Bi3 I11 93.99(3) . . ?
I10 Bi3 I8 171.43(4) . . ?
I10 Bi3 I8 85.64(3) . 2_566 ?
I10 Bi3 I7 89.33(3) . . ?
I9 Bi3 I11 92.21(4) . . ?
I9 Bi3 I8 177.19(4) . 2_566 ?
I9 Bi3 I8 91.89(4) . . ?
I9 Bi3 I7 96.16(4) . . ?
I9 Bi3 I10 96.27(4) . . ?
I10 Bi4 I11 83.39(3) . . ?
I14 Bi4 I11 92.65(4) . . ?
I14 Bi4 I10 172.90(4) . . ?
I12 Bi4 I11 91.41(3) . . ?
I12 Bi4 I10 92.02(4) . . ?
I12 Bi4 I14 93.98(4) . . ?
I12 Bi4 I13 98.92(4) . . ?
I13 Bi4 I11 165.91(4) . . ?
I13 Bi4 I10 86.69(4) . . ?
I13 Bi4 I14 96.13(4) . . ?
I4 Bi1 I5 79.08(3) . . ?
I2 Bi1 I5 87.50(4) . . ?
I2 Bi1 I4 166.53(4) . . ?
I3 Bi1 I5 101.22(4) . . ?
I3 Bi1 I4 84.96(3) . . ?
I3 Bi1 I2 96.70(4) . . ?
I1 Bi1 I5 163.77(4) . . ?
I1 Bi1 I4 98.26(3) . . ?
I1 Bi1 I2 94.94(4) . . ?
I1 Bi1 I3 94.45(4) . . ?
Bi3 I11 Bi2 95.30(3) . 2_566 ?
Bi3 I11 Bi4 88.81(3) . . ?
Bi4 I11 Bi2 90.42(3) . 2_566 ?
Bi2 I8 Bi3 94.61(3) . 2_566 ?
Bi2 I8 Bi3 90.75(3) . . ?
Bi3 I8 Bi3 93.71(3) . 2_566 ?
Bi2 I5 Bi1 93.39(3) . . ?
Bi2 I4 Bi1 94.89(3) . . ?
Bi3 I7 Bi2 94.33(3) . . ?
Bi3 I10 Bi4 92.93(3) . . ?
O7 Na2 O9 123.4(4) . . ?
O7 Na2 O10 172.2(4) . . ?
O7 Na2 O12 56.3(3) . . ?
O10 Na2 O9 54.2(3) . . ?
O12 Na2 O9 176.5(4) . . ?
O12 Na2 O10 125.4(4) . . ?
O8 Na2 O9 61.9(4) . . ?
O8 Na2 O7 62.8(4) . . ?
O8 Na2 O10 116.1(4) . . ?
O8 Na2 O12 118.5(4) . . ?
O11 Na2 O9 117.0(4) . . ?
O11 Na2 O7 119.5(4) . . ?
O11 Na2 O10 63.0(4) . . ?
O11 Na2 O12 63.2(4) . . ?
O11 Na2 O8 171.1(5) . . ?
N3 Na2 O9 82.9(5) . . ?
N3 Na2 O7 105.0(5) . . ?
N3 Na2 O10 82.4(5) . . ?
N3 Na2 O12 100.5(5) . . ?
N3 Na2 O8 86.9(5) . . ?
N3 Na2 O11 84.3(5) . . ?
N4 Na2 O9 80.5(5) . . ?
N4 Na2 O7 91.8(5) . . ?
N4 Na2 O10 80.5(5) . . ?
N4 Na2 O12 96.0(5) . . ?
N4 Na2 O8 93.4(5) . . ?
N4 Na2 O11 95.1(5) . . ?
N4 Na2 N3 161.0(6) . . ?
O2 Na1 O5 161.2(5) . . ?
O2 Na1 O1 59.9(4) . . ?
O2 Na1 O4 118.8(4) . . ?
O5 Na1 O4 53.9(4) . . ?
O1 Na1 O5 126.5(4) . . ?
O1 Na1 O4 177.3(4) . . ?
O6 Na1 O2 121.4(5) . . ?
O6 Na1 O5 64.3(4) . . ?
O6 Na1 O1 62.7(4) . . ?
O6 Na1 O4 118.0(5) . . ?
O6 Na1 O3 164.3(6) . . ?
O3 Na1 O2 64.7(5) . . ?
O3 Na1 O5 115.2(5) . . ?
O3 Na1 O1 117.8(5) . . ?
O3 Na1 O4 62.4(5) . . ?
N1 Na1 O2 85.1(6) . . ?
N1 Na1 O5 77.2(5) . . ?
N1 Na1 O1 92.8(5) . . ?
N1 Na1 O6 86.7(5) . . ?
N1 Na1 O4 84.7(5) . . ?
N1 Na1 O3 108.7(6) . . ?
N1 Na1 N2 170.2(7) . . ?
N2 Na1 O2 97.7(6) . . ?
N2 Na1 O5 100.9(6) . . ?
N2 Na1 O1 80.6(6) . . ?
N2 Na1 O6 83.8(6) . . ?
N2 Na1 O4 102.1(6) . . ?
N2 Na1 O3 80.9(7) . . ?
C24 O9 Na2 114.1(9) . . ?
C25 O9 Na2 117.5(9) . . ?
C25 O9 C24 117.2(12) . . ?
C21 O7 Na2 116.9(9) . . ?
C40 O7 Na2 116.7(10) . . ?
C40 O7 C21 117.1(13) . . ?
C30 O10 Na2 118.0(9) . . ?
C30 O10 C31 113.0(12) . . ?
C31 O10 Na2 113.0(9) . . ?
C6 O2 Na1 123.4(11) . . ?
C6 O2 C7 120.5(13) . . ?
C7 O2 Na1 115.3(10) . . ?
C16 O5 Na1 117.8(10) . . ?
C16 O5 C17 115.9(12) . . ?
C17 O5 Na1 113.3(11) . . ?
C34 O12 Na2 114.2(9) . . ?
C35 O12 Na2 114.1(9) . . ?
C35 O12 C34 115.5(12) . . ?
C22 O8 Na2 110.1(9) . . ?
C22 O8 C23 113.6(12) . . ?
C23 O8 Na2 111.4(9) . . ?
C1 O1 Na1 119.9(10) . . ?
C1 O1 C20 116.2(14) . . ?
C20 O1 Na1 116.6(10) . . ?
C32 O11 Na2 117.4(9) . . ?
C32 O11 C33 112.0(12) . . ?
C33 O11 Na2 111.9(9) . . ?
O9 C24 C23 108.1(12) . . ?
C19 O6 Na1 116.4(10) . . ?
C19 O6 C18 111.9(14) . . ?
C18 O6 Na1 112.0(10) . . ?
C11 O4 Na1 114.9(10) . . ?
C11 O4 C10 119.4(15) . . ?
C10 O4 Na1 114.1(12) . . ?
C45 N3 Na2 157.1(15) . . ?
O12 C34 C33 105.6(13) . . ?
O7 C21 C22 106.4(14) . . ?
O5 C16 C11 113.7(14) . . ?
C15 C16 O5 125.8(15) . . ?
C15 C16 C11 120.5(16) . . ?
C8 O3 Na1 102.4(12) . . ?
C8 O3 C9 114.0(18) . . ?
C9 O3 Na1 117.8(12) . . ?
O6 C19 C20 109.0(15) . . ?
C26 C27 C28 121.4(15) . . ?
C47 N4 Na2 146.1(14) . . ?
N3 C45 C46 178(2) . . ?
O1 C1 C2 127.7(16) . . ?
O1 C1 C6 114.5(16) . . ?
C2 C1 C6 117.7(17) . . ?
C38 C39 C40 122.7(16) . . ?
C3 C2 C1 121.3(19) . . ?
O8 C22 C21 106.9(14) . . ?
O11 C32 C31 107.7(13) . . ?
O10 C30 C25 111.7(13) . . ?
C29 C30 O10 127.9(13) . . ?
C29 C30 C25 120.3(13) . . ?
O2 C6 C1 117.5(16) . . ?
O2 C6 C5 122.9(17) . . ?
C5 C6 C1 119.6(18) . . ?
C41 N1 Na1 154.2(17) . . ?
O7 C40 C39 128.7(15) . . ?
O7 C40 C35 112.4(15) . . ?
C39 C40 C35 118.8(15) . . ?
C38 C37 C36 119.8(16) . . ?
C13 C14 C15 123.5(18) . . ?
O10 C31 C32 105.7(14) . . ?
C27 C26 C25 122.0(17) . . ?
C39 C38 C37 119.3(17) . . ?
O4 C11 C16 114.9(15) . . ?
O4 C11 C12 125.5(15) . . ?
C16 C11 C12 119.5(15) . . ?
O11 C33 C34 105.9(14) . . ?
N4 C47 C48 180(2) . . ?
O8 C23 C24 106.9(13) . . ?
C30 C29 C28 121.0(15) . . ?
C43 N2 Na1 137.0(17) . . ?
C35 C36 C37 122.2(17) . . ?
C8 C7 O2 109.2(15) . . ?
C16 C15 C14 117.7(17) . . ?
C2 C3 C4 121.1(19) . . ?
O12 C35 C40 114.2(14) . . ?
O12 C35 C36 128.7(16) . . ?
C36 C35 C40 117.1(16) . . ?
N2 C43 C44 176(2) . . ?
C6 C5 C4 120(2) . . ?
O9 C25 C30 114.2(13) . . ?
O9 C25 C26 128.5(16) . . ?
C26 C25 C30 117.3(15) . . ?
N6 C49 C50 177(2) . . ?
O6 C18 C17 111.0(16) . . ?
C13 C12 C11 118.4(17) . . ?
O1 C20 C19 108.3(15) . . ?
O5 C17 C18 107.2(14) . . ?
N7 C51 C52 178(3) . . ?
O4 C10 C9 107.3(19) . . ?
C14 C13 C12 120.3(19) . . ?
C3 C4 C5 120(2) . . ?
C27 C28 C29 117.9(16) . . ?
N1 C41 C42 178(2) . . ?
C7 C8 O3 113.1(18) . . ?
O3 C9 C10 114.3(17) . . ?
N5 C53 C54 176(3) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound3
_database_code_depnum_ccdc_archive 'CCDC 1050431'
_audit_update_record             
;
2015-04-02 deposited with the CCDC.
2015-04-29 downloaded from the CCDC.
;
_audit_creation_date             2015-03-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Bi6 I20, 2(C24 H30 N2 Na O6), 3(C2 H3 N)'
_chemical_formula_sum            'C54 H69 Bi6 I20 N7 Na2 O12'
_chemical_formula_weight         4846.02
_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 0.0033 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'
I I -0.4742 1.8119 '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'
Na Na 0.0362 0.0249 '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'

_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.
;
_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                   14.372(3)
_cell_length_b                   19.388(3)
_cell_length_c                   19.648(4)
_cell_angle_alpha                96.034(5)
_cell_angle_beta                 100.883(5)
_cell_angle_gamma                102.490(5)
_cell_volume                     5187.9(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9760
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.319
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    16.146
_exptl_absorpt_correction_T_max  0.745196
_exptl_absorpt_correction_T_min  0.394403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1709 before and 0.0511 after correction.
 The Ratio of minimum to maximum transmission not present.
 The λ/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1704 before and 0.0577 after correction.
 The Ratio of minimum to maximum transmission is 0.53.
 The λ/2 correction factor is Not present

Final HKLF 4 output contains 103600 reflections, Rint = 0.0566
 (61448 with I > 3sig(I), Rint = 0.0469)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.102
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4236
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.151
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.132
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            103600
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.437
_diffrn_reflns_theta_min         2.321
_diffrn_ambient_temperature      100.02
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.986
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 QUEST area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean 10.4167
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                15244
_reflns_number_total             18828
_reflns_special_details          
;
 _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       ?
_computing_data_collection       'Bruker APEX2 v2014.11-0'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         3.734
_refine_diff_density_min         -1.763
_refine_diff_density_rms         0.371
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     873
_refine_ls_number_reflns         18828
_refine_ls_number_restraints     120
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0576
_refine_ls_restrained_S_all      1.116
_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)+(0.0202P)²+220.5093P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1205
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.6323(9) 0.3677(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C22) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C45)
\\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C29) \\sim Ueq,
Uanis(C40) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C3) \\sim Ueq,
Uanis(C13) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C33) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C21(H21A,H21B), C32(H32A,H32B), C31(H31A,H31B), C13(H13A,
 H13B), C22(H22A,H22B), C24(H24A,H24B), C11(H11A,H11B), C12(H12A,H12B), C4(H4A,
 H4B), C23(H23A,H23B), C33(H33A,H33B), C14(H14A,H14B), C2(H2A,H2B), C3(H3A,H3B),
  C1(H1A,H1B)
4.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C39(H39), C27(H27), C37(H37), C17(H17), C29(H29), C26(H26),
 C18(H18), C16(H16), C6(H6), C36(H36), C8(H8), C9(H9), C28(H28), C38(H38),
 C7(H7)
4.c Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C42(H42A,H42B,
 H42C), C54(H54A,H54B,H54C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C)
;
_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 0.54598(6) 0.72964(4) 0.30131(4) 0.01909(17) Uani 1 1 d . . . . .
Bi4 Bi 1.05184(6) 0.80435(4) 0.23559(4) 0.01767(17) Uani 1 1 d . . . . .
Bi6 Bi 1.22510(6) 0.63641(4) 0.22176(4) 0.02146(19) Uani 1 1 d . . . . .
Bi3 Bi 0.72985(6) 0.72459(4) 0.13808(4) 0.02028(18) Uani 1 1 d . . . . .
Bi5 Bi 1.38023(6) 0.90297(4) 0.31597(4) 0.02022(18) Uani 1 1 d . . . . .
Bi2 Bi 0.86906(6) 0.80028(4) 0.40004(4) 0.01922(18) Uani 1 1 d . . . . .
I16 I 1.08011(10) 0.69294(7) 0.12059(7) 0.0203(3) Uani 1 1 d . . . . .
I15 I 1.20700(10) 0.76499(7) 0.34317(7) 0.0171(3) Uani 1 1 d . . . . .
I7 I 0.57278(10) 0.61764(7) 0.18686(7) 0.0202(3) Uani 1 1 d . . . . .
I12 I 0.89346(10) 0.68483(7) 0.26629(7) 0.0187(3) Uani 1 1 d . . . . .
I5 I 0.71024(10) 0.84339(7) 0.27015(7) 0.0186(3) Uani 1 1 d . . . . .
I2 I 0.40037(10) 0.77185(7) 0.19113(7) 0.0205(3) Uani 1 1 d . . . . .
I1 I 0.52520(11) 0.84206(8) 0.41430(7) 0.0235(3) Uani 1 1 d . . . . .
I9 I 1.02470(10) 0.91208(7) 0.35064(7) 0.0204(3) Uani 1 1 d . . . . .
I11 I 0.90519(11) 0.84289(7) 0.11894(8) 0.0237(3) Uani 1 1 d . . . . .
I6 I 0.69277(10) 0.68343(7) 0.41354(7) 0.0205(3) Uani 1 1 d . . . . .
I3 I 0.38991(10) 0.61160(7) 0.33678(8) 0.0226(3) Uani 1 1 d . . . . .
I14 I 1.21014(10) 0.92224(7) 0.20080(8) 0.0228(3) Uani 1 1 d . . . . .
I20 I 1.24633(12) 0.53234(8) 0.11336(8) 0.0288(3) Uani 1 1 d . . . . .
I13 I 0.74619(12) 0.61526(8) 0.03339(8) 0.0322(4) Uani 1 1 d . . . . .
I8 I 0.59281(12) 0.77512(8) 0.04649(8) 0.0318(4) Uani 1 1 d . . . . .
I4 I 0.84827(11) 0.90262(8) 0.50841(8) 0.0297(3) Uani 1 1 d . . . . .
I17 I 1.07852(12) 0.54066(9) 0.26614(9) 0.0351(4) Uani 1 1 d . . . . .
I10 I 1.00903(11) 0.74732(9) 0.48699(9) 0.0353(4) Uani 1 1 d . . . . .
I18 I 1.34162(12) 0.99103(8) 0.42662(9) 0.0378(4) Uani 1 1 d . . . . .
I19 I 1.53083(11) 1.01238(8) 0.28701(8) 0.0315(3) Uani 1 1 d . . . . .
Na1 Na 0.9315(6) 1.1570(4) 0.1373(4) 0.0255(19) Uani 1 1 d . . . . .
Na2 Na 0.5472(7) 0.3502(4) 0.3491(4) 0.0265(19) Uani 1 1 d . . . . .
O1 O 1.1003(11) 1.2369(7) 0.1353(7) 0.024(3) Uani 1 1 d . . . . .
O7 O 0.7249(10) 0.4386(7) 0.3514(7) 0.022(3) Uani 1 1 d . . . . .
O2 O 0.9281(11) 1.2559(8) 0.0582(8) 0.026(3) Uani 1 1 d . . . . .
O4 O 0.7528(11) 1.0613(7) 0.1266(8) 0.026(4) Uani 1 1 d . . . . .
O9 O 0.3855(10) 0.3608(7) 0.2708(7) 0.022(3) Uani 1 1 d . . . . .
O6 O 1.0944(11) 1.1493(8) 0.2217(7) 0.023(3) Uani 1 1 d . . . . .
O3 O 0.7556(11) 1.1575(8) 0.0481(7) 0.027(4) Uani 1 1 d . . . . .
O11 O 0.5453(10) 0.2515(8) 0.4307(7) 0.023(3) Uani 1 1 d . . . . .
O8 O 0.5610(12) 0.4363(8) 0.2542(8) 0.030(4) Uani 1 1 d . . . . .
O10 O 0.3765(10) 0.2707(8) 0.3542(8) 0.026(3) Uani 1 1 d . . . . .
O12 O 0.7170(11) 0.3491(8) 0.4351(8) 0.027(3) Uani 1 1 d . . . . .
O5 O 0.9180(10) 1.0660(7) 0.2257(8) 0.025(3) Uani 1 1 d . . . . .
N4 N 0.5868(15) 0.2648(10) 0.2657(10) 0.030(4) Uani 1 1 d . . . . .
C30 C 0.2949(15) 0.2960(11) 0.3412(11) 0.023(5) Uani 1 1 d . . . . .
C25 C 0.3006(16) 0.3458(11) 0.2946(11) 0.023(5) Uani 1 1 d . . . . .
N1 N 0.8929(14) 1.2396(10) 0.2238(10) 0.031(4) Uani 1 1 d . U . . .
C19 C 1.2654(15) 1.2286(11) 0.1212(11) 0.022(5) Uani 1 1 d . U . . .
H19 H 1.2683 1.2609 0.0881 0.026 Uiso 1 1 calc R . . . .
C34 C 0.7102(17) 0.2968(11) 0.4814(11) 0.025(5) Uani 1 1 d . U . . .
H34A H 0.6916 0.3156 0.5244 0.030 Uiso 1 1 calc R . . . .
H34B H 0.7739 0.2847 0.4952 0.030 Uiso 1 1 calc R . . . .
C5 C 0.6947(15) 1.0931(10) 0.0161(11) 0.020(5) Uani 1 1 d . . . . .
C21 C 0.7269(16) 0.4869(12) 0.2983(12) 0.027(5) Uani 1 1 d . U . . .
H21A H 0.7111 0.5320 0.3152 0.032 Uiso 1 1 calc R . . . .
H21B H 0.7918 0.4983 0.2863 0.032 Uiso 1 1 calc R . . . .
C32 C 0.4664(15) 0.1927(11) 0.3982(10) 0.023(5) Uani 1 1 d . . . . .
H32A H 0.4674 0.1521 0.4248 0.028 Uiso 1 1 calc R . . . .
H32B H 0.4721 0.1770 0.3498 0.028 Uiso 1 1 calc R . . . .
C31 C 0.3729(16) 0.2155(11) 0.3966(11) 0.025(5) Uani 1 1 d . U . . .
H31A H 0.3159 0.1750 0.3761 0.030 Uiso 1 1 calc R . . . .
H31B H 0.3680 0.2336 0.4445 0.030 Uiso 1 1 calc R . . . .
C39 C 0.8490(18) 0.5292(12) 0.4367(15) 0.038(6) Uani 1 1 d . . . . .
H39 H 0.8499 0.5629 0.4049 0.045 Uiso 1 1 calc R . . . .
C35 C 0.7831(18) 0.4138(15) 0.4635(13) 0.036(6) Uani 1 1 d . . . . .
C10 C 0.6944(16) 1.0398(11) 0.0621(12) 0.026(5) Uani 1 1 d . . . . .
C13 C 0.9885(16) 1.0963(12) 0.2881(12) 0.026(5) Uani 1 1 d . U . . .
H13A H 0.9803 1.0656 0.3248 0.031 Uiso 1 1 calc R . . . .
H13B H 0.9807 1.1441 0.3054 0.031 Uiso 1 1 calc R . . . .
C27 C 0.1389(19) 0.3563(12) 0.3034(12) 0.034(6) Uani 1 1 d . . . . .
H27 H 0.0839 0.3754 0.2896 0.041 Uiso 1 1 calc R . . . .
C22 C 0.6532(16) 0.4471(12) 0.2387(12) 0.029(5) Uani 1 1 d . U . . .
H22A H 0.6545 0.4736 0.1984 0.034 Uiso 1 1 calc R . . . .
H22B H 0.6672 0.4003 0.2255 0.034 Uiso 1 1 calc R . . . .
C24 C 0.3893(17) 0.4072(12) 0.2188(12) 0.029(5) Uani 1 1 d . . . . .
H24A H 0.3888 0.4561 0.2388 0.035 Uiso 1 1 calc R . . . .
H24B H 0.3328 0.3893 0.1787 0.035 Uiso 1 1 calc R . . . .
C37 C 0.902(2) 0.4993(14) 0.5471(13) 0.040(6) Uani 1 1 d . . . . .
H37 H 0.9407 0.5122 0.5935 0.048 Uiso 1 1 calc R . . . .
N7 N 1.2162(15) 0.8318(11) 0.6394(11) 0.042(5) Uiso 1 1 d . . . . .
C17 C 1.3422(16) 1.1539(11) 0.1901(11) 0.028(5) Uani 1 1 d . . . . .
H17 H 1.3969 1.1346 0.2043 0.034 Uiso 1 1 calc R . . . .
C29 C 0.2123(15) 0.2768(11) 0.3681(10) 0.021(4) Uani 1 1 d . U . . .
H29 H 0.2080 0.2417 0.3985 0.026 Uiso 1 1 calc R . . . .
C15 C 1.1773(18) 1.1638(12) 0.1975(12) 0.031(6) Uani 1 1 d . . . . .
C26 C 0.2232(17) 0.3767(11) 0.2755(13) 0.031(6) Uani 1 1 d . . . . .
H26 H 0.2264 0.4109 0.2442 0.037 Uiso 1 1 calc R . . . .
C11 C 0.7530(18) 1.0073(11) 0.1691(15) 0.039(6) Uani 1 1 d . . . . .
H11A H 0.7754 0.9675 0.1469 0.047 Uiso 1 1 calc R . . . .
H11B H 0.6866 0.9884 0.1766 0.047 Uiso 1 1 calc R . . . .
C41 C 0.8817(15) 1.2798(11) 0.2653(11) 0.024(5) Uani 1 1 d . U . . .
C12 C 0.8213(16) 1.0414(12) 0.2367(12) 0.027(5) Uani 1 1 d . U . . .
H12A H 0.7993 1.0822 0.2574 0.032 Uiso 1 1 calc R . . . .
H12B H 0.8215 1.0064 0.2699 0.032 Uiso 1 1 calc R . . . .
C18 C 1.3417(18) 1.1997(11) 0.1412(11) 0.029(5) Uani 1 1 d . . . . .
H18 H 1.3969 1.2114 0.1209 0.035 Uiso 1 1 calc R . . . .
C4 C 0.7609(17) 1.2131(12) 0.0069(12) 0.031(5) Uani 1 1 d . . . . .
H4A H 0.6976 1.2264 -0.0033 0.037 Uiso 1 1 calc R . . . .
H4B H 0.7773 1.1977 -0.0381 0.037 Uiso 1 1 calc R . . . .
C16 C 1.2586(15) 1.1369(11) 0.2182(11) 0.024(5) Uani 1 1 d . . . . .
H16 H 1.2577 1.1059 0.2526 0.029 Uiso 1 1 calc R . . . .
N2 N 0.9385(17) 1.0674(12) 0.0471(12) 0.046(6) Uani 1 1 d . U . . .
C44 C 0.842(2) 0.9599(15) -0.0460(13) 0.049(7) Uani 1 1 d . . . . .
H44A H 0.8227 0.9758 -0.0912 0.073 Uiso 1 1 calc GR . . . .
H44B H 0.7832 0.9359 -0.0313 0.073 Uiso 1 1 calc GR . . . .
H44C H 0.8834 0.9266 -0.0508 0.073 Uiso 1 1 calc GR . . . .
C6 C 0.6374(19) 1.0748(14) -0.0498(12) 0.038(6) Uani 1 1 d . . . . .
H6 H 0.6367 1.1107 -0.0792 0.046 Uiso 1 1 calc R . . . .
C46 C 0.6644(18) 0.5387(14) 0.5444(14) 0.039(6) Uani 1 1 d . . . . .
H46A H 0.7175 0.5691 0.5286 0.059 Uiso 1 1 calc GR . . . .
H46B H 0.6919 0.5155 0.5827 0.059 Uiso 1 1 calc GR . . . .
H46C H 0.6231 0.5679 0.5609 0.059 Uiso 1 1 calc GR . . . .
C40 C 0.7882(14) 0.4622(10) 0.4163(11) 0.019(4) Uani 1 1 d . U . . .
C47 C 0.6094(14) 0.2255(11) 0.2305(11) 0.023(5) Uani 1 1 d . . . . .
C23 C 0.4827(17) 0.4070(12) 0.1959(12) 0.028(5) Uani 1 1 d . . . . .
H23A H 0.4841 0.3576 0.1784 0.034 Uiso 1 1 calc R . . . .
H23B H 0.4883 0.4359 0.1575 0.034 Uiso 1 1 calc R . . . .
C33 C 0.6348(14) 0.2324(11) 0.4435(10) 0.020(4) Uani 1 1 d . U . . .
H33A H 0.6507 0.2157 0.3987 0.024 Uiso 1 1 calc R . . . .
H33B H 0.6316 0.1933 0.4722 0.024 Uiso 1 1 calc R . . . .
C20 C 1.1845(17) 1.2117(11) 0.1483(12) 0.026(5) Uani 1 1 d . . . . .
C36 C 0.8406(15) 0.4300(13) 0.5280(11) 0.027(5) Uani 1 1 d . . . . .
H36 H 0.8399 0.3961 0.5596 0.033 Uiso 1 1 calc R . . . .
C14 C 1.0870(19) 1.1024(11) 0.2721(12) 0.035(6) Uani 1 1 d . . . . .
H14A H 1.1385 1.1218 0.3151 0.041 Uiso 1 1 calc R . . . .
H14B H 1.0942 1.0550 0.2531 0.041 Uiso 1 1 calc R . . . .
C8 C 0.5783(19) 0.9559(13) -0.0326(15) 0.044(7) Uani 1 1 d . . . . .
H8 H 0.5375 0.9094 -0.0497 0.053 Uiso 1 1 calc R . . . .
C2 C 1.0089(16) 1.3155(12) 0.0877(12) 0.028(5) Uani 1 1 d . . . . .
H2A H 1.0052 1.3342 0.1357 0.034 Uiso 1 1 calc R . . . .
H2B H 1.0079 1.3543 0.0588 0.034 Uiso 1 1 calc R . . . .
N3 N 0.554(2) 0.4421(13) 0.4408(14) 0.055(6) Uani 1 1 d . U . . .
C53 C 1.2065(17) 0.8770(13) 0.6091(13) 0.039(6) Uiso 1 1 d . . . . .
C3 C 0.8403(15) 1.2761(11) 0.0490(11) 0.024(5) Uani 1 1 d . U . . .
H3A H 0.8441 1.3179 0.0237 0.028 Uiso 1 1 calc R . . . .
H3B H 0.8255 1.2896 0.0951 0.028 Uiso 1 1 calc R . . . .
C9 C 0.635(2) 0.9714(14) 0.0354(13) 0.040(6) Uani 1 1 d . . . . .
H9 H 0.6331 0.9350 0.0642 0.047 Uiso 1 1 calc R . . . .
C28 C 0.1372(18) 0.3085(11) 0.3507(12) 0.030(5) Uani 1 1 d . . . . .
H28 H 0.0824 0.2976 0.3717 0.036 Uiso 1 1 calc R . . . .
C45 C 0.609(2) 0.4871(16) 0.4892(17) 0.052(7) Uani 1 1 d . U . . .
C38 C 0.9095(18) 0.5486(12) 0.5034(12) 0.034(6) Uani 1 1 d . . . . .
H38 H 0.9537 0.5943 0.5174 0.041 Uiso 1 1 calc R . . . .
C7 C 0.5817(18) 1.0087(13) -0.0755(14) 0.038(6) Uani 1 1 d . U . . .
H7 H 0.5450 0.9981 -0.1225 0.045 Uiso 1 1 calc R . . . .
C43 C 0.894(2) 1.0201(14) 0.0051(14) 0.039(6) Uani 1 1 d . U . . .
C1 C 1.1000(17) 1.2905(12) 0.0893(12) 0.028(5) Uani 1 1 d . U . . .
H1A H 1.1021 1.2698 0.0416 0.034 Uiso 1 1 calc R . . . .
H1B H 1.1578 1.3310 0.1069 0.034 Uiso 1 1 calc R . . . .
C48 C 0.635(2) 0.1728(12) 0.1847(14) 0.044(7) Uani 1 1 d . . . . .
H48A H 0.5874 0.1611 0.1398 0.065 Uiso 1 1 calc GR . . . .
H48B H 0.6346 0.1296 0.2065 0.065 Uiso 1 1 calc GR . . . .
H48C H 0.7002 0.1920 0.1768 0.065 Uiso 1 1 calc GR . . . .
C42 C 0.8651(18) 1.3324(13) 0.3166(14) 0.041(6) Uani 1 1 d . U . . .
H42A H 0.8723 1.3784 0.2993 0.062 Uiso 1 1 calc GR . . . .
H42B H 0.9127 1.3376 0.3608 0.062 Uiso 1 1 calc GR . . . .
H42C H 0.7989 1.3168 0.3245 0.062 Uiso 1 1 calc GR . . . .
C54 C 1.188(2) 0.9303(15) 0.5656(15) 0.051(7) Uiso 1 1 d . . . . .
H54A H 1.1865 0.9122 0.5168 0.077 Uiso 1 1 calc GR . . . .
H54B H 1.2404 0.9741 0.5815 0.077 Uiso 1 1 calc GR . . . .
H54C H 1.1254 0.9408 0.5690 0.077 Uiso 1 1 calc GR . . . .
C49 C 0.615(2) 0.3537(16) 0.0616(16) 0.055(7) Uiso 1 1 d . . . . .
N5 N 0.626(2) 0.3061(14) 0.0891(15) 0.066(7) Uiso 1 1 d . . . . .
C50 C 0.583(3) 0.4097(18) 0.0255(19) 0.072(10) Uiso 1 1 d . . . . .
H50A H 0.6149 0.4160 -0.0142 0.108 Uiso 1 1 calc GR . . . .
H50B H 0.6017 0.4547 0.0582 0.108 Uiso 1 1 calc GR . . . .
H50C H 0.5123 0.3959 0.0085 0.108 Uiso 1 1 calc GR . . . .
C51 C 0.875(3) 0.463(2) 0.122(2) 0.074(10) Uiso 1 1 d . . . . .
N6 N 0.842(3) 0.4361(19) 0.166(2) 0.101(11) Uiso 1 1 d . . . . .
C52 C 0.936(2) 0.4904(17) 0.0776(17) 0.065(9) Uiso 1 1 d . . . . .
H52A H 0.9092 0.4645 0.0298 0.098 Uiso 1 1 calc GR . . . .
H52B H 1.0014 0.4842 0.0945 0.098 Uiso 1 1 calc GR . . . .
H52C H 0.9382 0.5413 0.0775 0.098 Uiso 1 1 calc GR . . . .


_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 I7 3.0956(16) . ?
Bi1 I5 3.0641(17) . ?
Bi1 I2 3.0230(16) . ?
Bi1 I1 3.0468(16) . ?
Bi1 I6 3.0972(17) . ?
Bi1 I3 3.0756(17) . ?
Bi4 I16 3.1042(16) . ?
Bi4 I15 3.0525(16) . ?
Bi4 I12 3.0734(16) . ?
Bi4 I9 3.0523(16) . ?
Bi4 I11 3.0775(17) . ?
Bi4 I14 3.0877(17) . ?
Bi6 I16 3.0620(17) . ?
Bi6 I15 3.3521(16) . ?
Bi6 I2 3.4126(17) 1_655 ?
Bi6 I3 3.1062(17) 1_655 ?
Bi6 I20 2.8824(16) . ?
Bi6 I17 2.8262(18) . ?
Bi3 I7 3.0860(16) . ?
Bi3 I12 3.3801(17) . ?
Bi3 I5 3.3790(16) . ?
Bi3 I11 3.1291(17) . ?
Bi3 I13 2.8741(16) . ?
Bi3 I8 2.8186(18) . ?
Bi5 I15 3.4003(16) . ?
Bi5 I1 3.0808(17) 1_655 ?
Bi5 I14 3.1178(17) . ?
Bi5 I18 2.8344(16) . ?
Bi5 I19 2.8708(17) . ?
Bi2 I12 3.3897(16) . ?
Bi2 I5 3.3906(16) . ?
Bi2 I9 3.1319(16) . ?
Bi2 I6 3.0854(17) . ?
Bi2 I4 2.8581(16) . ?
Bi2 I10 2.8257(17) . ?
I2 Bi6 3.4126(17) 1_455 ?
I1 Bi5 3.0807(17) 1_455 ?
I3 Bi6 3.1064(17) 1_455 ?
Na1 O1 2.592(17) . ?
Na1 O2 2.596(16) . ?
Na1 O4 2.780(18) . ?
Na1 O6 2.645(17) . ?
Na1 O3 2.794(18) . ?
Na1 O5 2.606(16) . ?
Na1 N1 2.43(2) . ?
Na1 N2 2.38(2) . ?
Na2 O7 2.740(17) . ?
Na2 O9 2.594(17) . ?
Na2 O11 2.622(16) . ?
Na2 O8 2.638(17) . ?
Na2 O10 2.625(17) . ?
Na2 O12 2.700(18) . ?
Na2 N4 2.437(19) . ?
Na2 N3 2.37(3) . ?
O1 C20 1.39(3) . ?
O1 C1 1.45(3) . ?
O7 C21 1.47(3) . ?
O7 C40 1.39(2) . ?
O2 C2 1.43(3) . ?
O2 C3 1.39(2) . ?
O4 C10 1.35(3) . ?
O4 C11 1.41(3) . ?
O9 C25 1.37(3) . ?
O9 C24 1.43(3) . ?
O6 C15 1.35(3) . ?
O6 C14 1.42(2) . ?
O3 C5 1.37(2) . ?
O3 C4 1.41(3) . ?
O11 C32 1.42(2) . ?
O11 C33 1.40(2) . ?
O8 C22 1.39(3) . ?
O8 C23 1.41(3) . ?
O10 C30 1.36(2) . ?
O10 C31 1.42(2) . ?
O12 C34 1.43(2) . ?
O12 C35 1.39(3) . ?
O5 C13 1.41(3) . ?
O5 C12 1.43(2) . ?
N4 C47 1.12(3) . ?
C30 C25 1.40(3) . ?
C30 C29 1.38(3) . ?
C25 C26 1.38(3) . ?
N1 C41 1.13(3) . ?
C19 C18 1.35(3) . ?
C19 C20 1.36(3) . ?
C34 C33 1.48(3) . ?
C5 C10 1.44(3) . ?
C5 C6 1.36(3) . ?
C21 C22 1.44(3) . ?
C32 C31 1.50(3) . ?
C39 C40 1.37(3) . ?
C39 C38 1.39(3) . ?
C35 C40 1.39(3) . ?
C35 C36 1.34(3) . ?
C10 C9 1.40(3) . ?
C13 C14 1.49(3) . ?
C27 C26 1.42(3) . ?
C27 C28 1.38(3) . ?
C24 C23 1.49(3) . ?
C37 C36 1.41(3) . ?
C37 C38 1.35(3) . ?
N7 C53 1.13(3) . ?
C17 C18 1.37(3) . ?
C17 C16 1.40(3) . ?
C29 C28 1.36(3) . ?
C15 C16 1.39(3) . ?
C15 C20 1.41(3) . ?
C11 C12 1.49(3) . ?
C41 C42 1.45(3) . ?
C4 C3 1.52(3) . ?
N2 C43 1.15(3) . ?
C44 C43 1.42(4) . ?
C6 C7 1.34(3) . ?
C46 C45 1.38(4) . ?
C47 C48 1.44(3) . ?
C8 C9 1.39(4) . ?
C8 C7 1.39(3) . ?
C2 C1 1.49(3) . ?
N3 C45 1.24(4) . ?
C53 C54 1.44(3) . ?
C49 N5 1.14(4) . ?
C49 C50 1.46(4) . ?
C51 N6 1.17(5) . ?
C51 C52 1.42(5) . ?

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
I7 Bi1 I6 90.65(4) . . ?
I5 Bi1 I7 90.90(4) . . ?
I5 Bi1 I6 91.22(4) . . ?
I5 Bi1 I3 176.78(5) . . ?
I2 Bi1 I7 88.76(4) . . ?
I2 Bi1 I5 89.71(4) . . ?
I2 Bi1 I1 91.85(4) . . ?
I2 Bi1 I6 178.91(5) . . ?
I2 Bi1 I3 93.38(5) . . ?
I1 Bi1 I7 178.47(5) . . ?
I1 Bi1 I5 87.71(4) . . ?
I1 Bi1 I6 88.76(5) . . ?
I1 Bi1 I3 93.11(5) . . ?
I3 Bi1 I7 88.25(4) . . ?
I3 Bi1 I6 85.69(4) . . ?
I15 Bi4 I16 90.15(4) . . ?
I15 Bi4 I12 90.45(4) . . ?
I15 Bi4 I11 175.62(5) . . ?
I15 Bi4 I14 90.15(4) . . ?
I12 Bi4 I16 87.43(4) . . ?
I12 Bi4 I11 92.15(4) . . ?
I12 Bi4 I14 178.48(5) . . ?
I9 Bi4 I16 178.95(5) . . ?
I9 Bi4 I15 88.99(4) . . ?
I9 Bi4 I12 91.96(4) . . ?
I9 Bi4 I11 94.44(5) . . ?
I9 Bi4 I14 89.44(4) . . ?
I11 Bi4 I16 86.45(4) . . ?
I11 Bi4 I14 87.16(4) . . ?
I14 Bi4 I16 91.17(4) . . ?
I16 Bi6 I15 85.51(4) . . ?
I16 Bi6 I2 85.95(4) . 1_655 ?
I16 Bi6 I3 168.36(5) . 1_655 ?
I15 Bi6 I2 82.06(4) . 1_655 ?
I3 Bi6 I15 85.35(4) 1_655 . ?
I3 Bi6 I2 85.67(4) 1_655 1_655 ?
I20 Bi6 I16 93.21(5) . . ?
I20 Bi6 I15 176.63(5) . . ?
I20 Bi6 I2 94.75(5) . 1_655 ?
I20 Bi6 I3 95.52(5) . 1_655 ?
I17 Bi6 I16 94.31(5) . . ?
I17 Bi6 I15 88.43(5) . . ?
I17 Bi6 I2 170.44(5) . 1_655 ?
I17 Bi6 I3 92.62(5) . 1_655 ?
I17 Bi6 I20 94.78(6) . . ?
I7 Bi3 I12 86.39(4) . . ?
I7 Bi3 I5 85.40(4) . . ?
I7 Bi3 I11 169.16(5) . . ?
I5 Bi3 I12 82.64(4) . . ?
I11 Bi3 I12 85.69(4) . . ?
I11 Bi3 I5 86.25(4) . . ?
I13 Bi3 I7 91.22(5) . . ?
I13 Bi3 I12 94.03(5) . . ?
I13 Bi3 I5 175.39(5) . . ?
I13 Bi3 I11 96.71(5) . . ?
I8 Bi3 I7 94.06(5) . . ?
I8 Bi3 I12 171.24(5) . . ?
I8 Bi3 I5 88.67(5) . . ?
I8 Bi3 I11 92.65(5) . . ?
I8 Bi3 I13 94.71(6) . . ?
I1 Bi5 I15 85.18(4) 1_655 . ?
I1 Bi5 I14 164.91(5) 1_655 . ?
I14 Bi5 I15 83.55(4) . . ?
I18 Bi5 I15 89.00(5) . . ?
I18 Bi5 I1 94.03(5) . 1_655 ?
I18 Bi5 I14 95.79(5) . . ?
I18 Bi5 I19 94.88(5) . . ?
I19 Bi5 I15 176.02(5) . . ?
I19 Bi5 I1 93.66(5) . 1_655 ?
I19 Bi5 I14 96.90(5) . . ?
I12 Bi2 I5 82.33(4) . . ?
I9 Bi2 I12 84.89(4) . . ?
I9 Bi2 I5 83.65(4) . . ?
I6 Bi2 I12 86.75(4) . . ?
I6 Bi2 I5 85.53(4) . . ?
I6 Bi2 I9 167.11(5) . . ?
I4 Bi2 I12 177.26(5) . . ?
I4 Bi2 I5 95.58(5) . . ?
I4 Bi2 I9 93.14(5) . . ?
I4 Bi2 I6 94.86(5) . . ?
I10 Bi2 I12 86.59(5) . . ?
I10 Bi2 I5 168.88(5) . . ?
I10 Bi2 I9 94.39(5) . . ?
I10 Bi2 I6 94.88(5) . . ?
I10 Bi2 I4 95.46(5) . . ?
Bi6 I16 Bi4 94.34(4) . . ?
Bi4 I15 Bi6 89.71(4) . . ?
Bi4 I15 Bi5 90.53(4) . . ?
Bi6 I15 Bi5 99.47(4) . . ?
Bi3 I7 Bi1 94.26(4) . . ?
Bi4 I12 Bi3 88.73(4) . . ?
Bi4 I12 Bi2 88.85(4) . . ?
Bi3 I12 Bi2 97.49(4) . . ?
Bi1 I5 Bi3 89.22(4) . . ?
Bi1 I5 Bi2 88.91(4) . . ?
Bi3 I5 Bi2 97.49(4) . . ?
Bi1 I2 Bi6 87.98(4) . 1_455 ?
Bi1 I1 Bi5 95.48(5) . 1_455 ?
Bi4 I9 Bi2 94.17(4) . . ?
Bi4 I11 Bi3 93.42(4) . . ?
Bi2 I6 Bi1 94.13(4) . . ?
Bi1 I3 Bi6 92.84(4) . 1_455 ?
Bi4 I14 Bi5 95.42(4) . . ?
O1 Na1 O2 64.5(5) . . ?
O1 Na1 O4 173.5(5) . . ?
O1 Na1 O6 57.7(5) . . ?
O1 Na1 O3 124.8(5) . . ?
O1 Na1 O5 119.9(6) . . ?
O2 Na1 O4 115.2(6) . . ?
O2 Na1 O6 121.7(6) . . ?
O2 Na1 O3 61.0(5) . . ?
O2 Na1 O5 171.7(6) . . ?
O4 Na1 O3 54.2(4) . . ?
O6 Na1 O4 123.1(5) . . ?
O6 Na1 O3 177.0(5) . . ?
O5 Na1 O4 61.3(5) . . ?
O5 Na1 O6 62.3(5) . . ?
O5 Na1 O3 115.2(5) . . ?
N1 Na1 O1 95.8(6) . . ?
N1 Na1 O2 85.7(6) . . ?
N1 Na1 O4 90.6(6) . . ?
N1 Na1 O6 93.4(6) . . ?
N1 Na1 O3 88.0(6) . . ?
N1 Na1 O5 86.8(6) . . ?
N2 Na1 O1 93.7(7) . . ?
N2 Na1 O2 95.1(7) . . ?
N2 Na1 O4 79.8(7) . . ?
N2 Na1 O6 94.9(7) . . ?
N2 Na1 O3 83.5(7) . . ?
N2 Na1 O5 91.7(7) . . ?
N2 Na1 N1 169.8(8) . . ?
O9 Na2 O7 123.0(5) . . ?
O9 Na2 O11 120.1(6) . . ?
O9 Na2 O8 62.8(5) . . ?
O9 Na2 O10 57.7(5) . . ?
O9 Na2 O12 175.8(6) . . ?
O11 Na2 O7 117.0(5) . . ?
O11 Na2 O8 170.7(6) . . ?
O11 Na2 O10 62.5(5) . . ?
O11 Na2 O12 62.1(5) . . ?
O8 Na2 O7 60.9(5) . . ?
O8 Na2 O12 115.7(6) . . ?
O10 Na2 O7 176.3(6) . . ?
O10 Na2 O8 120.2(6) . . ?
O10 Na2 O12 124.1(5) . . ?
O12 Na2 O7 55.0(5) . . ?
N4 Na2 O7 87.1(6) . . ?
N4 Na2 O9 97.1(6) . . ?
N4 Na2 O11 85.3(6) . . ?
N4 Na2 O8 85.6(6) . . ?
N4 Na2 O10 96.4(6) . . ?
N4 Na2 O12 86.6(6) . . ?
N3 Na2 O7 79.8(7) . . ?
N3 Na2 O9 96.2(8) . . ?
N3 Na2 O11 94.0(7) . . ?
N3 Na2 O8 94.4(8) . . ?
N3 Na2 O10 96.6(8) . . ?
N3 Na2 O12 79.9(7) . . ?
N3 Na2 N4 164.9(9) . . ?
C20 O1 Na1 121.2(12) . . ?
C20 O1 C1 116.2(16) . . ?
C1 O1 Na1 116.2(13) . . ?
C21 O7 Na2 116.3(11) . . ?
C40 O7 Na2 117.0(11) . . ?
C40 O7 C21 118.2(15) . . ?
C2 O2 Na1 109.0(12) . . ?
C3 O2 Na1 112.0(12) . . ?
C3 O2 C2 111.4(16) . . ?
C10 O4 Na1 117.4(12) . . ?
C10 O4 C11 114.4(17) . . ?
C11 O4 Na1 116.2(13) . . ?
C25 O9 Na2 119.6(12) . . ?
C25 O9 C24 116.6(16) . . ?
C24 O9 Na2 119.3(12) . . ?
C15 O6 Na1 117.3(13) . . ?
C15 O6 C14 118.8(18) . . ?
C14 O6 Na1 117.9(14) . . ?
C5 O3 Na1 118.1(12) . . ?
C5 O3 C4 115.7(17) . . ?
C4 O3 Na1 114.9(13) . . ?
C32 O11 Na2 107.4(11) . . ?
C33 O11 Na2 111.3(11) . . ?
C33 O11 C32 112.4(15) . . ?
C22 O8 Na2 110.2(12) . . ?
C22 O8 C23 114.7(16) . . ?
C23 O8 Na2 107.6(13) . . ?
C30 O10 Na2 120.7(12) . . ?
C30 O10 C31 115.5(16) . . ?
C31 O10 Na2 119.0(12) . . ?
C34 O12 Na2 115.3(12) . . ?
C35 O12 Na2 118.7(14) . . ?
C35 O12 C34 114.9(17) . . ?
C13 O5 Na1 108.0(11) . . ?
C13 O5 C12 113.7(15) . . ?
C12 O5 Na1 114.1(12) . . ?
C47 N4 Na2 175.9(19) . . ?
O10 C30 C25 112.4(19) . . ?
O10 C30 C29 127(2) . . ?
C29 C30 C25 121(2) . . ?
O9 C25 C30 116.0(19) . . ?
O9 C25 C26 124.2(19) . . ?
C26 C25 C30 120(2) . . ?
C41 N1 Na1 175.3(19) . . ?
C18 C19 C20 120(2) . . ?
O12 C34 C33 107.6(17) . . ?
O3 C5 C10 111.7(19) . . ?
C6 C5 O3 129(2) . . ?
C6 C5 C10 119(2) . . ?
C22 C21 O7 104.1(18) . . ?
O11 C32 C31 108.4(16) . . ?
O10 C31 C32 105.4(16) . . ?
C40 C39 C38 121(2) . . ?
O12 C35 C40 113(2) . . ?
C36 C35 O12 126(2) . . ?
C36 C35 C40 121(2) . . ?
O4 C10 C5 116.0(19) . . ?
O4 C10 C9 127(2) . . ?
C9 C10 C5 117(2) . . ?
O5 C13 C14 107.9(17) . . ?
C28 C27 C26 120(2) . . ?
O8 C22 C21 110.7(19) . . ?
O9 C24 C23 105.6(18) . . ?
C38 C37 C36 124(2) . . ?
C18 C17 C16 117(2) . . ?
C28 C29 C30 119(2) . . ?
O6 C15 C16 126(2) . . ?
O6 C15 C20 118(2) . . ?
C16 C15 C20 116(2) . . ?
C25 C26 C27 119(2) . . ?
O4 C11 C12 106.0(17) . . ?
N1 C41 C42 178(3) . . ?
O5 C12 C11 110.2(18) . . ?
C19 C18 C17 122(2) . . ?
O3 C4 C3 106.8(18) . . ?
C15 C16 C17 122(2) . . ?
C43 N2 Na1 145(2) . . ?
C7 C6 C5 124(2) . . ?
O7 C40 C35 115.1(18) . . ?
C39 C40 O7 125(2) . . ?
C39 C40 C35 120(2) . . ?
N4 C47 C48 178(2) . . ?
O8 C23 C24 108.3(17) . . ?
O11 C33 C34 107.4(16) . . ?
O1 C20 C15 109.9(19) . . ?
C19 C20 O1 128.5(19) . . ?
C19 C20 C15 122(2) . . ?
C35 C36 C37 117(2) . . ?
O6 C14 C13 106.6(19) . . ?
C9 C8 C7 120(2) . . ?
O2 C2 C1 107.7(18) . . ?
C45 N3 Na2 144(2) . . ?
N7 C53 C54 175(3) . . ?
O2 C3 C4 107.9(17) . . ?
C8 C9 C10 121(2) . . ?
C29 C28 C27 121(2) . . ?
N3 C45 C46 176(3) . . ?
C37 C38 C39 117(2) . . ?
C6 C7 C8 119(3) . . ?
N2 C43 C44 178(3) . . ?
O1 C1 C2 107.9(18) . . ?
N5 C49 C50 170(4) . . ?
N6 C51 C52 165(4) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.6323(9)
2 0.3677(9)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound4
_database_code_depnum_ccdc_archive 'CCDC 1050432'
_audit_update_record             
;
2015-04-02 deposited with the CCDC.
2015-04-29 downloaded from the CCDC.
;
_audit_creation_date             2015-03-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Bi3 I11, C44 H54 K2 N2 O12, C2 H3 N'
_chemical_formula_sum            'C46 H57 Bi3 I11 K2 N3 O12'
_chemical_formula_weight         2944.98
_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 0.0033 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'
I I -0.4742 1.8119 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_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                   19.4954(11)
_cell_length_b                   16.2145(6)
_cell_length_c                   23.3300(13)
_cell_angle_alpha                90
_cell_angle_beta                 92.905(5)
_cell_angle_gamma                90
_cell_volume                     7365.3(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4827
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.19
_cell_measurement_theta_min      1.69
_shelx_estimated_absorpt_T_max   0.199
_shelx_estimated_absorpt_T_min   0.099
_exptl_absorpt_coefficient_mu    11.923
_exptl_absorpt_correction_T_max  0.5364
_exptl_absorpt_correction_T_min  0.0857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.656
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             5280
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2233
_diffrn_reflns_av_unetI/netI     0.1311
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            79147
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.853
_diffrn_reflns_theta_min         1.328
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Stoe IPDS-II'
_diffrn_measurement_method       'area detetor, ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9570
_reflns_number_total             15628
_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       ?
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_refine_diff_density_max         3.126
_refine_diff_density_min         -2.195
_refine_diff_density_rms         0.347
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.919
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         15628
_refine_ls_number_restraints     41
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0666
_refine_ls_restrained_S_all      0.928
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0637P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1515
_refine_ls_wR_factor_ref         0.1618
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 K2-C28 = K2-C29 = K2-C39 = K1-C10 = K1-C1 = K1-C11
 -3.65 with sigma of 0.02
 K1-C20 = K2-C38
 -3.65 with sigma of 0.02
 K2-C39
 -3.65 with sigma of 0.02
 K2-C28
 -3.65 with sigma of 0.02
 K2-C30
 -3.65 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C22 \\sim C21: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C20 \\sim C19: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C28 \\sim C27: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C9 \\sim C10: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C11 \\sim C12: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C38(H38A,H38B), C30(H30A,H30B), C29(H29A,H29B), C9(H9A,H9B),
 C40(H40A,H40B), C37(H37A,H37B), C27(H27A,H27B), C19(H19A,H19B), C39(H39A,H39B),
  C12(H12A,H12B), C20(H20A,H20B), C11(H11A,H11B), C1(H1A,H1B), C10(H10A,H10B),
 C28(H28A,H28B)
4.b Aromatic/amide H refined with riding coordinates:
 C36(H36), C16(H16), C18(H18), C33(H33), C17(H17), C15(H15), C34(H34), C5(H5),
 C26(H26), C25(H25), C35(H35), C23(H23), C6(H6), C24(H24), C7(H7), C8(H8)
4.c Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C42(H42A,H42B,H42C), C46(H46A,H46B,H46C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 0.97549(3) 0.42332(3) 0.16253(2) 0.03187(14) Uani 1 1 d . . . . .
Bi2 Bi 1.10569(3) 0.57072(3) 0.02483(2) 0.03171(14) Uani 1 1 d . . . . .
Bi3 Bi 1.18425(3) 0.55531(3) 0.21780(2) 0.03149(14) Uani 1 1 d . . . . .
I4 I 1.03887(5) 0.37902(5) 0.03653(4) 0.0335(2) Uani 1 1 d . . . . .
I2 I 0.84410(5) 0.49175(5) 0.08735(4) 0.0329(2) Uani 1 1 d . . . . .
I5 I 1.04144(5) 0.61057(5) 0.14145(4) 0.0319(2) Uani 1 1 d . . . . .
I7 I 1.16263(5) 0.73388(6) 0.01292(5) 0.0409(2) Uani 1 1 d . . . . .
I1 I 0.92034(5) 0.49881(6) 0.26369(4) 0.0382(2) Uani 1 1 d . . . . .
I3 I 0.91009(5) 0.26376(6) 0.17023(5) 0.0408(2) Uani 1 1 d . . . . .
I6 I 1.10754(5) 0.36693(5) 0.21901(5) 0.0377(2) Uani 1 1 d . . . . .
I8 I 1.23109(5) 0.50630(6) 0.08783(4) 0.0391(2) Uani 1 1 d . . . . .
I9 I 1.12821(5) 0.58777(6) 0.32862(4) 0.0393(2) Uani 1 1 d . . . . .
I11 I 1.30630(5) 0.46974(6) 0.26091(4) 0.0377(2) Uani 1 1 d . . . . .
I10 I 1.24837(5) 0.71476(6) 0.21286(5) 0.0452(3) Uani 1 1 d . . . . .
K2 K 0.88969(16) 0.89573(18) 0.17374(15) 0.0372(7) Uani 1 1 d D . . . .
K1 K 0.58608(17) 0.69489(19) 0.01903(14) 0.0396(8) Uani 1 1 d D . . . .
O6 O 0.7254(5) 0.7403(6) 0.0372(4) 0.036(2) Uani 1 1 d . . . . .
O4 O 0.4985(6) 0.7217(6) 0.1076(5) 0.045(3) Uani 1 1 d . . . . .
O7 O 0.9513(5) 0.9023(6) 0.0697(4) 0.041(2) Uani 1 1 d . . . . .
O12 O 1.0133(5) 0.8236(6) 0.1653(5) 0.041(3) Uani 1 1 d . . . . .
O11 O 0.9492(5) 0.8226(5) 0.2738(5) 0.039(2) Uani 1 1 d . . . . .
O10 O 0.8368(5) 0.9068(6) 0.2811(5) 0.041(3) Uani 1 1 d . . . . .
O2 O 0.5349(5) 0.6153(5) -0.0775(4) 0.036(2) Uani 1 1 d . . . . .
O5 O 0.6413(6) 0.7611(6) 0.1187(4) 0.042(3) Uani 1 1 d . . . . .
O3 O 0.4538(5) 0.6408(6) 0.0062(4) 0.041(2) Uani 1 1 d . . . . .
O1 O 0.6721(5) 0.6689(6) -0.0662(4) 0.040(2) Uani 1 1 d . . . . .
O9 O 0.7739(6) 0.9867(6) 0.1838(5) 0.047(3) Uani 1 1 d . . . . .
O8 O 0.8325(5) 0.9680(7) 0.0762(5) 0.049(3) Uani 1 1 d . . . . .
C36 C 0.9205(7) 0.7350(8) 0.3547(7) 0.035(3) Uani 1 1 d . . . . .
H36 H 0.9626 0.7055 0.3539 0.042 Uiso 1 1 calc R . . . .
C14 C 0.7534(8) 0.7342(8) 0.0924(7) 0.036(3) Uani 1 1 d . . . . .
C2 C 0.5808(8) 0.6012(8) -0.1222(7) 0.040(4) Uani 1 1 d . . . . .
H2A H 0.5547 0.6004 -0.1597 0.047 Uiso 1 1 calc R . . . .
H2B H 0.6032 0.5468 -0.1166 0.047 Uiso 1 1 calc R . . . .
C16 C 0.8008(9) 0.7168(9) 0.2057(8) 0.049(4) Uani 1 1 d . . . . .
H16 H 0.8161 0.7087 0.2446 0.058 Uiso 1 1 calc R . . . .
C4 C 0.4325(8) 0.5797(9) -0.0331(6) 0.036(3) Uani 1 1 d . . . . .
C38 C 1.0511(6) 0.8133(8) 0.2206(7) 0.041(4) Uani 1 1 d D . . . .
H38A H 1.0656 0.8678 0.2361 0.049 Uiso 1 1 calc R . . . .
H38B H 1.0927 0.7796 0.2158 0.049 Uiso 1 1 calc R . . . .
C30 C 0.7770(7) 0.9542(9) 0.2843(6) 0.039(4) Uani 1 1 d D . . . .
H30A H 0.7743 0.9762 0.3237 0.047 Uiso 1 1 calc R . . . .
H30B H 0.7364 0.9186 0.2763 0.047 Uiso 1 1 calc R . . . .
C18 C 0.8220(8) 0.7150(8) 0.1058(6) 0.037(3) Uani 1 1 d . . . . .
H18 H 0.8527 0.7064 0.0761 0.044 Uiso 1 1 calc R . . . .
C3 C 0.4773(7) 0.5650(8) -0.0760(7) 0.037(4) Uani 1 1 d . . . . .
C29 C 0.7753(8) 1.0250(9) 0.2422(7) 0.047(4) Uani 1 1 d D . . . .
H29A H 0.7340 1.0594 0.2467 0.056 Uiso 1 1 calc R . . . .
H29B H 0.8166 1.0601 0.2485 0.056 Uiso 1 1 calc R . . . .
C33 C 0.8016(8) 0.8243(9) 0.3614(7) 0.040(4) Uani 1 1 d . . . . .
H33 H 0.7598 0.8541 0.3633 0.048 Uiso 1 1 calc R . . . .
C13 C 0.7085(8) 0.7454(8) 0.1366(7) 0.036(3) Uani 1 1 d . . . . .
C17 C 0.8447(8) 0.7086(9) 0.1616(8) 0.047(4) Uani 1 1 d . . . . .
H17 H 0.8921 0.6982 0.1705 0.056 Uiso 1 1 calc R . . . .
N1 N 0.5448(8) 0.8490(9) -0.0230(7) 0.058(4) Uani 1 1 d . . . . .
C43 C 1.0075(9) 1.0749(10) 0.2362(8) 0.052(5) Uani 1 1 d . . . . .
C22 C 0.8458(8) 0.9393(9) 0.0240(8) 0.043(4) Uani 1 1 d . U . . .
C32 C 0.9069(8) 0.7975(8) 0.3150(7) 0.037(3) Uani 1 1 d . . . . .
C9 C 0.4072(8) 0.6582(10) 0.0513(7) 0.047(4) Uani 1 1 d . U . . .
H9A H 0.4076 0.6116 0.0787 0.056 Uiso 1 1 calc R . . . .
H9B H 0.3599 0.6644 0.0344 0.056 Uiso 1 1 calc R . . . .
C40 C 1.0181(8) 0.8607(11) 0.0680(7) 0.045(4) Uani 1 1 d . . . . .
H40A H 1.0454 0.8870 0.0384 0.054 Uiso 1 1 calc R . . . .
H40B H 1.0107 0.8023 0.0570 0.054 Uiso 1 1 calc R . . . .
C37 C 1.0046(8) 0.7711(8) 0.2616(7) 0.039(4) Uani 1 1 d . . . . .
H37A H 0.9869 0.7190 0.2443 0.046 Uiso 1 1 calc R . . . .
H37B H 1.0311 0.7573 0.2977 0.046 Uiso 1 1 calc R . . . .
N2 N 0.9720(8) 1.0262(8) 0.2171(7) 0.062(4) Uani 1 1 d . . . . .
C15 C 0.7338(9) 0.7374(8) 0.1909(7) 0.041(4) Uani 1 1 d . . . . .
H15 H 0.7036 0.7465 0.2209 0.050 Uiso 1 1 calc R . . . .
C34 C 0.8160(8) 0.7608(9) 0.3997(7) 0.039(4) Uani 1 1 d . . . . .
H34 H 0.7854 0.7491 0.4291 0.047 Uiso 1 1 calc R . . . .
C5 C 0.4612(7) 0.5053(9) -0.1194(7) 0.041(4) Uani 1 1 d . . . . .
H5 H 0.4911 0.4976 -0.1499 0.049 Uiso 1 1 calc R . . . .
C26 C 0.8002(9) 0.9427(10) -0.0253(7) 0.050(4) Uani 1 1 d . . . . .
H26 H 0.7555 0.9653 -0.0234 0.060 Uiso 1 1 calc R . . . .
C27 C 0.7673(9) 1.0099(10) 0.0831(7) 0.054(5) Uani 1 1 d . U . . .
H27A H 0.7295 0.9692 0.0806 0.064 Uiso 1 1 calc R . . . .
H27B H 0.7593 1.0504 0.0517 0.064 Uiso 1 1 calc R . . . .
C19 C 0.7688(8) 0.7185(10) -0.0094(7) 0.045(4) Uani 1 1 d . U . . .
H19A H 0.7844 0.6607 -0.0048 0.055 Uiso 1 1 calc R . . . .
H19B H 0.8099 0.7545 -0.0082 0.055 Uiso 1 1 calc R . . . .
C25 C 0.8240(8) 0.9109(10) -0.0781(7) 0.048(4) Uani 1 1 d . . . . .
H25 H 0.7945 0.9126 -0.1118 0.058 Uiso 1 1 calc R . . . .
C41 C 0.5192(10) 0.9025(9) -0.0455(7) 0.050(4) Uani 1 1 d . . . . .
C35 C 0.8742(8) 0.7148(10) 0.3951(8) 0.046(4) Uani 1 1 d . . . . .
H35 H 0.8827 0.6690 0.4199 0.055 Uiso 1 1 calc R . . . .
C44 C 1.0520(8) 1.1400(9) 0.2631(8) 0.051(5) Uani 1 1 d . . . . .
H44A H 1.0434 1.1925 0.2432 0.077 Uiso 1 1 calc GR . . . .
H44B H 1.1003 1.1245 0.2604 0.077 Uiso 1 1 calc GR . . . .
H44C H 1.0416 1.1460 0.3036 0.077 Uiso 1 1 calc GR . . . .
C39 C 1.0576(6) 0.8645(10) 0.1249(6) 0.045(4) Uani 1 1 d D . . . .
H39A H 1.1020 0.8353 0.1232 0.054 Uiso 1 1 calc R . . . .
H39B H 1.0665 0.9224 0.1365 0.054 Uiso 1 1 calc R . . . .
C12 C 0.5950(8) 0.7755(10) 0.1637(7) 0.048(4) Uani 1 1 d . U . . .
H12A H 0.6125 0.8216 0.1881 0.058 Uiso 1 1 calc R . . . .
H12B H 0.5929 0.7257 0.1881 0.058 Uiso 1 1 calc R . . . .
C42 C 0.4877(8) 0.9748(10) -0.0739(8) 0.053(5) Uani 1 1 d . . . . .
H42A H 0.4849 0.9661 -0.1155 0.079 Uiso 1 1 calc GR . . . .
H42B H 0.5157 1.0237 -0.0648 0.079 Uiso 1 1 calc GR . . . .
H42C H 0.4414 0.9829 -0.0604 0.079 Uiso 1 1 calc GR . . . .
C23 C 0.9314(8) 0.8753(11) -0.0332(6) 0.045(4) Uani 1 1 d . . . . .
H23 H 0.9762 0.8536 -0.0369 0.054 Uiso 1 1 calc R . . . .
C21 C 0.9118(9) 0.9027(10) 0.0191(7) 0.045(4) Uani 1 1 d . U . . .
C20 C 0.7292(7) 0.7285(9) -0.0662(7) 0.051(4) Uani 1 1 d D U . . .
H20A H 0.7113 0.7855 -0.0703 0.061 Uiso 1 1 calc R . . . .
H20B H 0.7591 0.7171 -0.0983 0.061 Uiso 1 1 calc R . . . .
N3 N 0.6379(7) 1.0749(8) -0.0200(6) 0.049(3) Uani 1 1 d . . . . .
C45 C 0.6719(8) 1.0917(8) -0.0567(7) 0.039(4) Uani 1 1 d . . . . .
C11 C 0.5242(8) 0.7960(10) 0.1393(7) 0.050(4) Uani 1 1 d D U . . .
H11A H 0.4936 0.8097 0.1705 0.060 Uiso 1 1 calc R . . . .
H11B H 0.5259 0.8438 0.1131 0.060 Uiso 1 1 calc R . . . .
C1 C 0.6355(8) 0.6686(9) -0.1224(5) 0.039(4) Uani 1 1 d D . . . .
H1A H 0.6679 0.6576 -0.1528 0.047 Uiso 1 1 calc R . . . .
H1B H 0.6136 0.7229 -0.1299 0.047 Uiso 1 1 calc R . . . .
C31 C 0.8485(8) 0.8457(9) 0.3191(7) 0.045(4) Uani 1 1 d . . . . .
C6 C 0.3745(8) 0.5322(10) -0.0292(8) 0.046(4) Uani 1 1 d . . . . .
H6 H 0.3453 0.5393 0.0018 0.055 Uiso 1 1 calc R . . . .
C10 C 0.4282(8) 0.7354(10) 0.0823(9) 0.066(5) Uani 1 1 d D U . . .
H10A H 0.4277 0.7826 0.0554 0.079 Uiso 1 1 calc R . . . .
H10B H 0.3961 0.7475 0.1128 0.079 Uiso 1 1 calc R . . . .
C24 C 0.8860(10) 0.8793(10) -0.0807(7) 0.054(5) Uani 1 1 d . . . . .
H24 H 0.9000 0.8586 -0.1164 0.065 Uiso 1 1 calc R . . . .
C28 C 0.7674(9) 1.0534(10) 0.1395(7) 0.063(5) Uani 1 1 d D U . . .
H28A H 0.7242 1.0846 0.1430 0.075 Uiso 1 1 calc R . . . .
H28B H 0.8065 1.0922 0.1436 0.075 Uiso 1 1 calc R . . . .
C46 C 0.7121(9) 1.1136(10) -0.1072(7) 0.051(4) Uani 1 1 d . . . . .
H46A H 0.6823 1.1102 -0.1423 0.076 Uiso 1 1 calc GR . . . .
H46B H 0.7505 1.0751 -0.1099 0.076 Uiso 1 1 calc GR . . . .
H46C H 0.7299 1.1699 -0.1027 0.076 Uiso 1 1 calc GR . . . .
C7 C 0.4027(8) 0.4590(10) -0.1174(7) 0.046(4) Uani 1 1 d . . . . .
H7 H 0.3917 0.4187 -0.1460 0.056 Uiso 1 1 calc R . . . .
C8 C 0.3592(9) 0.4726(9) -0.0719(7) 0.047(4) Uani 1 1 d . . . . .
H8 H 0.3185 0.4408 -0.0699 0.056 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
Bi1 I4 3.3247(11) . ?
Bi1 I2 3.2269(11) . ?
Bi1 I5 3.3434(10) . ?
Bi1 I1 2.9122(11) . ?
Bi1 I3 2.8939(10) . ?
Bi1 I6 2.9757(11) . ?
Bi2 I4 3.2011(11) 3_765 ?
Bi2 I4 3.3866(10) . ?
Bi2 I2 3.0155(11) 3_765 ?
Bi2 I5 3.1199(11) . ?
Bi2 I7 2.8879(11) . ?
Bi2 I8 2.9772(11) . ?
Bi3 I5 3.3503(11) . ?
Bi3 I6 3.4016(10) . ?
Bi3 I8 3.3077(11) . ?
Bi3 I9 2.9053(11) . ?
Bi3 I11 2.8907(11) . ?
Bi3 I10 2.8767(10) . ?
I4 Bi2 3.2010(11) 3_765 ?
I2 Bi2 3.0154(11) 3_765 ?
K2 O7 2.765(11) . ?
K2 O12 2.695(10) . ?
K2 O11 2.816(11) . ?
K2 O10 2.763(11) . ?
K2 O9 2.718(10) . ?
K2 O8 2.745(11) . ?
K2 C16 3.479(15) . ?
K2 C29 3.504(12) . ?
K2 C17 3.167(14) . ?
K2 N2 2.811(15) . ?
K1 O6 2.826(11) . ?
K1 O4 2.781(12) . ?
K1 O2 2.740(10) . ?
K1 O5 2.732(11) . ?
K1 O3 2.727(11) . ?
K1 O1 2.699(11) . ?
K1 N1 2.788(15) . ?
K1 C11 3.516(13) . ?
K1 C1 3.509(12) . ?
K1 C7 3.390(16) 3_665 ?
K1 C8 3.146(15) 3_665 ?
O6 C14 1.378(17) . ?
O6 C19 1.453(17) . ?
O4 C11 1.487(17) . ?
O4 C10 1.48(2) . ?
O7 C40 1.469(17) . ?
O7 C21 1.376(18) . ?
O12 C38 1.464(17) . ?
O12 C39 1.467(16) . ?
O11 C32 1.360(18) . ?
O11 C37 1.406(16) . ?
O10 C30 1.401(15) . ?
O10 C31 1.342(19) . ?
O2 C2 1.426(16) . ?
O2 C3 1.389(16) . ?
O5 C13 1.379(18) . ?
O5 C12 1.438(18) . ?
O3 C4 1.398(17) . ?
O3 C9 1.453(18) . ?
O1 C20 1.474(16) . ?
O1 C1 1.460(16) . ?
O9 C29 1.496(18) . ?
O9 C28 1.497(18) . ?
O8 C22 1.342(19) . ?
O8 C27 1.457(18) . ?
C36 C32 1.39(2) . ?
C36 C35 1.38(2) . ?
C14 C18 1.39(2) . ?
C14 C13 1.40(2) . ?
C2 C1 1.53(2) . ?
C16 C17 1.38(2) . ?
C16 C15 1.38(2) . ?
C4 C3 1.38(2) . ?
C4 C6 1.37(2) . ?
C38 C37 1.52(2) . ?
C30 C29 1.51(2) . ?
C18 C17 1.36(2) . ?
C3 C5 1.43(2) . ?
C33 C34 1.38(2) . ?
C33 C31 1.42(2) . ?
C13 C15 1.34(2) . ?
N1 C41 1.12(2) . ?
C43 N2 1.13(2) . ?
C43 C44 1.49(2) . ?
C22 C26 1.42(2) . ?
C22 C21 1.43(2) . ?
C32 C31 1.39(2) . ?
C9 C10 1.49(2) . ?
C40 C39 1.50(2) . ?
C34 C35 1.37(2) . ?
C5 C7 1.37(2) . ?
C26 C25 1.43(2) . ?
C27 C28 1.49(2) . ?
C19 C20 1.51(2) . ?
C25 C24 1.32(2) . ?
C41 C42 1.47(2) . ?
C12 C11 1.50(2) . ?
C23 C21 1.37(2) . ?
C23 C24 1.39(2) . ?
N3 C45 1.140(19) . ?
C45 C46 1.49(2) . ?
C6 C8 1.41(2) . ?
C7 K1 3.390(16) 3_665 ?
C7 C8 1.41(2) . ?
C8 K1 3.146(15) 3_665 ?

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
I4 Bi1 I5 84.44(2) . . ?
I2 Bi1 I4 85.07(3) . . ?
I2 Bi1 I5 84.74(3) . . ?
I1 Bi1 I4 167.53(3) . . ?
I1 Bi1 I2 88.88(3) . . ?
I1 Bi1 I5 84.15(3) . . ?
I1 Bi1 I6 96.72(3) . . ?
I3 Bi1 I4 92.66(3) . . ?
I3 Bi1 I2 90.06(3) . . ?
I3 Bi1 I5 174.24(3) . . ?
I3 Bi1 I1 98.26(3) . . ?
I3 Bi1 I6 94.12(3) . . ?
I6 Bi1 I4 88.46(3) . . ?
I6 Bi1 I2 172.46(3) . . ?
I6 Bi1 I5 90.78(3) . . ?
I4 Bi2 I4 86.34(3) 3_765 . ?
I2 Bi2 I4 84.53(3) 3_765 . ?
I2 Bi2 I4 90.84(3) 3_765 3_765 ?
I2 Bi2 I5 171.39(3) 3_765 . ?
I5 Bi2 I4 86.95(3) . . ?
I5 Bi2 I4 87.36(3) . 3_765 ?
I7 Bi2 I4 93.31(3) . 3_765 ?
I7 Bi2 I4 179.10(3) . . ?
I7 Bi2 I2 94.64(3) . 3_765 ?
I7 Bi2 I5 93.87(3) . . ?
I7 Bi2 I8 93.38(3) . . ?
I8 Bi2 I4 87.00(3) . . ?
I8 Bi2 I4 172.92(3) . 3_765 ?
I8 Bi2 I2 90.92(3) . 3_765 ?
I8 Bi2 I5 89.89(3) . . ?
I5 Bi3 I6 83.73(2) . . ?
I8 Bi3 I5 80.64(3) . . ?
I8 Bi3 I6 86.20(3) . . ?
I9 Bi3 I5 94.87(3) . . ?
I9 Bi3 I6 88.28(3) . . ?
I9 Bi3 I8 173.23(3) . . ?
I11 Bi3 I5 163.86(3) . . ?
I11 Bi3 I6 85.45(3) . . ?
I11 Bi3 I8 86.73(3) . . ?
I11 Bi3 I9 96.74(3) . . ?
I10 Bi3 I5 95.13(3) . . ?
I10 Bi3 I6 178.17(4) . . ?
I10 Bi3 I8 92.20(3) . . ?
I10 Bi3 I9 93.25(3) . . ?
I10 Bi3 I11 95.37(3) . . ?
Bi1 I4 Bi2 91.99(3) . . ?
Bi2 I4 Bi1 88.97(3) 3_765 . ?
Bi2 I4 Bi2 93.66(3) 3_765 . ?
Bi2 I2 Bi1 94.17(3) 3_765 . ?
Bi1 I5 Bi3 89.67(2) . . ?
Bi2 I5 Bi1 96.58(3) . . ?
Bi2 I5 Bi3 92.80(3) . . ?
Bi1 I6 Bi3 95.24(3) . . ?
Bi2 I8 Bi3 96.34(3) . . ?
O7 K2 O11 124.4(3) . . ?
O7 K2 C16 117.6(4) . . ?
O7 K2 C29 133.8(4) . . ?
O7 K2 C17 95.1(4) . . ?
O7 K2 N2 91.2(4) . . ?
O12 K2 O7 61.5(3) . . ?
O12 K2 O11 63.0(3) . . ?
O12 K2 O10 118.1(3) . . ?
O12 K2 O9 172.7(3) . . ?
O12 K2 O8 116.8(3) . . ?
O12 K2 C16 96.4(4) . . ?
O12 K2 C29 152.2(4) . . ?
O12 K2 C17 79.8(4) . . ?
O12 K2 N2 81.7(4) . . ?
O11 K2 C16 70.1(4) . . ?
O11 K2 C29 96.8(4) . . ?
O11 K2 C17 76.8(4) . . ?
O10 K2 O7 172.9(3) . . ?
O10 K2 O11 55.4(3) . . ?
O10 K2 C16 69.3(4) . . ?
O10 K2 C29 43.3(3) . . ?
O10 K2 C17 91.7(4) . . ?
O10 K2 N2 81.8(4) . . ?
O9 K2 O7 117.1(3) . . ?
O9 K2 O11 117.8(3) . . ?
O9 K2 O10 62.4(3) . . ?
O9 K2 O8 62.3(3) . . ?
O9 K2 C16 90.5(4) . . ?
O9 K2 C29 23.8(4) . . ?
O9 K2 C17 107.5(4) . . ?
O9 K2 N2 91.2(4) . . ?
O8 K2 O7 55.4(3) . . ?
O8 K2 O11 179.5(3) . . ?
O8 K2 O10 124.7(3) . . ?
O8 K2 C16 110.4(4) . . ?
O8 K2 C29 83.2(4) . . ?
O8 K2 C17 103.7(4) . . ?
O8 K2 N2 100.2(4) . . ?
C16 K2 C29 93.8(4) . . ?
C17 K2 C16 23.3(4) . . ?
C17 K2 C29 115.7(4) . . ?
N2 K2 O11 79.3(4) . . ?
N2 K2 C16 146.2(5) . . ?
N2 K2 C29 75.6(4) . . ?
N2 K2 C17 154.6(4) . . ?
O6 K1 C11 97.2(3) . . ?
O6 K1 C1 82.2(3) . . ?
O6 K1 C7 93.6(3) . 3_665 ?
O6 K1 C8 82.1(4) . 3_665 ?
O4 K1 O6 118.0(3) . . ?
O4 K1 N1 86.8(4) . . ?
O4 K1 C11 23.9(3) . . ?
O4 K1 C1 157.8(4) . . ?
O4 K1 C7 68.4(4) . 3_665 ?
O4 K1 C8 93.0(4) . 3_665 ?
O2 K1 O6 123.6(3) . . ?
O2 K1 O4 118.2(3) . . ?
O2 K1 N1 92.6(4) . . ?
O2 K1 C11 138.6(3) . . ?
O2 K1 C1 43.6(3) . . ?
O2 K1 C7 102.6(3) . 3_665 ?
O2 K1 C8 91.0(4) . 3_665 ?
O5 K1 O6 55.6(3) . . ?
O5 K1 O4 62.4(3) . . ?
O5 K1 O2 174.9(3) . . ?
O5 K1 N1 92.4(4) . . ?
O5 K1 C11 43.4(3) . . ?
O5 K1 C1 137.1(4) . . ?
O5 K1 C7 72.8(4) . 3_665 ?
O5 K1 C8 83.9(4) . 3_665 ?
O3 K1 O6 175.8(3) . . ?
O3 K1 O4 61.3(3) . . ?
O3 K1 O2 57.0(3) . . ?
O3 K1 O5 123.4(3) . . ?
O3 K1 N1 89.7(4) . . ?
O3 K1 C11 82.9(3) . . ?
O3 K1 C1 99.2(3) . . ?
O3 K1 C7 82.3(3) . 3_665 ?
O3 K1 C8 93.8(4) . 3_665 ?
O1 K1 O6 61.5(3) . . ?
O1 K1 O4 179.4(3) . . ?
O1 K1 O2 62.3(3) . . ?
O1 K1 O5 117.1(3) . . ?
O1 K1 O3 119.2(3) . . ?
O1 K1 N1 93.4(4) . . ?
O1 K1 C11 155.8(4) . . ?
O1 K1 C1 22.8(3) . . ?
O1 K1 C7 111.3(4) . 3_665 ?
O1 K1 C8 86.7(4) . 3_665 ?
N1 K1 O6 94.4(4) . . ?
N1 K1 C11 76.0(4) . . ?
N1 K1 C1 82.3(4) . . ?
N1 K1 C7 154.9(4) . 3_665 ?
N1 K1 C8 176.0(5) . 3_665 ?
C1 K1 C11 158.2(4) . . ?
C7 K1 C11 79.4(4) 3_665 . ?
C7 K1 C1 122.4(4) 3_665 . ?
C8 K1 C11 102.3(4) 3_665 . ?
C8 K1 C1 99.2(4) 3_665 . ?
C8 K1 C7 24.6(4) 3_665 3_665 ?
C14 O6 K1 117.0(8) . . ?
C14 O6 C19 117.6(12) . . ?
C19 O6 K1 114.6(9) . . ?
C11 O4 K1 107.0(8) . . ?
C10 O4 K1 108.5(9) . . ?
C10 O4 C11 111.0(11) . . ?
C40 O7 K2 115.5(8) . . ?
C21 O7 K2 120.3(9) . . ?
C21 O7 C40 116.0(12) . . ?
C38 O12 K2 113.4(8) . . ?
C38 O12 C39 109.4(10) . . ?
C39 O12 K2 114.1(7) . . ?
C32 O11 K2 118.2(8) . . ?
C32 O11 C37 117.7(11) . . ?
C37 O11 K2 111.8(8) . . ?
C30 O10 K2 115.7(8) . . ?
C31 O10 K2 119.5(9) . . ?
C31 O10 C30 118.9(12) . . ?
C2 O2 K1 117.4(9) . . ?
C3 O2 K1 121.1(8) . . ?
C3 O2 C2 117.5(11) . . ?
C13 O5 K1 120.9(9) . . ?
C13 O5 C12 115.5(12) . . ?
C12 O5 K1 116.8(9) . . ?
C4 O3 K1 123.2(8) . . ?
C4 O3 C9 115.9(12) . . ?
C9 O3 K1 118.7(9) . . ?
C20 O1 K1 113.2(8) . . ?
C1 O1 K1 111.6(8) . . ?
C1 O1 C20 109.8(11) . . ?
C29 O9 K2 109.0(8) . . ?
C29 O9 C28 109.1(11) . . ?
C28 O9 K2 111.9(8) . . ?
C22 O8 K2 121.1(9) . . ?
C22 O8 C27 118.1(13) . . ?
C27 O8 K2 115.3(9) . . ?
C35 C36 C32 121.3(14) . . ?
O6 C14 C18 123.8(13) . . ?
O6 C14 C13 116.6(13) . . ?
C18 C14 C13 119.5(14) . . ?
O2 C2 C1 110.5(11) . . ?
C17 C16 K2 65.5(8) . . ?
C15 C16 K2 102.7(9) . . ?
C15 C16 C17 116.9(17) . . ?
C3 C4 O3 114.8(13) . . ?
C6 C4 O3 124.8(14) . . ?
C6 C4 C3 120.2(14) . . ?
O12 C38 C37 108.6(10) . . ?
O10 C30 C29 111.8(11) . . ?
C17 C18 C14 119.7(15) . . ?
O2 C3 C5 122.0(13) . . ?
C4 C3 O2 117.3(13) . . ?
C4 C3 C5 120.4(14) . . ?
O9 C29 K2 47.2(5) . . ?
O9 C29 C30 106.0(11) . . ?
C30 C29 K2 81.3(6) . . ?
C34 C33 C31 120.9(15) . . ?
O5 C13 C14 114.9(14) . . ?
C15 C13 O5 127.1(15) . . ?
C15 C13 C14 118.0(15) . . ?
C16 C17 K2 91.2(9) . . ?
C18 C17 K2 95.0(9) . . ?
C18 C17 C16 121.6(16) . . ?
C41 N1 K1 167.1(15) . . ?
N2 C43 C44 178(2) . . ?
O8 C22 C26 125.6(15) . . ?
O8 C22 C21 115.6(15) . . ?
C26 C22 C21 118.8(16) . . ?
O11 C32 C36 125.9(13) . . ?
O11 C32 C31 114.2(13) . . ?
C31 C32 C36 119.6(15) . . ?
O3 C9 C10 110.4(13) . . ?
O7 C40 C39 111.9(12) . . ?
O11 C37 C38 110.4(11) . . ?
C43 N2 K2 175.7(14) . . ?
C13 C15 C16 124.1(16) . . ?
C35 C34 C33 119.9(15) . . ?
C7 C5 C3 120.2(15) . . ?
C22 C26 C25 117.8(15) . . ?
O8 C27 C28 110.8(14) . . ?
O6 C19 C20 109.8(13) . . ?
C24 C25 C26 121.2(16) . . ?
N1 C41 C42 178(2) . . ?
C34 C35 C36 119.9(15) . . ?
O12 C39 C40 104.9(11) . . ?
O5 C12 C11 111.0(13) . . ?
C21 C23 C24 120.1(16) . . ?
O7 C21 C22 113.6(14) . . ?
C23 C21 O7 126.4(15) . . ?
C23 C21 C22 119.9(16) . . ?
O1 C20 C19 106.4(12) . . ?
N3 C45 C46 176.2(18) . . ?
O4 C11 K1 49.1(6) . . ?
O4 C11 C12 106.8(12) . . ?
C12 C11 K1 81.6(8) . . ?
O1 C1 K1 45.7(6) . . ?
O1 C1 C2 108.1(11) . . ?
C2 C1 K1 82.0(7) . . ?
O10 C31 C33 123.0(15) . . ?
O10 C31 C32 118.9(15) . . ?
C32 C31 C33 118.0(15) . . ?
C4 C6 C8 118.9(16) . . ?
O4 C10 C9 107.0(12) . . ?
C25 C24 C23 122.1(16) . . ?
C27 C28 O9 105.4(12) . . ?
C5 C7 K1 113.7(10) . 3_665 ?
C5 C7 C8 118.3(15) . . ?
C8 C7 K1 68.0(9) . 3_665 ?
C6 C8 K1 105.0(10) . 3_665 ?
C6 C8 C7 121.7(16) . . ?
C7 C8 K1 87.4(9) . 3_665 ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
