# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013


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#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material 
#  of the CCDC or of third parties, and may not be copied or further 
#  disseminated in any form, whether machine-readable or not,  
#  except for the purpose of generating routine backup copies 
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk 
#
#  Bona fide researchers may freely download Mercury and enCIFer
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data_c:\xraydata\etsulf\1081
_database_code_depnum_ccdc_archive 'CCDC 903495'
#TrackingRef '14303_web_deposit_cif_file_0_PROFJOHNWALLIS_1348751138.WALLIS_DALTON_ALLCIFS.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
Tris(bis(ethylenedithio)tetrathiafulvalene) bis(sulfamate) dihydrate
;
_chemical_name_common            ET3(H2NSO3)2.2H2O
_chemical_melting_point          491
_chemical_formula_moiety         '3(C10 H8 S8), 2(H2 N O3 S), 2(H2 O)'
_chemical_formula_sum            'C30 H32 N2 O8 S26'
_chemical_formula_weight         1382.14
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   6.57440(10)
_cell_length_b                   11.5052(3)
_cell_length_c                   16.3531(4)
_cell_angle_alpha                90.0380(10)
_cell_angle_beta                 93.6690(10)
_cell_angle_gamma                96.9530(10)
_cell_volume                     1225.29(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    15400
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48
_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.873
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             706
_exptl_absorpt_coefficient_mu    1.183
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7644
_exptl_absorpt_correction_T_max  0.9767
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_measurement_device_type  
'Bruker-Nonius APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20949
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.06
_diffrn_reflns_theta_max         27.61
_reflns_number_total             5602
_reflns_number_gt                4944
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Mercury
_computing_publication_material  ?
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+2.2975P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5601
_refine_ls_number_parameters     362
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_ref         0.0716
_refine_ls_wR_factor_gt          0.0676
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.23786(8) 0.01501(5) -0.27135(4) 0.01651(13) Uani 1 1 d . . .
S2 S -0.29309(9) -0.02514(5) -0.31938(4) 0.01674(13) Uani 1 1 d . . .
S3 S 0.12710(8) 0.09967(5) -0.11231(3) 0.01344(12) Uani 1 1 d . . .
S4 S -0.31802(8) 0.05981(5) -0.15059(3) 0.01364(12) Uani 1 1 d . . .
S5 S 0.05626(8) 0.20046(5) 0.06549(3) 0.01283(12) Uani 1 1 d . . .
S6 S -0.38952(8) 0.17260(5) 0.02614(3) 0.01493(12) Uani 1 1 d . . .
S7 S 0.03790(8) 0.30316(5) 0.23038(3) 0.01470(12) Uani 1 1 d . . .
S8 S -0.49504(9) 0.27294(6) 0.18058(4) 0.02154(14) Uani 1 1 d . . .
S9 S -0.00424(9) 0.31482(5) 0.73151(3) 0.01489(12) Uani 1 1 d . . .
S10 S -0.49116(9) 0.39486(7) 0.76995(4) 0.02575(16) Uani 1 1 d . . .
S11 S 0.11482(8) 0.41372(5) 0.89709(3) 0.01447(12) Uani 1 1 d . . .
S12 S -0.28976(9) 0.47932(6) 0.92702(4) 0.01749(13) Uani 1 1 d . . .
S13 S 0.22205(9) 0.35917(5) 0.48452(4) 0.01480(12) Uani 1 1 d . . .
O1 O -0.0018(3) 0.33662(16) 0.47445(11) 0.0237(4) Uani 1 1 d . . .
O2 O 0.3097(3) 0.40225(16) 0.40897(10) 0.0203(4) Uani 1 1 d . . .
O3 O 0.3184(3) 0.26120(15) 0.51846(11) 0.0223(4) Uani 1 1 d . . .
O4 O -0.6728(4) -0.1478(2) -0.47775(15) 0.0379(5) Uani 1 1 d . . .
N3 N 0.2624(4) 0.4617(2) 0.55614(13) 0.0195(4) Uani 1 1 d . . .
C1 C 0.1057(4) 0.0308(2) -0.37062(15) 0.0182(5) Uani 1 1 d . . .
C2 C -0.0881(4) -0.0546(2) -0.38297(16) 0.0190(5) Uani 1 1 d . . .
C3 C 0.0426(3) 0.03609(19) -0.20755(14) 0.0121(4) Uani 1 1 d . . .
C4 C -0.1617(3) 0.01957(19) -0.22618(13) 0.0115(4) Uani 1 1 d . . .
C5 C -0.1178(3) 0.10767(19) -0.07954(14) 0.0118(4) Uani 1 1 d . . .
C6 C -0.1477(3) 0.1539(2) -0.00510(13) 0.0118(4) Uani 1 1 d . . .
C7 C -0.0957(3) 0.24721(19) 0.14019(13) 0.0119(4) Uani 1 1 d . . .
C8 C -0.3011(3) 0.2340(2) 0.12211(14) 0.0137(4) Uani 1 1 d . . .
C9 C -0.1602(3) 0.3688(2) 0.28035(15) 0.0145(5) Uani 1 1 d . . .
C10 C -0.3634(4) 0.2915(2) 0.28124(14) 0.0150(5) Uani 1 1 d . . .
C11 C -0.2168(4) 0.3384(2) 0.65955(15) 0.0202(5) Uani 1 1 d . . .
C12 C -0.4243(4) 0.2982(2) 0.69146(16) 0.0181(5) Uani 1 1 d . . .
C13 C -0.0789(3) 0.3797(2) 0.81960(14) 0.0129(4) Uani 1 1 d . . .
C14 C -0.2671(3) 0.4102(2) 0.83363(14) 0.0148(5) Uani 1 1 d . . .
C15 C -0.0373(3) 0.4770(2) 0.96249(14) 0.0138(4) Uani 1 1 d . . .
H1A H 0.202(4) 0.012(3) -0.4071(19) 0.027(8) Uiso 1 1 d . . .
H1B H 0.079(4) 0.113(2) -0.3787(16) 0.014(7) Uiso 1 1 d . . .
H2A H -0.151(5) -0.052(3) -0.436(2) 0.034(9) Uiso 1 1 d . . .
H2B H -0.061(5) -0.136(3) -0.3706(19) 0.030(8) Uiso 1 1 d . . .
H3A H 0.389(5) 0.488(3) 0.564(2) 0.039(10) Uiso 1 1 d . . .
H3B H 0.193(5) 0.515(3) 0.5440(18) 0.021(8) Uiso 1 1 d . . .
H4A H -0.566(6) -0.178(3) -0.491(2) 0.057(12) Uiso 1 1 d . . .
H4B H -0.768(7) -0.203(4) -0.472(3) 0.065(13) Uiso 1 1 d . . .
H9A H -0.097(4) 0.381(2) 0.3323(18) 0.019(7) Uiso 1 1 d . . .
H9B H -0.175(4) 0.443(2) 0.2521(16) 0.011(6) Uiso 1 1 d . . .
H10A H -0.458(5) 0.333(3) 0.3117(19) 0.030(8) Uiso 1 1 d . . .
H10B H -0.348(4) 0.216(2) 0.3023(17) 0.018(7) Uiso 1 1 d . . .
H11A H -0.192(4) 0.290(3) 0.6139(19) 0.029(8) Uiso 1 1 d . . .
H11B H -0.204(4) 0.417(3) 0.6433(18) 0.023(7) Uiso 1 1 d . . .
H12A H -0.531(5) 0.298(3) 0.650(2) 0.034(9) Uiso 1 1 d . . .
H12B H -0.431(4) 0.223(3) 0.7124(18) 0.023(7) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.0124(3) 0.0227(3) 0.0147(3) -0.0055(2) 0.0035(2) 0.0017(2)
S2 0.0143(3) 0.0243(3) 0.0110(3) -0.0052(2) 0.0006(2) 0.0000(2)
S3 0.0106(2) 0.0180(3) 0.0117(3) -0.0037(2) 0.0010(2) 0.0016(2)
S4 0.0108(2) 0.0198(3) 0.0103(3) -0.0036(2) 0.0007(2) 0.0019(2)
S5 0.0102(2) 0.0180(3) 0.0103(3) -0.0033(2) 0.00046(19) 0.0020(2)
S6 0.0102(2) 0.0233(3) 0.0113(3) -0.0043(2) 0.0004(2) 0.0025(2)
S7 0.0119(3) 0.0201(3) 0.0118(3) -0.0053(2) 0.0006(2) 0.0006(2)
S8 0.0109(3) 0.0387(4) 0.0154(3) -0.0112(3) 0.0014(2) 0.0045(2)
S9 0.0174(3) 0.0159(3) 0.0114(3) -0.0035(2) 0.0008(2) 0.0026(2)
S10 0.0138(3) 0.0451(4) 0.0181(3) -0.0130(3) -0.0036(2) 0.0051(3)
S11 0.0140(3) 0.0181(3) 0.0115(3) -0.0034(2) -0.0002(2) 0.0030(2)
S12 0.0131(3) 0.0270(3) 0.0128(3) -0.0060(2) -0.0010(2) 0.0050(2)
S13 0.0161(3) 0.0163(3) 0.0121(3) -0.0010(2) 0.0003(2) 0.0029(2)
O1 0.0177(9) 0.0278(10) 0.0247(10) -0.0048(8) -0.0004(7) 0.0007(7)
O2 0.0242(9) 0.0223(9) 0.0153(9) 0.0011(7) 0.0054(7) 0.0038(7)
O3 0.0275(9) 0.0184(9) 0.0205(9) 0.0004(7) -0.0060(7) 0.0044(7)
O4 0.0352(12) 0.0283(12) 0.0512(15) -0.0083(10) 0.0147(11) 0.0016(10)
N3 0.0210(11) 0.0200(11) 0.0178(11) -0.0051(9) 0.0009(9) 0.0036(9)
C1 0.0197(12) 0.0210(13) 0.0147(12) 0.0002(10) 0.0050(9) 0.0029(10)
C2 0.0190(12) 0.0264(14) 0.0118(12) -0.0057(10) 0.0008(9) 0.0032(10)
C3 0.0135(10) 0.0117(11) 0.0108(11) -0.0022(8) 0.0019(8) -0.0003(8)
C4 0.0140(10) 0.0116(10) 0.0090(10) -0.0012(8) 0.0024(8) 0.0010(8)
C5 0.0113(10) 0.0118(11) 0.0128(11) 0.0000(8) 0.0013(8) 0.0033(8)
C6 0.0101(10) 0.0145(11) 0.0105(11) -0.0004(8) -0.0007(8) 0.0014(8)
C7 0.0149(10) 0.0116(11) 0.0095(11) -0.0015(8) 0.0022(8) 0.0023(8)
C8 0.0152(11) 0.0160(11) 0.0101(11) -0.0035(9) 0.0011(8) 0.0027(9)
C9 0.0155(11) 0.0154(12) 0.0128(12) -0.0046(9) 0.0012(9) 0.0024(9)
C10 0.0154(11) 0.0176(12) 0.0122(11) -0.0031(9) 0.0017(9) 0.0024(9)
C11 0.0258(13) 0.0258(14) 0.0104(12) -0.0002(10) 0.0002(10) 0.0096(11)
C12 0.0207(12) 0.0173(12) 0.0150(12) -0.0032(10) -0.0068(9) 0.0018(10)
C13 0.0156(11) 0.0118(11) 0.0109(11) -0.0030(8) -0.0018(8) 0.0008(8)
C14 0.0150(11) 0.0199(12) 0.0091(11) -0.0039(9) -0.0003(8) 0.0005(9)
C15 0.0132(10) 0.0140(11) 0.0144(11) -0.0021(9) 0.0007(8) 0.0022(8)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C3 1.744(2) . ?
S1 C1 1.811(3) . ?
S2 C4 1.748(2) . ?
S2 C2 1.817(2) . ?
S3 C5 1.742(2) . ?
S3 C3 1.749(2) . ?
S4 C5 1.736(2) . ?
S4 C4 1.754(2) . ?
S5 C6 1.745(2) . ?
S5 C7 1.751(2) . ?
S6 C6 1.739(2) . ?
S6 C8 1.756(2) . ?
S7 C7 1.748(2) . ?
S7 C9 1.819(2) . ?
S8 C8 1.742(2) . ?
S8 C10 1.810(2) . ?
S9 C13 1.747(2) . ?
S9 C11 1.815(3) . ?
S10 C14 1.740(2) . ?
S10 C12 1.807(3) . ?
S11 C15 1.728(2) . ?
S11 C13 1.747(2) . ?
S12 C15 1.726(2) . ?
S12 C14 1.745(2) . ?
S13 O3 1.4521(18) . ?
S13 O2 1.4584(17) . ?
S13 O1 1.4619(18) . ?
S13 N3 1.648(2) . ?
O4 H4A 0.86(4) . ?
O4 H4B 0.85(4) . ?
N3 H3A 0.85(4) . ?
N3 H3B 0.82(3) . ?
C1 C2 1.515(3) . ?
C1 H1A 0.94(3) . ?
C1 H1B 0.99(3) . ?
C2 H2A 0.94(3) . ?
C2 H2B 1.00(3) . ?
C3 C4 1.348(3) . ?
C5 C6 1.363(3) . ?
C7 C8 1.354(3) . ?
C9 C10 1.513(3) . ?
C9 H9A 0.92(3) . ?
C9 H9B 0.98(3) . ?
C10 H10A 0.99(3) . ?
C10 H10B 0.95(3) . ?
C11 C12 1.512(4) . ?
C11 H11A 0.96(3) . ?
C11 H11B 0.93(3) . ?
C12 H12A 0.94(3) . ?
C12 H12B 0.92(3) . ?
C13 C14 1.360(3) . ?
C15 C15 1.373(5) 2_567 ?
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
C3 S1 C1 100.12(11) . . ?
C4 S2 C2 103.04(11) . . ?
C5 S3 C3 95.37(10) . . ?
C5 S4 C4 95.73(10) . . ?
C6 S5 C7 95.73(10) . . ?
C6 S6 C8 95.47(11) . . ?
C7 S7 C9 101.70(11) . . ?
C8 S8 C10 101.57(11) . . ?
C13 S9 C11 100.39(11) . . ?
C14 S10 C12 101.08(11) . . ?
C15 S11 C13 95.60(11) . . ?
C15 S12 C14 95.73(11) . . ?
O3 S13 O2 112.50(11) . . ?
O3 S13 O1 113.71(11) . . ?
O2 S13 O1 111.37(11) . . ?
O3 S13 N3 105.07(12) . . ?
O2 S13 N3 110.19(11) . . ?
O1 S13 N3 103.38(11) . . ?
H4A O4 H4B 108(4) . . ?
S13 N3 H3A 112(2) . . ?
S13 N3 H3B 109(2) . . ?
H3A N3 H3B 111(3) . . ?
C2 C1 S1 112.18(18) . . ?
C2 C1 H1A 109.5(18) . . ?
S1 C1 H1A 102.7(18) . . ?
C2 C1 H1B 112.2(15) . . ?
S1 C1 H1B 110.1(15) . . ?
H1A C1 H1B 110(2) . . ?
C1 C2 S2 114.31(18) . . ?
C1 C2 H2A 112.6(19) . . ?
S2 C2 H2A 102.2(19) . . ?
C1 C2 H2B 111.3(17) . . ?
S2 C2 H2B 106.2(18) . . ?
H2A C2 H2B 110(3) . . ?
C4 C3 S1 127.60(18) . . ?
C4 C3 S3 117.34(17) . . ?
S1 C3 S3 114.74(12) . . ?
C3 C4 S2 128.60(17) . . ?
C3 C4 S4 116.47(17) . . ?
S2 C4 S4 114.68(12) . . ?
C6 C5 S4 122.97(17) . . ?
C6 C5 S3 121.92(17) . . ?
S4 C5 S3 115.02(13) . . ?
C5 C6 S6 122.87(17) . . ?
C5 C6 S5 122.06(17) . . ?
S6 C6 S5 115.06(13) . . ?
C8 C7 S7 127.88(17) . . ?
C8 C7 S5 116.64(17) . . ?
S7 C7 S5 115.47(12) . . ?
C7 C8 S8 128.87(18) . . ?
C7 C8 S6 117.10(17) . . ?
S8 C8 S6 114.02(12) . . ?
C10 C9 S7 114.29(16) . . ?
C10 C9 H9A 112.2(17) . . ?
S7 C9 H9A 100.2(17) . . ?
C10 C9 H9B 111.5(15) . . ?
S7 C9 H9B 106.3(15) . . ?
H9A C9 H9B 112(2) . . ?
C9 C10 S8 112.62(17) . . ?
C9 C10 H10A 108.4(18) . . ?
S8 C10 H10A 102.4(17) . . ?
C9 C10 H10B 112.4(16) . . ?
S8 C10 H10B 107.9(16) . . ?
H10A C10 H10B 113(2) . . ?
C12 C11 S9 113.10(18) . . ?
C12 C11 H11A 110.5(18) . . ?
S9 C11 H11A 101.4(18) . . ?
C12 C11 H11B 112.5(17) . . ?
S9 C11 H11B 109.9(18) . . ?
H11A C11 H11B 109(3) . . ?
C11 C12 S10 112.34(18) . . ?
C11 C12 H12A 111.8(19) . . ?
S10 C12 H12A 104.3(19) . . ?
C11 C12 H12B 112.0(18) . . ?
S10 C12 H12B 108.4(18) . . ?
H12A C12 H12B 108(3) . . ?
C14 C13 S9 127.73(18) . . ?
C14 C13 S11 116.55(17) . . ?
S9 C13 S11 115.68(13) . . ?
C13 C14 S10 129.28(18) . . ?
C13 C14 S12 116.60(17) . . ?
S10 C14 S12 114.08(13) . . ?
C15 C15 S12 122.1(2) 2_567 . ?
C15 C15 S11 122.4(2) 2_567 . ?
S12 C15 S11 115.52(13) . . ?
_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.097


data_borpbaxx
_database_code_depnum_ccdc_archive 'CCDC 903496'
#TrackingRef '14303_web_deposit_cif_file_0_PROFJOHNWALLIS_1348751138.WALLIS_DALTON_ALLCIFS.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
Bis(Bis(ethylenedithio)tetrathiafulvalene) B5O6(OH)4
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C10 H8 S8), B5 H4 O10'
_chemical_formula_sum            'C20 H20 B5 O10 S16'
_chemical_formula_weight         987.53
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   9.1142(3)
_cell_length_b                   11.5777(4)
_cell_length_c                   18.1484(7)
_cell_angle_alpha                97.136(2)
_cell_angle_beta                 101.350(2)
_cell_angle_gamma                104.651(2)
_cell_volume                     1785.72(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    30162
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48
_exptl_crystal_description       'cut plate'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.837
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             978
_exptl_absorpt_coefficient_mu    1.020
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_special_details           ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_measurement_device_type  
;
'Bruker-Nonius APEX II CCD camera on \k-goniostat'
;
_diffrn_measurement_method       '\f & \w scans'
_diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26707
_diffrn_reflns_av_R_equivalents  0.0675
_diffrn_reflns_av_sigmaI/netI    0.0775
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         27.74
_reflns_number_total             8141
_reflns_number_gt                5418
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+15.5099P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8141
_refine_ls_number_parameters     477
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.1453
_refine_ls_R_factor_gt           0.0933
_refine_ls_wR_factor_ref         0.2166
_refine_ls_wR_factor_gt          0.1871
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.5397(2) 2.09458(15) 1.80681(10) 0.0332(4) Uani 1 1 d D . .
S2 S 0.28822(19) 1.81365(15) 1.81250(10) 0.0278(4) Uani 1 1 d D . .
S3 S 0.5458(2) 1.97627(14) 1.65503(10) 0.0269(4) Uani 1 1 d . . .
S4 S 0.3380(2) 1.73845(14) 1.65811(10) 0.0272(4) Uani 1 1 d . . .
S5 S 0.6020(2) 1.87008(14) 1.49440(10) 0.0278(4) Uani 1 1 d . . .
S6 S 0.3908(2) 1.63170(15) 1.49403(11) 0.0319(4) Uani 1 1 d . . .
S7 S 0.6874(2) 1.79587(17) 1.35216(11) 0.0389(5) Uani 1 1 d D . .
S8 S 0.4357(3) 1.51365(16) 1.34899(12) 0.0419(5) Uani 1 1 d D . .
S11 S 0.0698(2) 1.04455(15) 0.73747(10) 0.0296(4) Uani 1 1 d D . .
S12 S -0.1955(3) 0.76571(17) 0.74033(11) 0.0434(5) Uani 1 1 d D . .
S13 S 0.0760(2) 0.92359(14) 0.58634(10) 0.0278(4) Uani 1 1 d . . .
S14 S -0.1392(2) 0.68931(15) 0.58986(10) 0.0323(4) Uani 1 1 d . . .
S15 S 0.1234(2) 0.81558(15) 0.42425(10) 0.0314(4) Uani 1 1 d . B .
S16 S -0.0856(2) 0.57760(15) 0.42774(10) 0.0331(4) Uani 1 1 d . B .
S17 S 0.1668(3) 0.74202(17) 0.27045(12) 0.0431(5) Uani 1 1 d D . .
S18 S -0.0807(3) 0.46184(17) 0.27555(12) 0.0508(6) Uani 1 1 d D . .
O1 O -0.2136(6) 1.4048(4) 0.9779(3) 0.0384(12) Uani 1 1 d . . .
H1 H -0.1560 1.4737 0.9771 0.046 Uiso 1 1 calc R . .
O2 O -0.2029(5) 1.2078(4) 0.9896(3) 0.0303(11) Uani 1 1 d . . .
O3 O -0.2049(5) 1.0080(4) 0.9936(3) 0.0281(10) Uani 1 1 d . . .
H3 H -0.1474 0.9617 0.9929 0.034 Uiso 1 1 calc R . .
O4 O 0.0311(5) 1.1527(4) 0.9921(3) 0.0288(10) Uani 1 1 d . . .
O5 O 0.0307(5) 1.3623(4) 0.9963(3) 0.0292(11) Uani 1 1 d . . .
O6 O 0.4615(7) 1.3412(6) 1.1704(3) 0.0513(15) Uani 1 1 d . . .
H6 H 0.5569 1.3519 1.1723 0.062 Uiso 1 1 calc R . .
O7 O 0.4620(6) 1.3331(5) 1.0396(3) 0.0395(12) Uani 1 1 d . . .
O8 O 0.4621(6) 1.3372(5) 0.9104(3) 0.0374(12) Uani 1 1 d . . .
H8 H 0.5582 1.3568 0.9307 0.045 Uiso 1 1 calc R . .
O9 O 0.2213(5) 1.2908(4) 0.9459(3) 0.0332(11) Uani 1 1 d . . .
O10 O 0.2289(5) 1.3117(4) 1.0807(3) 0.0307(11) Uani 1 1 d . . .
C1 C 0.4460(8) 2.0513(5) 1.8820(4) 0.0289(15) Uani 1 1 d D . .
H1A H 0.5074 2.1052 1.9309 0.035 Uiso 1 1 calc R . .
H1B H 0.3411 2.0642 1.8713 0.035 Uiso 1 1 calc R . .
C2 C 0.4289(7) 1.9207(5) 1.8911(3) 0.0264(14) Uani 1 1 d D . .
H2A H 0.3965 1.9085 1.9392 0.032 Uiso 1 1 calc R . .
H2B H 0.5316 1.9046 1.8952 0.032 Uiso 1 1 calc R . .
C3 C 0.4716(7) 1.9629(6) 1.7374(4) 0.0250(13) Uani 1 1 d . . .
C4 C 0.3745(8) 1.8538(6) 1.7381(4) 0.0262(14) Uani 1 1 d . . .
C5 C 0.4567(7) 1.8257(6) 1.6102(4) 0.0257(14) Uani 1 1 d . . .
C6 C 0.4796(7) 1.7798(6) 1.5410(4) 0.0253(14) Uani 1 1 d . . .
C7 C 0.5824(8) 1.7531(6) 1.4200(4) 0.0255(14) Uani 1 1 d . A .
C8 C 0.4846(8) 1.6429(6) 1.4190(4) 0.0264(14) Uani 1 1 d . A .
C9 C 0.6257(9) 1.6655(6) 1.2769(4) 0.0427(19) Uani 1 1 d D A 3
H9A H 0.6335 1.6937 1.2281 0.051 Uiso 1 1 calc R A 3
H9B H 0.6990 1.6159 1.2865 0.051 Uiso 1 1 calc R A 3
C10 C 0.4637(10) 1.5863(8) 1.2677(5) 0.057(2) Uani 1 1 d D A 3
H10A H 0.4374 1.5227 1.2216 0.068 Uiso 1 1 calc R A 3
H10B H 0.3901 1.6360 1.2593 0.068 Uiso 1 1 calc R A 3
C11 C -0.0595(10) 1.0117(7) 0.8003(5) 0.027(2) Uani 0.784(17) 1 d PD B 5
H11A H -0.0158 1.0716 0.8486 0.032 Uiso 0.784(17) 1 calc PR B 5
H11B H -0.1614 1.0224 0.7763 0.032 Uiso 0.784(17) 1 calc PR B 5
C11A C 0.006(3) 0.988(3) 0.8178(10) 0.019(6) Uiso 0.216(17) 1 d PD B 6
H11C H 0.0746 0.9399 0.8387 0.023 Uiso 0.216(17) 1 calc PR B 6
H11D H 0.0191 1.0582 0.8582 0.023 Uiso 0.216(17) 1 calc PR B 6
C12 C -0.0868(10) 0.8858(6) 0.8190(4) 0.026(2) Uani 0.784(17) 1 d PD B 5
H12A H -0.1432 0.8814 0.8605 0.031 Uiso 0.784(17) 1 calc PR B 5
H12B H 0.0156 0.8725 0.8388 0.031 Uiso 0.784(17) 1 calc PR B 5
C12A C -0.161(3) 0.9107(14) 0.7982(15) 0.019(6) Uiso 0.216(17) 1 d PD B 6
H12C H -0.2275 0.9552 0.7710 0.023 Uiso 0.216(17) 1 calc PR B 6
H12D H -0.1932 0.8985 0.8463 0.023 Uiso 0.216(17) 1 calc PR B 6
C13 C 0.0021(8) 0.9121(6) 0.6688(4) 0.0255(14) Uani 1 1 d . B .
C14 C -0.0971(8) 0.8048(6) 0.6692(4) 0.0299(15) Uani 1 1 d . B .
C15 C -0.0151(8) 0.7734(6) 0.5419(4) 0.0273(14) Uani 1 1 d . B .
C16 C 0.0078(8) 0.7262(6) 0.4738(4) 0.0285(14) Uani 1 1 d . . .
C17 C 0.0831(9) 0.7012(6) 0.3451(4) 0.0317(16) Uani 1 1 d . B .
C18 C -0.0125(9) 0.5924(6) 0.3462(4) 0.0320(16) Uani 1 1 d . B .
C19 C 0.040(2) 0.6314(11) 0.1912(7) 0.040(3) Uiso 0.50 1 d PD C 7
H19A H -0.0624 0.6488 0.1803 0.049 Uiso 0.50 1 calc PR C 7
H19B H 0.0837 0.6410 0.1458 0.049 Uiso 0.50 1 calc PR C 7
C19A C 0.086(3) 0.6114(13) 0.1951(9) 0.033(5) Uiso 0.30 1 d PD C 8
H19C H -0.0152 0.6168 0.1659 0.039 Uiso 0.30 1 calc PR C 8
H19D H 0.1566 0.6156 0.1598 0.039 Uiso 0.30 1 calc PR C 8
C19B C -0.010(3) 0.659(2) 0.2007(19) 0.041(7) Uiso 0.20 1 d PD C 9
H19E H -0.0954 0.6887 0.2137 0.049 Uiso 0.20 1 calc PR C 9
H19F H 0.0023 0.6801 0.1506 0.049 Uiso 0.20 1 calc PR C 9
C20 C 0.013(2) 0.5025(13) 0.2011(8) 0.040(3) Uiso 0.50 1 d PD C 7
H20A H 0.1150 0.4848 0.2112 0.049 Uiso 0.50 1 calc PR C 7
H20B H -0.0512 0.4498 0.1523 0.049 Uiso 0.50 1 calc PR C 7
C20A C 0.060(3) 0.4899(19) 0.2183(14) 0.033(5) Uiso 0.30 1 d PD C 8
H20C H 0.1605 0.4834 0.2475 0.039 Uiso 0.30 1 calc PR C 8
H20D H 0.0243 0.4261 0.1718 0.039 Uiso 0.30 1 calc PR C 8
C20B C -0.062(5) 0.522(3) 0.1900(12) 0.041(7) Uiso 0.20 1 d PD C 9
H20E H 0.0141 0.4898 0.1679 0.049 Uiso 0.20 1 calc PR C 9
H20F H -0.1638 0.4918 0.1524 0.049 Uiso 0.20 1 calc PR C 9
B1 B -0.1255(9) 1.3272(7) 0.9888(5) 0.0277(16) Uani 1 1 d . . .
B2 B -0.1217(9) 1.1218(6) 0.9931(4) 0.0253(15) Uani 1 1 d . . .
B3 B 0.1310(8) 1.2797(7) 1.0047(5) 0.0255(15) Uani 1 1 d . . .
B4 B 0.3810(9) 1.3229(7) 0.9653(5) 0.0280(16) Uani 1 1 d . . .
B5 B 0.3822(10) 1.3293(7) 1.0964(5) 0.0345(18) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.0472(11) 0.0258(8) 0.0237(9) 0.0008(7) 0.0180(8) -0.0006(7)
S2 0.0283(8) 0.0314(8) 0.0238(9) 0.0055(7) 0.0112(7) 0.0045(7)
S3 0.0341(9) 0.0228(8) 0.0226(9) 0.0036(6) 0.0113(7) 0.0027(7)
S4 0.0320(9) 0.0241(8) 0.0257(9) 0.0047(6) 0.0132(7) 0.0036(7)
S5 0.0364(9) 0.0219(8) 0.0245(9) 0.0027(6) 0.0149(7) 0.0025(7)
S6 0.0399(10) 0.0227(8) 0.0309(10) 0.0012(7) 0.0168(8) 0.0004(7)
S7 0.0513(12) 0.0350(10) 0.0303(10) 0.0035(8) 0.0238(9) 0.0026(8)
S8 0.0576(13) 0.0255(9) 0.0353(11) -0.0062(8) 0.0167(10) 0.0005(8)
S11 0.0408(10) 0.0244(8) 0.0247(9) 0.0037(7) 0.0163(8) 0.0048(7)
S12 0.0613(13) 0.0311(9) 0.0319(11) -0.0017(8) 0.0295(10) -0.0079(9)
S13 0.0352(9) 0.0243(8) 0.0223(9) 0.0035(6) 0.0122(7) 0.0019(7)
S14 0.0395(10) 0.0270(8) 0.0247(9) 0.0005(7) 0.0150(8) -0.0043(7)
S15 0.0396(10) 0.0257(8) 0.0281(10) 0.0054(7) 0.0174(8) 0.0006(7)
S16 0.0438(10) 0.0243(8) 0.0246(9) 0.0000(7) 0.0168(8) -0.0064(7)
S17 0.0684(14) 0.0299(9) 0.0438(12) 0.0107(8) 0.0421(11) 0.0125(9)
S18 0.0869(17) 0.0271(9) 0.0377(12) -0.0013(8) 0.0354(12) 0.0025(10)
O1 0.031(3) 0.028(2) 0.061(4) 0.014(2) 0.017(3) 0.010(2)
O2 0.024(2) 0.027(2) 0.042(3) 0.008(2) 0.014(2) 0.0065(19)
O3 0.026(2) 0.024(2) 0.039(3) 0.009(2) 0.014(2) 0.0102(19)
O4 0.022(2) 0.027(2) 0.039(3) 0.004(2) 0.011(2) 0.0086(18)
O5 0.022(2) 0.023(2) 0.045(3) 0.011(2) 0.010(2) 0.0077(18)
O6 0.043(3) 0.080(4) 0.033(3) 0.007(3) 0.010(3) 0.023(3)
O7 0.037(3) 0.048(3) 0.032(3) 0.002(2) 0.015(2) 0.007(2)
O8 0.034(3) 0.049(3) 0.032(3) 0.009(2) 0.014(2) 0.012(2)
O9 0.035(3) 0.036(3) 0.034(3) 0.009(2) 0.014(2) 0.013(2)
O10 0.031(3) 0.029(2) 0.032(3) 0.005(2) 0.009(2) 0.006(2)
C1 0.031(4) 0.033(3) 0.025(4) 0.005(3) 0.018(3) 0.006(3)
C2 0.028(3) 0.035(4) 0.017(3) 0.010(3) 0.010(3) 0.006(3)
C3 0.029(3) 0.023(3) 0.021(3) 0.004(3) 0.005(3) 0.004(3)
C4 0.030(3) 0.028(3) 0.021(3) 0.003(3) 0.009(3) 0.008(3)
C5 0.027(3) 0.024(3) 0.026(4) 0.008(3) 0.005(3) 0.006(3)
C6 0.028(3) 0.022(3) 0.025(4) 0.003(3) 0.010(3) 0.003(3)
C7 0.035(4) 0.028(3) 0.014(3) 0.002(3) 0.006(3) 0.011(3)
C8 0.034(4) 0.022(3) 0.021(3) -0.001(3) 0.010(3) 0.004(3)
C9 0.066(5) 0.038(4) 0.026(4) 0.001(3) 0.017(4) 0.017(4)
C10 0.065(6) 0.063(6) 0.040(5) -0.003(4) 0.015(5) 0.019(5)
C11 0.029(5) 0.030(4) 0.021(5) 0.001(3) 0.008(4) 0.008(4)
C12 0.031(5) 0.026(4) 0.020(4) 0.009(3) 0.006(4) 0.003(4)
C13 0.031(3) 0.027(3) 0.017(3) -0.001(3) 0.009(3) 0.005(3)
C14 0.036(4) 0.030(3) 0.022(4) 0.004(3) 0.014(3) 0.002(3)
C15 0.027(3) 0.025(3) 0.031(4) 0.004(3) 0.013(3) 0.005(3)
C16 0.030(3) 0.030(3) 0.022(4) 0.004(3) 0.006(3) 0.003(3)
C17 0.046(4) 0.027(3) 0.032(4) 0.012(3) 0.027(3) 0.012(3)
C18 0.049(4) 0.028(3) 0.027(4) 0.007(3) 0.023(3) 0.015(3)
B1 0.024(4) 0.030(4) 0.027(4) 0.007(3) 0.007(3) 0.003(3)
B2 0.032(4) 0.023(3) 0.023(4) 0.003(3) 0.008(3) 0.010(3)
B3 0.020(3) 0.025(4) 0.032(4) 0.005(3) 0.010(3) 0.005(3)
B4 0.032(4) 0.026(4) 0.029(4) 0.004(3) 0.014(3) 0.009(3)
B5 0.041(5) 0.030(4) 0.034(5) 0.001(3) 0.014(4) 0.012(4)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C3 1.742(7) . ?
S1 C1 1.804(6) . ?
S2 C4 1.745(7) . ?
S2 C2 1.803(6) . ?
S3 C5 1.741(7) . ?
S3 C3 1.765(7) . ?
S4 C5 1.727(7) . ?
S4 C4 1.763(7) . ?
S5 C7 1.737(6) . ?
S5 C6 1.748(6) . ?
S6 C6 1.728(7) . ?
S6 C8 1.747(7) . ?
S7 C7 1.747(7) . ?
S7 C9 1.793(6) . ?
S8 C8 1.738(7) . ?
S8 C10 1.815(7) . ?
S11 C13 1.741(6) . ?
S11 C11 1.801(7) . ?
S11 C11A 1.805(10) . ?
S12 C14 1.752(7) . ?
S12 C12A 1.784(10) . ?
S12 C12 1.791(7) . ?
S13 C15 1.738(7) . ?
S13 C13 1.764(6) . ?
S14 C15 1.739(7) . ?
S14 C14 1.748(7) . ?
S15 C17 1.739(7) . ?
S15 C16 1.743(7) . ?
S16 C16 1.734(7) . ?
S16 C18 1.749(7) . ?
S17 C17 1.739(7) . ?
S17 C19 1.785(9) . ?
S17 C19A 1.797(10) . ?
S17 C19B 1.797(11) . ?
S18 C18 1.745(7) . ?
S18 C20 1.784(9) . ?
S18 C20A 1.795(10) . ?
S18 C20B 1.800(11) . ?
O1 B1 1.356(9) . ?
O2 B2 1.383(8) . ?
O2 B1 1.387(9) . ?
O3 B2 1.346(8) . ?
O4 B2 1.351(9) . ?
O4 B3 1.484(8) . ?
O5 B1 1.351(8) . ?
O5 B3 1.482(8) . ?
O6 B5 1.367(10) . ?
O7 B5 1.373(9) . ?
O7 B4 1.379(10) . ?
O8 B4 1.354(9) . ?
O9 B4 1.368(9) . ?
O9 B3 1.469(8) . ?
O10 B5 1.327(10) . ?
O10 B3 1.434(9) . ?
C1 C2 1.513(7) . ?
C3 C4 1.349(9) . ?
C5 C6 1.377(9) . ?
C7 C8 1.354(9) . ?
C9 C10 1.493(8) . ?
C11 C12 1.508(8) . ?
C11A C12A 1.506(10) . ?
C13 C14 1.341(9) . ?
C15 C16 1.365(9) . ?
C17 C18 1.343(9) . ?
C19 C20 1.489(9) . ?
C19A C20A 1.494(10) . ?
C19B C20B 1.507(10) . ?
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
C3 S1 C1 102.8(3) . . ?
C4 S2 C2 99.0(3) . . ?
C5 S3 C3 95.4(3) . . ?
C5 S4 C4 95.5(3) . . ?
C7 S5 C6 94.8(3) . . ?
C6 S6 C8 95.6(3) . . ?
C7 S7 C9 104.9(3) . . ?
C8 S8 C10 98.8(4) . . ?
C13 S11 C11 101.4(3) . . ?
C13 S11 C11A 100.5(9) . . ?
C11 S11 C11A 24.0(8) . . ?
C14 S12 C12A 101.5(9) . . ?
C14 S12 C12 101.3(4) . . ?
C12A S12 C12 27.2(9) . . ?
C15 S13 C13 95.5(3) . . ?
C15 S14 C14 95.3(3) . . ?
C17 S15 C16 94.8(3) . . ?
C16 S16 C18 95.0(3) . . ?
C17 S17 C19 101.6(6) . . ?
C17 S17 C19A 104.7(8) . . ?
C19 S17 C19A 16.9(9) . . ?
C17 S17 C19B 91.6(14) . . ?
C19 S17 C19B 20.9(12) . . ?
C19A S17 C19B 37.4(14) . . ?
C18 S18 C20 104.1(6) . . ?
C18 S18 C20A 101.7(8) . . ?
C20 S18 C20A 17.4(9) . . ?
C18 S18 C20B 102.5(10) . . ?
C20 S18 C20B 24.7(13) . . ?
C20A S18 C20B 42.0(15) . . ?
B2 O2 B1 119.9(5) . . ?
B2 O4 B3 124.1(5) . . ?
B1 O5 B3 124.2(5) . . ?
B5 O7 B4 118.8(6) . . ?
B4 O9 B3 121.1(6) . . ?
B5 O10 B3 123.8(6) . . ?
C2 C1 S1 113.9(4) . . ?
C1 C2 S2 112.8(4) . . ?
C4 C3 S1 129.8(5) . . ?
C4 C3 S3 116.4(5) . . ?
S1 C3 S3 113.7(3) . . ?
C3 C4 S2 126.3(5) . . ?
C3 C4 S4 117.0(5) . . ?
S2 C4 S4 116.6(4) . . ?
C6 C5 S4 122.4(5) . . ?
C6 C5 S3 122.0(5) . . ?
S4 C5 S3 115.6(4) . . ?
C5 C6 S6 123.3(5) . . ?
C5 C6 S5 121.3(5) . . ?
S6 C6 S5 115.4(4) . . ?
C8 C7 S5 117.7(5) . . ?
C8 C7 S7 127.7(5) . . ?
S5 C7 S7 114.5(4) . . ?
C7 C8 S8 127.1(5) . . ?
C7 C8 S6 116.3(5) . . ?
S8 C8 S6 116.5(4) . . ?
C10 C9 S7 115.3(6) . . ?
C9 C10 S8 114.0(6) . . ?
C12 C11 S11 114.7(6) . . ?
C12A C11A S11 113.8(16) . . ?
C11 C12 S12 114.7(6) . . ?
C11A C12A S12 114.5(17) . . ?
C14 C13 S11 129.9(5) . . ?
C14 C13 S13 116.2(5) . . ?
S11 C13 S13 113.9(4) . . ?
C13 C14 S14 117.8(5) . . ?
C13 C14 S12 127.5(5) . . ?
S14 C14 S12 114.7(4) . . ?
C16 C15 S13 122.1(5) . . ?
C16 C15 S14 122.8(5) . . ?
S13 C15 S14 115.1(4) . . ?
C15 C16 S16 122.6(5) . . ?
C15 C16 S15 121.7(5) . . ?
S16 C16 S15 115.6(4) . . ?
C18 C17 S15 117.7(5) . . ?
C18 C17 S17 126.4(6) . . ?
S15 C17 S17 115.9(4) . . ?
C17 C18 S18 129.0(5) . . ?
C17 C18 S16 116.9(5) . . ?
S18 C18 S16 114.0(4) . . ?
C20 C19 S17 115.7(11) . . ?
C20A C19A S17 116.8(15) . . ?
C20B C19B S17 119(2) . . ?
C19 C20 S18 115.9(11) . . ?
C19A C20A S18 113.7(14) . . ?
C19B C20B S18 115(2) . . ?
O5 B1 O1 122.1(6) . . ?
O5 B1 O2 120.7(6) . . ?
O1 B1 O2 117.2(6) . . ?
O3 B2 O4 123.5(6) . . ?
O3 B2 O2 116.4(6) . . ?
O4 B2 O2 120.1(6) . . ?
O10 B3 O9 112.5(5) . . ?
O10 B3 O5 108.7(6) . . ?
O9 B3 O5 108.1(5) . . ?
O10 B3 O4 109.3(6) . . ?
O9 B3 O4 108.9(5) . . ?
O5 B3 O4 109.3(5) . . ?
O8 B4 O9 120.1(7) . . ?
O8 B4 O7 118.6(6) . . ?
O9 B4 O7 121.2(6) . . ?
O10 B5 O6 119.2(7) . . ?
O10 B5 O7 121.3(7) . . ?
O6 B5 O7 119.4(7) . . ?
_diffrn_measured_fraction_theta_max 0.968
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         1.432
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.146
_vrf_PLAT097_borpbaxx            
;
PROBLEM: Large Reported Max. (Positive) Residual Density 1.43 eA-3
RESPONSE: The highest difference density peak is 0.88 Ang from S12
which does not correspond to any sensible chemical entity.
This next highest peak is 1.01.
The quality of the diffraction data is not high, but this was the
best that could be obtained. There is some streaking of diffractions
especially notable in the planes of fixed index l.
;
_vrf_PLAT241_borpbaxx            
;
PROBLEM: Check High Ueq as Compared to Neighbors for S12
RESPONSE: S12 is adjacent to a disordered ethylene bridge
;
_vrf_PLAT432_borpbaxx            
;
PROBLEM: Short Inter X...Y Contact S2 .. S18 .. 3.29 Ang.
RESPONSE: Short S--S contacts between donors in these materials are
often observed
;
_vrf_PLAT779_borpbaxx            
;
PROBLEM: Suspect or Irrelevant (Bond) Angle in CIF .... # 11
RESPONSE: These are all concerned with angles between atoms belonging to
different disordered PARTs of the structure and are not real.
;


data_c:etbrc2c
_database_code_depnum_ccdc_archive 'CCDC 903497'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
bis(ethylenedithio)tetrathiafulvalene bromide
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H8 Br S8'
_chemical_formula_weight         464.55
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a                   12.867(3)
_cell_length_b                   11.036(2)
_cell_length_c                   11.270(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.66(3)
_cell_angle_gamma                90.00
_cell_volume                     1555.0(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    928
_cell_measurement_theta_min      2.4605
_cell_measurement_theta_max      23.254
_exptl_crystal_description       'cut rod'
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.984
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             924
_exptl_absorpt_coefficient_mu    3.698
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   'SADABS (Sheldrich, G. M. (1996))'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_standards_number         81
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_reflns_number            3375
_diffrn_reflns_av_R_equivalents  0.0168
_diffrn_reflns_av_sigmaI/netI    0.0181
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.46
_diffrn_reflns_theta_max         23.28
_reflns_number_total             1131
_reflns_number_gt                1099
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+2.9735P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1131
_refine_ls_number_parameters     87
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0282
_refine_ls_wR_factor_ref         0.0705
_refine_ls_wR_factor_gt          0.0702
_refine_ls_goodness_of_fit_ref   1.256
_refine_ls_restrained_S_all      1.256
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.5000 0.09284(5) 0.7500 0.0488(2) Uani 1 2 d S . .
S4 S 0.42429(6) 0.36317(7) 0.86997(7) 0.0313(2) Uani 1 1 d . . .
S3 S 0.41618(7) 0.62738(7) 0.86403(7) 0.0341(2) Uani 1 1 d . . .
S2 S 0.27834(7) 0.33380(7) 0.62438(7) 0.0351(2) Uani 1 1 d . . .
S1 S 0.27747(8) 0.64766(8) 0.61912(7) 0.0397(3) Uani 1 1 d . . .
C2 C 0.1633(3) 0.4296(3) 0.5658(3) 0.0393(8) Uani 1 1 d . . .
H2B H 0.1118 0.3846 0.5017 0.047 Uiso 1 1 calc R . .
H2A H 0.1277 0.4471 0.6327 0.047 Uiso 1 1 calc R . .
C4 C 0.3460(2) 0.4295(3) 0.7395(3) 0.0259(7) Uani 1 1 d . . .
C1 C 0.1897(3) 0.5474(3) 0.5131(3) 0.0460(9) Uani 1 1 d . . .
H1A H 0.1221 0.5909 0.4787 0.055 Uiso 1 1 calc R . .
H1B H 0.2236 0.5293 0.4448 0.055 Uiso 1 1 calc R . .
C5 C 0.4662(2) 0.4976(3) 0.9421(3) 0.0282(7) Uani 1 1 d . . .
C3 C 0.3422(2) 0.5521(3) 0.7360(3) 0.0281(7) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br1 0.0570(4) 0.0544(4) 0.0327(3) 0.000 0.0058(2) 0.000
S4 0.0350(5) 0.0226(4) 0.0304(5) -0.0043(3) -0.0041(4) -0.0001(3)
S3 0.0381(5) 0.0232(4) 0.0331(5) -0.0050(3) -0.0076(4) 0.0039(3)
S2 0.0412(5) 0.0318(4) 0.0267(4) -0.0077(3) -0.0030(4) -0.0029(4)
S1 0.0517(6) 0.0321(5) 0.0283(5) 0.0042(3) -0.0044(4) -0.0019(4)
C2 0.0308(18) 0.0415(19) 0.040(2) -0.0029(15) -0.0022(15) -0.0034(15)
C4 0.0267(16) 0.0302(16) 0.0192(15) -0.0036(12) 0.0022(13) -0.0025(13)
C1 0.049(2) 0.042(2) 0.037(2) 0.0012(17) -0.0095(17) -0.0051(18)
C5 0.0274(16) 0.0217(16) 0.0310(16) -0.0043(12) -0.0020(13) 0.0025(12)
C3 0.0277(16) 0.0292(16) 0.0253(16) -0.0022(13) 0.0023(13) -0.0013(14)
_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
S4 C5 1.716(3) . ?
S4 C4 1.736(3) . ?
S3 C5 1.724(3) . ?
S3 C3 1.741(3) . ?
S2 C4 1.738(3) . ?
S2 C2 1.812(3) . ?
S1 C3 1.738(3) . ?
S1 C1 1.814(4) . ?
C2 C1 1.500(5) . ?
C4 C3 1.355(5) . ?
C5 C5 1.388(6) 5_667 ?
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
C5 S4 C4 95.23(14) . . ?
C5 S3 C3 95.26(15) . . ?
C4 S2 C2 98.04(15) . . ?
C3 S1 C1 103.95(17) . . ?
C1 C2 S2 114.1(3) . . ?
C3 C4 S4 117.1(2) . . ?
C3 C4 S2 125.2(2) . . ?
S4 C4 S2 117.68(18) . . ?
C2 C1 S1 115.6(2) . . ?
C5 C5 S4 122.3(3) 5_667 . ?
C5 C5 S3 121.6(3) 5_667 . ?
S4 C5 S3 116.04(18) . . ?
C4 C3 S1 129.5(2) . . ?
C4 C3 S3 116.3(2) . . ?
S1 C3 S3 114.13(18) . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        23.28
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.118
_vrf_THETM01_c:etbrc2c           
;
PROBLEM:The value of sine(theta_max)/wavelength is less than 0.575
Calculated sin(theta_max)/wavelength = 0.5561
RESPONSE: weakly diffracting small crystal, sin(theta_max)wavelength
is 0.019 less than 0.575.
;


data_etbrbig
_database_code_depnum_ccdc_archive 'CCDC 903498'
#TrackingRef '14303_web_deposit_cif_file_0_PROFJOHNWALLIS_1348751138.WALLIS_DALTON_ALLCIFS.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
Penta-bis(ethylenedithio)tetrathiafulvalene tetrabromide
hydroxonium hydrate
;
_chemical_name_common            ?
_chemical_melting_point          482
_chemical_formula_moiety         '5(C10 H8 S8), 4(Br), (H2 O), (H3 O)'
_chemical_formula_sum            'C50 H45 Br4 O2 S40'
_chemical_formula_weight         2280.11
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   11.1312(2)
_cell_length_b                   18.0651(4)
_cell_length_c                   20.7862(4)
_cell_angle_alpha                75.8770(10)
_cell_angle_beta                 89.9950(10)
_cell_angle_gamma                72.0850(10)
_cell_volume                     3844.19(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    102788
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48
_exptl_crystal_description       'cut slab'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.970
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2282
_exptl_absorpt_coefficient_mu    3.223
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6794
_exptl_absorpt_correction_T_max  0.7826
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_measurement_device_type  
'Bruker-Nonius APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            62725
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         27.48
_reflns_number_total             17619
_reflns_number_gt                15225
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Mercury
_computing_publication_material  ?
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. ;
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+16.7542P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         17616
_refine_ls_number_parameters     911
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0495
_refine_ls_wR_factor_ref         0.1172
_refine_ls_wR_factor_gt          0.1123
_refine_ls_goodness_of_fit_ref   1.345
_refine_ls_restrained_S_all      1.344
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.47250(11) -0.18873(7) 0.07103(6) 0.0175(2) Uani 1 1 d . . .
S2 S 0.76344(11) -0.20411(7) 0.15037(6) 0.0177(2) Uani 1 1 d . . .
S3 S 0.40135(11) -0.01929(7) 0.07462(6) 0.0174(2) Uani 1 1 d . . .
S4 S 0.64331(11) -0.03129(7) 0.13916(6) 0.0170(2) Uani 1 1 d . . .
S5 S 0.29714(10) 0.16871(6) 0.06398(6) 0.0154(2) Uani 1 1 d . . .
S6 S 0.53885(10) 0.16340(6) 0.12354(6) 0.0157(2) Uani 1 1 d . . .
S7 S 0.18215(11) 0.34465(7) 0.03406(6) 0.0181(2) Uani 1 1 d . . .
S8 S 0.47568(10) 0.33923(6) 0.10147(6) 0.0161(2) Uani 1 1 d . . .
C1 C 0.5875(4) -0.2777(3) 0.1232(2) 0.0167(9) Uani 1 1 d . . .
H1A H 0.5686 -0.2817 0.1702 0.020 Uiso 1 1 calc R . .
H1B H 0.5786 -0.3258 0.1115 0.020 Uiso 1 1 calc R . .
C2 C 0.7236(4) -0.2779(3) 0.1165(2) 0.0180(9) Uani 1 1 d . . .
H2A H 0.7393 -0.2678 0.0687 0.022 Uiso 1 1 calc R . .
H2B H 0.7810 -0.3321 0.1393 0.022 Uiso 1 1 calc R . .
C3 C 0.5185(4) -0.1135(3) 0.0933(2) 0.0163(9) Uani 1 1 d . . .
C4 C 0.6300(4) -0.1194(3) 0.1229(2) 0.0143(9) Uani 1 1 d . . .
C5 C 0.4939(4) 0.0299(3) 0.1030(2) 0.0153(9) Uani 1 1 d . . .
C6 C 0.4486(4) 0.1109(3) 0.0980(2) 0.0162(9) Uani 1 1 d . . .
C7 C 0.3130(4) 0.2606(3) 0.0672(2) 0.0141(9) Uani 1 1 d . . .
C8 C 0.4262(4) 0.2585(3) 0.0938(2) 0.0131(8) Uani 1 1 d . . .
C9 C 0.2577(4) 0.4216(3) 0.0142(2) 0.0191(10) Uani 1 1 d . . .
H9A H 0.3151 0.4116 -0.0213 0.023 Uiso 1 1 calc R . .
H9B H 0.1922 0.4746 -0.0032 0.023 Uiso 1 1 calc R . .
C10 C 0.3323(4) 0.4243(3) 0.0736(3) 0.0194(10) Uani 1 1 d . . .
H10A H 0.2772 0.4270 0.1109 0.023 Uiso 1 1 calc R . .
H10B H 0.3557 0.4743 0.0624 0.023 Uiso 1 1 calc R . .
S11 S 0.02661(11) 0.65548(7) 0.46617(6) 0.0181(2) Uani 1 1 d . . .
S12 S 0.31484(10) 0.66080(7) 0.39859(6) 0.0164(2) Uani 1 1 d . . .
S13 S -0.03410(10) 0.83137(6) 0.43620(6) 0.0156(2) Uani 1 1 d . . .
S14 S 0.20194(10) 0.83664(6) 0.37650(6) 0.0157(2) Uani 1 1 d . . .
S15 S -0.11796(11) 1.01943(7) 0.42540(6) 0.0170(2) Uani 1 1 d . . .
S16 S 0.11156(11) 1.03133(7) 0.36057(6) 0.0172(2) Uani 1 1 d . . .
S17 S -0.21658(11) 1.18886(7) 0.42870(6) 0.0178(2) Uani 1 1 d . . .
S18 S 0.05899(11) 1.20412(7) 0.34912(6) 0.0179(2) Uani 1 1 d . . .
C11 C 0.1793(4) 0.5784(3) 0.4858(2) 0.0195(10) Uani 1 1 d . . .
H11A H 0.2270 0.5885 0.5212 0.023 Uiso 1 1 calc R . .
H11B H 0.1670 0.5254 0.5032 0.023 Uiso 1 1 calc R . .
C12 C 0.2561(4) 0.5762(3) 0.4260(3) 0.0197(10) Uani 1 1 d . . .
H12B H 0.2030 0.5741 0.3887 0.024 Uiso 1 1 calc R . .
H12A H 0.3292 0.5260 0.4368 0.024 Uiso 1 1 calc R . .
C13 C 0.0735(4) 0.7393(2) 0.4326(2) 0.0128(8) Uani 1 1 d . . .
C14 C 0.1847(4) 0.7416(3) 0.4060(2) 0.0132(8) Uani 1 1 d . . .
C15 C 0.0591(4) 0.8891(3) 0.4016(2) 0.0153(9) Uani 1 1 d . . .
C16 C 0.0225(4) 0.9702(3) 0.3965(2) 0.0153(9) Uani 1 1 d . . .
C17 C -0.0955(4) 1.1135(3) 0.4065(2) 0.0150(9) Uani 1 1 d . . .
C18 C 0.0102(4) 1.1197(3) 0.3769(2) 0.0140(9) Uani 1 1 d . . .
C19 C -0.1901(4) 1.2775(3) 0.3768(2) 0.0166(9) Uani 1 1 d . . .
H19B H -0.2130 1.2816 0.3297 0.020 Uiso 1 1 calc R . .
H19A H -0.2471 1.3257 0.3884 0.020 Uiso 1 1 calc R . .
C20 C -0.0545(4) 1.2781(3) 0.3833(2) 0.0176(9) Uani 1 1 d . . .
H20B H -0.0285 1.2679 0.4311 0.021 Uiso 1 1 calc R . .
H20A H -0.0515 1.3323 0.3605 0.021 Uiso 1 1 calc R . .
S21 S 1.47640(11) -0.22094(7) 0.27832(6) 0.0179(2) Uani 1 1 d . . .
S22 S 1.77721(10) -0.23635(7) 0.34568(6) 0.0166(2) Uani 1 1 d . . .
S23 S 1.41322(11) -0.04978(7) 0.27728(6) 0.0177(2) Uani 1 1 d . . .
S24 S 1.66057(11) -0.06478(7) 0.33825(6) 0.0186(2) Uani 1 1 d . . .
S25 S 1.32389(10) 0.14165(7) 0.25964(6) 0.0161(2) Uani 1 1 d . . .
S26 S 1.56400(11) 0.12665(7) 0.32848(6) 0.0167(2) Uani 1 1 d . . .
S27 S 1.22082(11) 0.31810(7) 0.23160(6) 0.0189(2) Uani 1 1 d . . .
S28 S 1.50622(11) 0.29973(7) 0.31833(6) 0.0176(2) Uani 1 1 d . . .
C21 C 1.5922(4) -0.3080(3) 0.3318(2) 0.0171(9) Uani 1 1 d . . .
H21A H 1.5788 -0.3072 0.3787 0.020 Uiso 1 1 calc R . .
H21B H 1.5783 -0.3572 0.3251 0.020 Uiso 1 1 calc R . .
C22 C 1.7287(4) -0.3123(3) 0.3196(2) 0.0172(9) Uani 1 1 d . . .
H22B H 1.7394 -0.3063 0.2715 0.021 Uiso 1 1 calc R . .
H22A H 1.7852 -0.3662 0.3438 0.021 Uiso 1 1 calc R . .
C23 C 1.5275(4) -0.1457(3) 0.2957(2) 0.0153(9) Uani 1 1 d . . .
C24 C 1.6420(4) -0.1517(2) 0.3222(2) 0.0140(9) Uani 1 1 d . . .
C25 C 1.5110(4) -0.0017(3) 0.3029(2) 0.0149(9) Uani 1 1 d . . .
C26 C 1.4716(4) 0.0790(3) 0.2974(2) 0.0150(9) Uani 1 1 d . . .
C27 C 1.3458(4) 0.2309(3) 0.2680(2) 0.0153(9) Uani 1 1 d . . .
C28 C 1.4562(4) 0.2242(2) 0.2998(2) 0.0142(9) Uani 1 1 d . . .
C29 C 1.2596(4) 0.3919(3) 0.2659(2) 0.0197(10) Uani 1 1 d . . .
H29B H 1.2056 0.4463 0.2413 0.024 Uiso 1 1 calc R . .
H29A H 1.2385 0.3837 0.3129 0.024 Uiso 1 1 calc R . .
C30 C 1.3964(5) 0.3890(3) 0.2634(2) 0.0191(10) Uani 1 1 d . . .
H30A H 1.4051 0.4370 0.2754 0.023 Uiso 1 1 calc R . .
H30B H 1.4201 0.3918 0.2172 0.023 Uiso 1 1 calc R . .
S31 S 1.03877(11) 0.68248(7) 0.26862(6) 0.0186(2) Uani 1 1 d . . .
S32 S 1.30583(11) 0.70063(7) 0.18199(6) 0.0180(2) Uani 1 1 d . . .
S33 S 0.96487(10) 0.85908(7) 0.24008(6) 0.0160(2) Uani 1 1 d . . .
S34 S 1.19044(11) 0.87383(7) 0.17116(6) 0.0164(2) Uani 1 1 d . . .
S35 S 0.86298(11) 1.05039(7) 0.22234(6) 0.0177(2) Uani 1 1 d . . .
S36 S 1.09537(11) 1.06544(7) 0.16116(6) 0.0187(2) Uani 1 1 d . . .
S37 S 0.75588(11) 1.22133(7) 0.22188(6) 0.0178(2) Uani 1 1 d . . .
S38 S 1.04092(10) 1.23676(7) 0.15446(6) 0.0161(2) Uani 1 1 d . . .
C31 C 1.1501(5) 0.6090(3) 0.2345(3) 0.0204(10) Uani 1 1 d . . .
H31A H 1.1500 0.5547 0.2592 0.024 Uiso 1 1 calc R . .
H31B H 1.1207 0.6172 0.1876 0.024 Uiso 1 1 calc R . .
C32 C 1.2852(4) 0.6112(3) 0.2369(2) 0.0175(9) Uani 1 1 d . . .
H32B H 1.3412 0.5632 0.2247 0.021 Uiso 1 1 calc R . .
H32A H 1.3122 0.6081 0.2831 0.021 Uiso 1 1 calc R . .
C33 C 1.0771(4) 0.7693(3) 0.2319(2) 0.0163(9) Uani 1 1 d . . .
C34 C 1.1803(4) 0.7760(2) 0.2004(2) 0.0135(8) Uani 1 1 d . . .
C35 C 1.0508(4) 0.9216(3) 0.2024(2) 0.0148(9) Uani 1 1 d . . .
C36 C 1.0090(4) 1.0023(3) 0.1969(2) 0.0145(9) Uani 1 1 d . . .
C37 C 0.8826(4) 1.1458(3) 0.2044(2) 0.0137(8) Uani 1 1 d . . .
C38 C 0.9903(4) 1.1521(3) 0.1777(2) 0.0141(9) Uani 1 1 d . . .
C39 C 0.7847(4) 1.3085(3) 0.1684(2) 0.0178(9) Uani 1 1 d . . .
H39B H 0.7717 1.3078 0.1214 0.021 Uiso 1 1 calc R . .
H39A H 0.7215 1.3576 0.1752 0.021 Uiso 1 1 calc R . .
C40 C 0.9166(4) 1.3133(3) 0.1801(2) 0.0164(9) Uani 1 1 d . . .
H40A H 0.9334 1.3079 0.2281 0.020 Uiso 1 1 calc R . .
H40B H 0.9191 1.3671 0.1554 0.020 Uiso 1 1 calc R . .
S41 S 0.01362(11) 0.71888(7) 0.06007(6) 0.0167(2) Uani 1 1 d . . .
S42 S 0.29086(11) 0.74121(7) -0.01240(6) 0.0173(2) Uani 1 1 d . . .
S43 S -0.06355(10) 0.89587(6) 0.03774(6) 0.0169(2) Uani 1 1 d . . .
S44 S 0.16676(11) 0.91297(7) -0.02437(6) 0.0178(2) Uani 1 1 d . . .
C41 C 0.1161(4) 0.6568(3) 0.0130(2) 0.0165(9) Uani 1 1 d . . .
H41A H 0.1071 0.6024 0.0259 0.020 Uiso 1 1 calc R . .
H41B H 0.0880 0.6799 -0.0349 0.020 Uiso 1 1 calc R . .
C42 C 0.2547(4) 0.6492(3) 0.0233(2) 0.0170(9) Uani 1 1 d . . .
H42B H 0.3061 0.6065 0.0033 0.020 Uiso 1 1 calc R . .
H42A H 0.2799 0.6322 0.0717 0.020 Uiso 1 1 calc R . .
C43 C 0.0521(4) 0.8069(3) 0.0315(2) 0.0145(9) Uani 1 1 d . . .
C44 C 0.1586(4) 0.8146(3) 0.0035(2) 0.0151(9) Uani 1 1 d . . .
C45 C 0.0217(4) 0.9594(3) 0.0029(2) 0.0150(9) Uani 1 1 d . . .
S51 S 1.23266(10) 0.28122(7) 0.43951(6) 0.0168(2) Uani 1 1 d . . .
S52 S 1.53193(10) 0.25868(7) 0.51246(6) 0.0176(2) Uani 1 1 d . . .
S53 S 1.33214(10) 0.10422(7) 0.46219(6) 0.0171(2) Uani 1 1 d . . .
S54 S 1.57980(11) 0.08685(7) 0.52469(6) 0.0178(2) Uani 1 1 d . . .
C51 C 1.2728(4) 0.3433(3) 0.4872(2) 0.0144(9) Uani 1 1 d . . .
H51A H 1.2095 0.3978 0.4744 0.017 Uiso 1 1 calc R . .
H51B H 1.2677 0.3200 0.5351 0.017 Uiso 1 1 calc R . .
C52 C 1.4039(4) 0.3508(3) 0.4770(2) 0.0171(9) Uani 1 1 d . . .
H52B H 1.4128 0.3934 0.4971 0.021 Uiso 1 1 calc R . .
H52A H 1.4121 0.3681 0.4287 0.021 Uiso 1 1 calc R . .
C53 C 1.3594(4) 0.1932(3) 0.4686(2) 0.0154(9) Uani 1 1 d . . .
C54 C 1.4737(4) 0.1853(3) 0.4966(2) 0.0152(9) Uani 1 1 d . . .
C55 C 1.4815(4) 0.0408(3) 0.4973(2) 0.0151(9) Uani 1 1 d . . .
Br1 Br 0.54214(5) 0.51876(3) 0.12395(3) 0.02222(11) Uani 1 1 d D . .
Br2 Br 1.00395(5) 0.50848(3) 0.12306(2) 0.02207(11) Uani 1 1 d D . .
Br3 Br 0.56091(4) 0.48136(3) 0.37623(3) 0.02216(11) Uani 1 1 d D . .
Br4 Br 1.01180(5) 0.49189(3) 0.37723(2) 0.02220(11) Uani 1 1 d D . .
O1 O 0.8516(7) 0.5399(4) 0.2419(4) 0.0248(15) Uani 0.50 1 d PD A 1
O2 O 0.8917(7) 0.4610(5) 0.2583(4) 0.0264(16) Uani 0.50 1 d PD B 2
O3 O 0.7147(7) 0.4562(5) 0.2555(4) 0.0282(16) Uani 0.50 1 d PD C 1
O4 O 0.6706(7) 0.5448(5) 0.2448(3) 0.0265(16) Uani 0.50 1 d PD D 2
H11 H 0.903(7) 0.539(5) 0.212(3) 0.032 Uiso 0.50 1 d PD E 1
H12 H 0.899(7) 0.527(7) 0.278(2) 0.032 Uiso 0.50 1 d PD F 1
H21 H 0.928(8) 0.475(7) 0.223(2) 0.032 Uiso 0.50 1 d PD G 2
H22 H 0.942(5) 0.458(4) 0.290(3) 0.032 Uiso 0.50 1 d PD H 2
H31 H 0.662(7) 0.480(5) 0.221(2) 0.032 Uiso 0.50 1 d PD I 1
H32 H 0.669(7) 0.455(5) 0.288(3) 0.032 Uiso 0.50 1 d PD J 1
H41 H 0.633(9) 0.542(6) 0.210(2) 0.032 Uiso 0.50 1 d PD K 2
H42 H 0.634(9) 0.524(7) 0.277(2) 0.032 Uiso 0.50 1 d PD L 2
H51 H 0.7796(8) 0.5004(7) 0.248(3) 0.032 Uiso 1 1 d D M 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.0167(5) 0.0130(5) 0.0251(6) -0.0067(5) -0.0014(4) -0.0063(4)
S2 0.0155(5) 0.0122(5) 0.0240(6) -0.0033(4) -0.0026(4) -0.0033(4)
S3 0.0138(5) 0.0117(5) 0.0269(6) -0.0060(4) -0.0023(4) -0.0034(4)
S4 0.0160(5) 0.0127(5) 0.0232(6) -0.0058(4) -0.0018(4) -0.0049(4)
S5 0.0128(5) 0.0114(5) 0.0227(6) -0.0047(4) 0.0005(4) -0.0044(4)
S6 0.0133(5) 0.0114(5) 0.0220(6) -0.0039(4) -0.0005(4) -0.0035(4)
S7 0.0135(5) 0.0117(5) 0.0286(6) -0.0050(5) -0.0029(5) -0.0033(4)
S8 0.0126(5) 0.0117(5) 0.0256(6) -0.0069(4) 0.0001(4) -0.0044(4)
C1 0.017(2) 0.014(2) 0.021(2) -0.0033(18) 0.0032(18) -0.0076(17)
C2 0.017(2) 0.016(2) 0.020(2) -0.0041(18) 0.0028(18) -0.0045(18)
C3 0.019(2) 0.009(2) 0.018(2) -0.0014(17) -0.0011(18) -0.0029(17)
C4 0.014(2) 0.0092(19) 0.019(2) -0.0017(17) 0.0001(17) -0.0026(16)
C5 0.014(2) 0.013(2) 0.019(2) -0.0043(17) 0.0006(17) -0.0033(17)
C6 0.017(2) 0.015(2) 0.018(2) -0.0066(18) 0.0041(18) -0.0060(17)
C7 0.016(2) 0.0097(19) 0.017(2) -0.0054(17) 0.0049(17) -0.0028(16)
C8 0.013(2) 0.014(2) 0.012(2) -0.0029(16) 0.0032(16) -0.0048(16)
C9 0.019(2) 0.015(2) 0.022(2) 0.0009(18) -0.0022(19) -0.0067(18)
C10 0.019(2) 0.011(2) 0.029(3) -0.0068(19) -0.0020(19) -0.0039(17)
S11 0.0139(5) 0.0111(5) 0.0297(6) -0.0051(5) 0.0068(5) -0.0047(4)
S12 0.0114(5) 0.0123(5) 0.0262(6) -0.0068(4) 0.0052(4) -0.0034(4)
S13 0.0124(5) 0.0121(5) 0.0221(6) -0.0047(4) 0.0033(4) -0.0033(4)
S14 0.0136(5) 0.0116(5) 0.0219(6) -0.0037(4) 0.0041(4) -0.0042(4)
S15 0.0148(5) 0.0114(5) 0.0257(6) -0.0057(4) 0.0065(4) -0.0045(4)
S16 0.0155(5) 0.0126(5) 0.0238(6) -0.0059(4) 0.0065(4) -0.0041(4)
S17 0.0149(5) 0.0125(5) 0.0256(6) -0.0066(5) 0.0061(5) -0.0022(4)
S18 0.0157(5) 0.0129(5) 0.0252(6) -0.0039(4) 0.0062(5) -0.0054(4)
C11 0.019(2) 0.015(2) 0.021(2) 0.0002(18) 0.0028(19) -0.0037(18)
C12 0.017(2) 0.013(2) 0.030(3) -0.0062(19) 0.0071(19) -0.0054(18)
C13 0.014(2) 0.0080(19) 0.016(2) -0.0029(16) -0.0001(17) -0.0041(16)
C14 0.014(2) 0.012(2) 0.015(2) -0.0052(17) 0.0011(17) -0.0047(16)
C15 0.015(2) 0.014(2) 0.016(2) -0.0040(17) 0.0005(17) -0.0046(17)
C16 0.013(2) 0.013(2) 0.019(2) -0.0032(17) 0.0021(17) -0.0042(17)
C17 0.015(2) 0.012(2) 0.018(2) -0.0027(17) 0.0010(17) -0.0045(17)
C18 0.015(2) 0.0093(19) 0.016(2) -0.0023(17) 0.0003(17) -0.0030(16)
C19 0.014(2) 0.012(2) 0.020(2) -0.0025(18) -0.0004(18) -0.0002(16)
C20 0.017(2) 0.016(2) 0.021(2) -0.0067(18) -0.0013(18) -0.0050(18)
S21 0.0171(6) 0.0143(5) 0.0243(6) -0.0069(5) -0.0013(5) -0.0061(4)
S22 0.0135(5) 0.0120(5) 0.0229(6) -0.0035(4) -0.0009(4) -0.0028(4)
S23 0.0129(5) 0.0130(5) 0.0264(6) -0.0065(5) -0.0016(4) -0.0017(4)
S24 0.0140(5) 0.0133(5) 0.0293(6) -0.0084(5) -0.0020(5) -0.0033(4)
S25 0.0135(5) 0.0127(5) 0.0219(6) -0.0053(4) -0.0005(4) -0.0031(4)
S26 0.0144(5) 0.0123(5) 0.0228(6) -0.0043(4) -0.0015(4) -0.0037(4)
S27 0.0141(5) 0.0117(5) 0.0285(6) -0.0024(5) -0.0047(5) -0.0026(4)
S28 0.0138(5) 0.0128(5) 0.0264(6) -0.0059(5) -0.0016(4) -0.0040(4)
C21 0.017(2) 0.013(2) 0.021(2) -0.0036(18) 0.0043(18) -0.0052(17)
C22 0.013(2) 0.016(2) 0.022(2) -0.0055(18) 0.0029(18) -0.0030(17)
C23 0.016(2) 0.012(2) 0.018(2) -0.0043(17) 0.0006(17) -0.0039(17)
C24 0.017(2) 0.0079(19) 0.019(2) -0.0056(17) 0.0042(17) -0.0043(16)
C25 0.013(2) 0.013(2) 0.019(2) -0.0051(17) 0.0003(17) -0.0042(16)
C26 0.016(2) 0.011(2) 0.017(2) -0.0028(17) 0.0010(17) -0.0021(16)
C27 0.016(2) 0.014(2) 0.015(2) -0.0018(17) 0.0012(17) -0.0064(17)
C28 0.015(2) 0.0082(19) 0.018(2) -0.0041(17) 0.0046(17) -0.0017(16)
C29 0.020(2) 0.015(2) 0.022(2) -0.0067(19) -0.0015(19) -0.0005(18)
C30 0.026(3) 0.014(2) 0.018(2) -0.0023(18) -0.0012(19) -0.0093(19)
S31 0.0154(5) 0.0118(5) 0.0273(6) -0.0022(5) 0.0059(5) -0.0048(4)
S32 0.0147(5) 0.0128(5) 0.0267(6) -0.0052(5) 0.0058(5) -0.0044(4)
S33 0.0152(5) 0.0123(5) 0.0220(6) -0.0056(4) 0.0042(4) -0.0057(4)
S34 0.0153(5) 0.0120(5) 0.0224(6) -0.0049(4) 0.0052(4) -0.0046(4)
S35 0.0167(5) 0.0134(5) 0.0252(6) -0.0061(4) 0.0062(5) -0.0071(4)
S36 0.0154(5) 0.0124(5) 0.0299(6) -0.0080(5) 0.0077(5) -0.0050(4)
S37 0.0155(5) 0.0143(5) 0.0235(6) -0.0059(5) 0.0059(4) -0.0035(4)
S38 0.0145(5) 0.0122(5) 0.0221(6) -0.0036(4) 0.0033(4) -0.0053(4)
C31 0.026(3) 0.016(2) 0.023(3) -0.0068(19) 0.005(2) -0.0099(19)
C32 0.018(2) 0.013(2) 0.019(2) -0.0039(18) 0.0048(18) 0.0001(17)
C33 0.016(2) 0.014(2) 0.019(2) -0.0019(18) -0.0003(18) -0.0063(17)
C34 0.013(2) 0.0083(19) 0.018(2) -0.0024(17) -0.0026(17) -0.0030(16)
C35 0.014(2) 0.016(2) 0.015(2) -0.0050(17) 0.0033(17) -0.0053(17)
C36 0.018(2) 0.010(2) 0.016(2) -0.0057(17) 0.0036(17) -0.0038(17)
C37 0.014(2) 0.012(2) 0.015(2) -0.0033(17) 0.0011(17) -0.0040(16)
C38 0.018(2) 0.0091(19) 0.015(2) -0.0031(16) 0.0023(17) -0.0049(16)
C39 0.017(2) 0.010(2) 0.022(2) -0.0006(18) -0.0020(18) -0.0003(17)
C40 0.013(2) 0.013(2) 0.025(2) -0.0082(18) 0.0008(18) -0.0052(17)
S41 0.0173(5) 0.0130(5) 0.0227(6) -0.0060(4) 0.0080(4) -0.0079(4)
S42 0.0137(5) 0.0140(5) 0.0280(6) -0.0097(5) 0.0070(4) -0.0062(4)
S43 0.0131(5) 0.0113(5) 0.0255(6) -0.0035(4) 0.0051(4) -0.0037(4)
S44 0.0151(5) 0.0123(5) 0.0255(6) -0.0031(4) 0.0059(4) -0.0050(4)
C41 0.015(2) 0.017(2) 0.021(2) -0.0081(18) 0.0056(18) -0.0078(18)
C42 0.016(2) 0.015(2) 0.021(2) -0.0049(18) 0.0032(18) -0.0050(17)
C43 0.013(2) 0.013(2) 0.019(2) -0.0074(17) 0.0029(17) -0.0045(16)
C44 0.016(2) 0.014(2) 0.018(2) -0.0046(17) 0.0025(17) -0.0072(17)
C45 0.012(2) 0.014(2) 0.019(2) -0.0038(18) 0.0017(17) -0.0048(17)
S51 0.0132(5) 0.0131(5) 0.0228(6) -0.0065(4) -0.0033(4) -0.0007(4)
S52 0.0121(5) 0.0147(5) 0.0275(6) -0.0098(5) -0.0004(4) -0.0033(4)
S53 0.0127(5) 0.0113(5) 0.0263(6) -0.0037(4) -0.0025(4) -0.0032(4)
S54 0.0140(5) 0.0119(5) 0.0262(6) -0.0031(4) -0.0035(4) -0.0034(4)
C51 0.013(2) 0.012(2) 0.017(2) -0.0054(17) 0.0010(17) -0.0022(16)
C52 0.019(2) 0.016(2) 0.016(2) -0.0027(18) -0.0010(18) -0.0062(18)
C53 0.015(2) 0.014(2) 0.018(2) -0.0061(18) 0.0042(17) -0.0055(17)
C54 0.014(2) 0.015(2) 0.018(2) -0.0057(18) 0.0033(17) -0.0049(17)
C55 0.015(2) 0.014(2) 0.016(2) -0.0011(17) 0.0017(17) -0.0068(17)
Br1 0.0187(2) 0.0203(2) 0.0273(3) -0.00271(19) -0.00265(19) -0.00838(18)
Br2 0.0201(2) 0.0215(2) 0.0223(2) -0.00007(19) 0.00229(19) -0.00762(19)
Br3 0.0164(2) 0.0202(2) 0.0273(3) -0.00252(19) 0.00503(19) -0.00499(18)
Br4 0.0192(2) 0.0217(2) 0.0227(2) -0.00008(19) -0.00161(19) -0.00661(19)
O1 0.025(4) 0.030(4) 0.018(4) -0.005(3) 0.000(3) -0.006(3)
O2 0.029(4) 0.031(4) 0.023(4) -0.005(3) 0.001(3) -0.015(3)
O3 0.026(4) 0.033(4) 0.021(4) -0.004(3) 0.002(3) -0.005(3)
O4 0.029(4) 0.033(4) 0.018(4) -0.008(3) 0.002(3) -0.011(3)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C3 1.749(5) . ?
S1 C1 1.811(5) . ?
S2 C4 1.746(4) . ?
S2 C2 1.815(5) . ?
S3 C5 1.736(5) . ?
S3 C3 1.749(5) . ?
S4 C5 1.737(5) . ?
S4 C4 1.754(4) . ?
S5 C6 1.730(5) . ?
S5 C7 1.740(4) . ?
S6 C6 1.738(5) . ?
S6 C8 1.750(4) . ?
S7 C7 1.741(4) . ?
S7 C9 1.803(5) . ?
S8 C8 1.750(4) . ?
S8 C10 1.817(5) . ?
C1 C2 1.521(6) . ?
C3 C4 1.348(6) . ?
C5 C6 1.371(6) . ?
C7 C8 1.362(6) . ?
C9 C10 1.507(6) . ?
S11 C13 1.739(4) . ?
S11 C11 1.806(5) . ?
S12 C14 1.750(4) . ?
S12 C12 1.811(5) . ?
S13 C15 1.726(5) . ?
S13 C13 1.744(4) . ?
S14 C15 1.736(5) . ?
S14 C14 1.746(4) . ?
S15 C16 1.733(5) . ?
S15 C17 1.744(4) . ?
S16 C16 1.741(4) . ?
S16 C18 1.759(4) . ?
S17 C17 1.749(5) . ?
S17 C19 1.807(5) . ?
S18 C18 1.742(4) . ?
S18 C20 1.820(5) . ?
C11 C12 1.511(6) . ?
C13 C14 1.364(6) . ?
C15 C16 1.372(6) . ?
C17 C18 1.350(6) . ?
C19 C20 1.519(6) . ?
S21 C23 1.737(4) . ?
S21 C21 1.808(5) . ?
S22 C24 1.750(4) . ?
S22 C22 1.813(5) . ?
S23 C25 1.741(4) . ?
S23 C23 1.757(5) . ?
S24 C25 1.742(5) . ?
S24 C24 1.753(4) . ?
S25 C26 1.739(5) . ?
S25 C27 1.752(5) . ?
S26 C26 1.741(5) . ?
S26 C28 1.757(4) . ?
S27 C27 1.749(5) . ?
S27 C29 1.815(5) . ?
S28 C28 1.744(4) . ?
S28 C30 1.813(5) . ?
C21 C22 1.521(6) . ?
C23 C24 1.351(6) . ?
C25 C26 1.362(6) . ?
C27 C28 1.353(6) . ?
C29 C30 1.509(7) . ?
S31 C33 1.746(4) . ?
S31 C31 1.802(5) . ?
S32 C34 1.743(4) . ?
S32 C32 1.814(5) . ?
S33 C35 1.742(5) . ?
S33 C33 1.764(5) . ?
S34 C35 1.741(5) . ?
S34 C34 1.762(4) . ?
S35 C36 1.741(5) . ?
S35 C37 1.753(4) . ?
S36 C36 1.743(4) . ?
S36 C38 1.753(4) . ?
S37 C37 1.744(5) . ?
S37 C39 1.810(5) . ?
S38 C38 1.749(4) . ?
S38 C40 1.815(5) . ?
C31 C32 1.518(6) . ?
C33 C34 1.346(6) . ?
C35 C36 1.363(6) . ?
C37 C38 1.346(6) . ?
C39 C40 1.520(6) . ?
S41 C43 1.738(4) . ?
S41 C41 1.806(5) . ?
S42 C44 1.746(5) . ?
S42 C42 1.812(5) . ?
S43 C45 1.733(4) . ?
S43 C43 1.757(4) . ?
S44 C45 1.741(5) . ?
S44 C44 1.761(4) . ?
C41 C42 1.517(6) . ?
C43 C44 1.351(6) . ?
C45 C45 1.371(9) 2_575 ?
S51 C53 1.743(5) . ?
S51 C51 1.815(4) . ?
S52 C54 1.741(4) . ?
S52 C52 1.812(5) . ?
S53 C55 1.741(5) . ?
S53 C53 1.759(4) . ?
S54 C55 1.733(4) . ?
S54 C54 1.760(5) . ?
C51 C52 1.517(6) . ?
C53 C54 1.351(6) . ?
C55 C55 1.379(9) 2_856 ?
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
C3 S1 C1 100.3(2) . . ?
C4 S2 C2 102.0(2) . . ?
C5 S3 C3 95.3(2) . . ?
C5 S4 C4 95.5(2) . . ?
C6 S5 C7 96.0(2) . . ?
C6 S6 C8 95.4(2) . . ?
C7 S7 C9 100.2(2) . . ?
C8 S8 C10 102.1(2) . . ?
C2 C1 S1 113.5(3) . . ?
C1 C2 S2 114.4(3) . . ?
C4 C3 S1 128.6(3) . . ?
C4 C3 S3 117.3(3) . . ?
S1 C3 S3 114.2(3) . . ?
C3 C4 S2 129.0(3) . . ?
C3 C4 S4 116.5(3) . . ?
S2 C4 S4 114.5(2) . . ?
C6 C5 S3 121.2(4) . . ?
C6 C5 S4 123.5(4) . . ?
S3 C5 S4 115.2(2) . . ?
C5 C6 S5 121.8(4) . . ?
C5 C6 S6 123.0(4) . . ?
S5 C6 S6 115.1(3) . . ?
C8 C7 S5 116.6(3) . . ?
C8 C7 S7 127.9(3) . . ?
S5 C7 S7 115.4(3) . . ?
C7 C8 S8 128.4(3) . . ?
C7 C8 S6 116.6(3) . . ?
S8 C8 S6 115.0(2) . . ?
C10 C9 S7 112.5(3) . . ?
C9 C10 S8 114.6(3) . . ?
C13 S11 C11 100.1(2) . . ?
C14 S12 C12 102.1(2) . . ?
C15 S13 C13 95.9(2) . . ?
C15 S14 C14 95.5(2) . . ?
C16 S15 C17 95.7(2) . . ?
C16 S16 C18 95.5(2) . . ?
C17 S17 C19 100.3(2) . . ?
C18 S18 C20 101.8(2) . . ?
C12 C11 S11 112.3(3) . . ?
C11 C12 S12 114.6(3) . . ?
C14 C13 S11 128.2(3) . . ?
C14 C13 S13 116.5(3) . . ?
S11 C13 S13 115.3(2) . . ?
C13 C14 S14 116.6(3) . . ?
C13 C14 S12 128.2(3) . . ?
S14 C14 S12 115.2(2) . . ?
C16 C15 S13 121.5(4) . . ?
C16 C15 S14 123.2(4) . . ?
S13 C15 S14 115.3(3) . . ?
C15 C16 S15 121.7(3) . . ?
C15 C16 S16 123.2(4) . . ?
S15 C16 S16 115.0(2) . . ?
C18 C17 S15 117.4(3) . . ?
C18 C17 S17 128.3(3) . . ?
S15 C17 S17 114.4(2) . . ?
C17 C18 S18 129.3(3) . . ?
C17 C18 S16 116.3(3) . . ?
S18 C18 S16 114.4(2) . . ?
C20 C19 S17 113.8(3) . . ?
C19 C20 S18 114.2(3) . . ?
C23 S21 C21 99.3(2) . . ?
C24 S22 C22 102.4(2) . . ?
C25 S23 C23 95.6(2) . . ?
C25 S24 C24 95.3(2) . . ?
C26 S25 C27 95.6(2) . . ?
C26 S26 C28 95.5(2) . . ?
C27 S27 C29 101.4(2) . . ?
C28 S28 C30 101.2(2) . . ?
C22 C21 S21 113.8(3) . . ?
C21 C22 S22 113.7(3) . . ?
C24 C23 S21 128.6(3) . . ?
C24 C23 S23 116.4(3) . . ?
S21 C23 S23 115.0(3) . . ?
C23 C24 S22 128.9(3) . . ?
C23 C24 S24 117.4(3) . . ?
S22 C24 S24 113.7(2) . . ?
C26 C25 S23 122.2(4) . . ?
C26 C25 S24 122.7(3) . . ?
S23 C25 S24 115.1(2) . . ?
C25 C26 S25 122.1(4) . . ?
C25 C26 S26 122.7(4) . . ?
S25 C26 S26 115.2(2) . . ?
C28 C27 S27 128.6(3) . . ?
C28 C27 S25 117.0(3) . . ?
S27 C27 S25 114.4(3) . . ?
C27 C28 S28 128.7(3) . . ?
C27 C28 S26 116.7(3) . . ?
S28 C28 S26 114.5(3) . . ?
C30 C29 S27 114.6(3) . . ?
C29 C30 S28 114.1(3) . . ?
C33 S31 C31 101.2(2) . . ?
C34 S32 C32 101.2(2) . . ?
C35 S33 C33 95.3(2) . . ?
C35 S34 C34 95.5(2) . . ?
C36 S35 C37 95.4(2) . . ?
C36 S36 C38 95.1(2) . . ?
C37 S37 C39 99.4(2) . . ?
C38 S38 C40 102.8(2) . . ?
C32 C31 S31 114.9(3) . . ?
C31 C32 S32 113.9(3) . . ?
C34 C33 S31 129.0(4) . . ?
C34 C33 S33 117.0(3) . . ?
S31 C33 S33 114.0(3) . . ?
C33 C34 S32 128.7(3) . . ?
C33 C34 S34 116.9(3) . . ?
S32 C34 S34 114.4(2) . . ?
C36 C35 S34 123.0(3) . . ?
C36 C35 S33 121.7(3) . . ?
S34 C35 S33 115.2(3) . . ?
C35 C36 S35 122.4(3) . . ?
C35 C36 S36 122.4(3) . . ?
S35 C36 S36 115.1(2) . . ?
C38 C37 S37 128.4(3) . . ?
C38 C37 S35 116.8(3) . . ?
S37 C37 S35 114.8(2) . . ?
C37 C38 S38 129.0(3) . . ?
C37 C38 S36 117.2(3) . . ?
S38 C38 S36 113.7(2) . . ?
C40 C39 S37 114.2(3) . . ?
C39 C40 S38 113.5(3) . . ?
C43 S41 C41 99.5(2) . . ?
C44 S42 C42 102.2(2) . . ?
C45 S43 C43 95.6(2) . . ?
C45 S44 C44 95.3(2) . . ?
C42 C41 S41 113.6(3) . . ?
C41 C42 S42 114.0(3) . . ?
C44 C43 S41 127.4(3) . . ?
C44 C43 S43 116.8(3) . . ?
S41 C43 S43 115.8(2) . . ?
C43 C44 S42 129.8(3) . . ?
C43 C44 S44 116.8(3) . . ?
S42 C44 S44 113.4(2) . . ?
C45 C45 S43 122.6(5) 2_575 . ?
C45 C45 S44 122.0(5) 2_575 . ?
S43 C45 S44 115.4(2) . . ?
C53 S51 C51 99.2(2) . . ?
C54 S52 C52 102.6(2) . . ?
C55 S53 C53 95.2(2) . . ?
C55 S54 C54 95.3(2) . . ?
C52 C51 S51 113.3(3) . . ?
C51 C52 S52 114.1(3) . . ?
C54 C53 S51 127.8(3) . . ?
C54 C53 S53 116.9(3) . . ?
S51 C53 S53 115.4(3) . . ?
C53 C54 S52 129.5(4) . . ?
C53 C54 S54 116.9(3) . . ?
S52 C54 S54 113.6(2) . . ?
C55 C55 S54 122.5(5) 2_856 . ?
C55 C55 S53 121.7(5) 2_856 . ?
S54 C55 S53 115.7(2) . . ?
_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        27.60
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.112
_vrf_PLAT411_etbrbig             
;
PROBLEM: Short Inter H...H Contact H29B .. H31A .. 1.99 Ang.
RESPONSE: Both H atoms are placed geometrically on different ethylene bridges.
There is sometimes a degree of disorder in such bridges so this may reflect
a contact between two averaged coordinates.
;
_vrf_PLAT303_etbrbig             
;
PROBLEM: Full Occupancy H-Atom H51 with # Connections 2.00
RESPONSE: The H5O2+ cation involves a H+ (H51) bonded to two waters.
This is likely to involve two unequal H---OH2 bonds, which are averaged
in the structural model.
;