# Supplementary Material (ESI) for ChemComm
# This journal is © The Royal Society of Chemistry 1999
# CCDC Number: 182/1459

data_1

_audit_creation_method            SHELXL-97
_publ_contact_author_name             ' Colin L. Raston'
_publ_contact_author_email            ' c.raston@sci.monash.edu.au '
_publ_contact_author_fax              ' 61 - 3 - 9905 4597 '
loop_
_publ_author_name
_publ_author_address

' Michaele J. Hardie '
;
  Department of Chemistry
  Monash University
  Clayton 3168
  Victoria
  AUSTRALIA
;
' Mohamed Makha '
;
  Department of Chemistry
  Monash University
  Clayton 3168
  Victoria
  AUSTRALIA
;
' Colin L. Raston'
;
  Department of Chemistry
  Monash University
  Clayton 3168
  Victoria
  AUSTRALIA
;
_publ_requested_journal               ' Chemical Communications'

_chemical_name_systematic
;
 calix[5]arene-penta-(p-sulfonic acid) tetra-(sulfuric acid) hydrate
;
_chemical_name_common             (calix[5]arene-p-sulfonicacid)(H2SO4)4(H2O)1.5
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C35 H49 O37.50 S9'
_chemical_formula_weight          1358.28

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'

_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                    11.7770(3)
_cell_length_b                    15.9118(4)
_cell_length_c                    16.0580(4)
_cell_angle_alpha                 105.459(1)
_cell_angle_beta                  90.871(1)
_cell_angle_gamma                 105.767(1)
_cell_volume                      2778.68(12)
_cell_formula_units_Z             2
_cell_measurement_temperature     123(1)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?

_exptl_crystal_description        prism
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.25 
_exptl_crystal_size_mid           0.20 
_exptl_crystal_size_min           0.15 
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.623
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1406
_exptl_absorpt_coefficient_mu     0.464
_exptl_absorpt_correction_type    none
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?

_exptl_special_details
;
 Crystals were extremely hygroscopic and lost clarity (indicating
degradation)
 during mounting.
;

_diffrn_ambient_temperature       123(1)
_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
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             57663
_diffrn_reflns_av_R_equivalents   0.073
_diffrn_reflns_av_sigmaI/netI     0.0912
_diffrn_reflns_limit_h_min        -15
_diffrn_reflns_limit_h_max        15
_diffrn_reflns_limit_k_min        -20
_diffrn_reflns_limit_k_max        20
_diffrn_reflns_limit_l_min        -20
_diffrn_reflns_limit_l_max        20
_diffrn_reflns_theta_min          1.32
_diffrn_reflns_theta_max          27.50
_reflns_number_total              12660
_reflns_number_gt                 7156
_reflns_threshold_expression      2sigma(I)

_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_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. Two S-O bond lengths of
 disordered sulfuric acid groups were restrained at 1.45 A.
;

_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^)+(0.2000P)^2^+0.0000P] 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          12660
_refine_ls_number_parameters      846
_refine_ls_number_restraints      2
_refine_ls_R_factor_all           0.1995
_refine_ls_R_factor_gt            0.1267
_refine_ls_wR_factor_ref          0.4012
_refine_ls_wR_factor_gt           0.3569
_refine_ls_goodness_of_fit_ref    1.384
_refine_ls_restrained_S_all       1.384
_refine_ls_shift/su_max           0.004
_refine_ls_shift/su_mean          0.001

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
C1 C 0.6578(5) 0.8003(4) 0.2975(4) 0.0297(13) Uani 1 1 d . . .
C2 C 0.5449(5) 0.7615(4) 0.2547(4) 0.0303(14) Uani 1 1 d . . .
C3 C 0.4496(6) 0.7748(4) 0.3037(4) 0.0318(14) Uani 1 1 d . . .
H3 H 0.3720 0.7478 0.2787 0.038 Uiso 1 1 calc R . .
C4 C 0.4715(6) 0.8277(4) 0.3882(4) 0.0341(15) Uani 1 1 d . . .
C5 C 0.5855(5) 0.8740(4) 0.4256(4) 0.0315(14) Uani 1 1 d . . .
H5 H 0.5983 0.9128 0.4817 0.038 Uiso 1 1 calc R . .
C6 C 0.6805(5) 0.8621(4) 0.3789(4) 0.0278(13) Uani 1 1 d . . .
C7 C 0.8054(5) 0.9226(4) 0.4171(4) 0.0317(14) Uani 1 1 d . . .
H7A H 0.8573 0.9189 0.3707 0.038 Uiso 1 1 calc R . .
H7B H 0.8025 0.9850 0.4367 0.038 Uiso 1 1 calc R . .
C8 C 0.9107(5) 0.8289(4) 0.4764(4) 0.0328(14) Uani 1 1 d . . .
C9 C 0.8606(5) 0.9014(4) 0.4906(4) 0.0295(14) Uani 1 1 d . . .
C10 C 0.8659(6) 0.9546(4) 0.5755(4) 0.0365(15) Uani 1 1 d . . .
H10 H 0.8324 1.0026 0.5876 0.044 Uiso 1 1 calc R . .
C11 C 0.9216(6) 0.9357(5) 0.6419(4) 0.0394(16) Uani 1 1 d . . .
C12 C 0.9756(6) 0.8675(4) 0.6260(4) 0.0355(15) Uani 1 1 d . . .
H12 H 1.0167 0.8585 0.6713 0.043 Uiso 1 1 calc R . .
C13 C 0.9685(5) 0.8112(4) 0.5413(5) 0.0364(15) Uani 1 1 d . . .
C14 C 1.0275(5) 0.7347(4) 0.5230(5) 0.0355(15) Uani 1 1 d . . .
H14A H 1.0592 0.7294 0.4671 0.043 Uiso 1 1 calc R . .
H14B H 1.0934 0.7506 0.5667 0.043 Uiso 1 1 calc R . .
C15 C 0.9042(5) 0.5737(4) 0.4457(4) 0.0299(14) Uani 1 1 d . . .
C16 C 0.9440(5) 0.6433(4) 0.5227(4) 0.0304(14) Uani 1 1 d . . .
C17 C 0.9109(5) 0.6266(5) 0.6002(5) 0.0339(15) Uani 1 1 d . . .
H17 H 0.9339 0.6729 0.6519 0.041 Uiso 1 1 calc R . .
C18 C 0.8416(5) 0.5388(5) 0.6004(4) 0.0347(15) Uani 1 1 d . . .
C19 C 0.8119(5) 0.4679(5) 0.5238(4) 0.0344(15) Uani 1 1 d . . .
H19 H 0.7707 0.4094 0.5248 0.041 Uiso 1 1 calc R . .
C20 C 0.8443(5) 0.4852(4) 0.4456(4) 0.0298(14) Uani 1 1 d . . .
C21 C 0.8220(5) 0.4066(5) 0.3642(4) 0.0337(15) Uani 1 1 d . . .
H21A H 0.8331 0.3544 0.3799 0.040 Uiso 1 1 calc R . .
H21B H 0.8817 0.4225 0.3257 0.040 Uiso 1 1 calc R . .
C22 C 0.6826(6) 0.4089(4) 0.2421(4) 0.0326(14) Uani 1 1 d . . .
C23 C 0.7006(5) 0.3780(4) 0.3139(4) 0.0257(13) Uani 1 1 d . . .
C24 C 0.6060(6) 0.3165(4) 0.3335(4) 0.0337(15) Uani 1 1 d . . .
H24 H 0.6149 0.2941 0.3804 0.040 Uiso 1 1 calc R . .
C25 C 0.4991(6) 0.2876(4) 0.2853(4) 0.0356(15) Uani 1 1 d . . .
C26 C 0.4876(6) 0.3125(5) 0.2095(4) 0.0369(15) Uani 1 1 d . . .
H26 H 0.4170 0.2871 0.1736 0.044 Uiso 1 1 calc R . .
C27 C 0.5801(5) 0.3744(4) 0.1873(4) 0.0303(14) Uani 1 1 d . . .
C28 C 0.5690(6) 0.3963(5) 0.1019(4) 0.0351(15) Uani 1 1 d . . .
H28A H 0.5360 0.3398 0.0566 0.042 Uiso 1 1 calc R . .
H28B H 0.6477 0.4244 0.0881 0.042 Uiso 1 1 calc R . .
C29 C 0.5387(5) 0.5525(5) 0.1337(4) 0.0318(14) Uani 1 1 d . . .
C30 C 0.4921(6) 0.4593(4) 0.1009(4) 0.0316(14) Uani 1 1 d . . .
C31 C 0.3766(6) 0.4236(5) 0.0668(4) 0.0374(15) Uani 1 1 d . . .
H31 H 0.3440 0.3609 0.0454 0.045 Uiso 1 1 calc R . .
C32 C 0.3061(6) 0.4838(5) 0.0645(4) 0.0374(15) Uani 1 1 d . . .
C33 C 0.3536(6) 0.5766(5) 0.0959(4) 0.0359(15) Uani 1 1 d . . .
H33 H 0.3071 0.6149 0.0939 0.043 Uiso 1 1 calc R . .
C34 C 0.4708(6) 0.6129(4) 0.1306(4) 0.0308(14) Uani 1 1 d . . .
C35 C 0.5248(6) 0.7148(4) 0.1572(4) 0.0354(15) Uani 1 1 d . . .
S1 S 0.35322(15) 0.83657(12) 0.45208(13) 0.0416(5) Uani 1 1 d . . .
S2 S 0.93275(19) 1.00640(14) 0.74752(12) 0.0541(6) Uani 1 1 d . . .
S3 S 0.80023(18) 0.51925(15) 0.69761(13) 0.0525(6) Uani 1 1 d . . .
S4 S 0.37785(18) 0.21147(17) 0.31161(14) 0.0592(6) Uani 1 1 d . . .
S5 S 0.16097(17) 0.43741(15) 0.01549(14) 0.0561(6) Uani 1 1 d . . .
O1 O 0.7496(4) 0.7769(3) 0.2524(3) 0.0339(10) Uani 1 1 d . . .
O2 O 0.9026(4) 0.7766(3) 0.3913(3) 0.0383(11) Uani 1 1 d . . .
O3 O 0.9294(4) 0.5953(3) 0.3699(3) 0.0380(11) Uani 1 1 d . . .
O4 O 0.7764(4) 0.4765(3) 0.2253(3) 0.0399(11) Uani 1 1 d . . .
O5 O 0.6560(4) 0.5860(3) 0.1633(3) 0.0383(11) Uani 1 1 d . . .
O6 O 0.2696(5) 0.8696(4) 0.4024(4) 0.0613(16) Uani 1 1 d . . .
O7 O 0.2934(5) 0.7504(4) 0.4623(4) 0.0621(16) Uani 1 1 d . . .
O8 O 0.3963(5) 0.9095(4) 0.5307(4) 0.0551(14) Uani 1 1 d . . .
O9 O 0.8441(10) 1.0530(6) 0.7507(5) 0.117(3) Uani 1 1 d . . .
O10 O 1.0525(8) 1.0593(6) 0.7732(4) 0.130(4) Uani 1 1 d . . .
O11 O 0.9075(6) 0.9450(4) 0.8061(4) 0.0667(17) Uani 1 1 d . . .
O12 O 0.7602(8) 0.6012(6) 0.7481(5) 0.106(3) Uani 1 1 d . . .
O13 O 0.9054(6) 0.5215(7) 0.7455(4) 0.100(3) Uani 1 1 d . . .
O14 O 0.7038(5) 0.4388(4) 0.6839(4) 0.0680(17) Uani 1 1 d . . .
O15 O 0.2987(6) 0.2656(7) 0.3550(6) 0.108(3) Uani 1 1 d . . .
O16 O 0.4174(6) 0.1748(7) 0.3743(6) 0.115(3) Uani 1 1 d . . .
O17 O 0.3181(7) 0.1463(6) 0.2346(5) 0.108(3) Uani 1 1 d . . .
O18 O 0.1424(6) 0.3444(5) -0.0295(7) 0.116(3) Uani 1 1 d . . .
O19 O 0.1451(6) 0.4898(5) -0.0422(4) 0.082(2) Uani 1 1 d . . .
O20 O 0.0799(5) 0.4517(7) 0.0837(4) 0.101(3) Uani 1 1 d . . .
S6 S 0.58143(16) 0.60069(13) 0.41903(13) 0.0450(5) Uani 1 1 d . . .
O21 O 0.6286(13) 0.6017(7) 0.3463(7) 0.164(5) Uani 1 1 d . . .
O22 O 0.6645(11) 0.6504(13) 0.4941(10) 0.253(11) Uani 1 1 d . . .
O23 O 0.5412(10) 0.5132(6) 0.4277(8) 0.157(5) Uani 1 1 d . . .
O24 O 0.4879(6) 0.6483(4) 0.4422(4) 0.0739(19) Uani 1 1 d . . .
S7 S 0.0709(2) 0.70424(16) 0.20164(16) 0.0616(6) Uani 1 1 d . . .
O25 O 0.106(2) 0.7619(11) 0.1479(9) 0.267(11) Uani 1 1 d . . .
O26 O -0.0462(10) 0.6967(17) 0.2026(7) 0.279(13) Uani 1 1 d . . .
O27 O 0.1239(7) 0.7386(7) 0.2863(6) 0.120(3) Uani 1 1 d . . .
O28 O 0.0985(13) 0.6329(13) 0.1481(10) 0.246(10) Uani 1 1 d . . .
S8 S 0.8276(4) 0.8677(3) 0.0096(2) 0.0497(10) Uani 0.50 1 d P A 1
O29 O 0.9548(14) 0.8927(16) 0.0167(10) 0.138(9) Uani 0.50 1 d P A 1
O30 O 0.7909(10) 0.8509(8) 0.0903(6) 0.063(3) Uani 0.50 1 d P A 1
O31 O 0.8076(19) 0.9518(9) -0.0051(10) 0.112(7) Uani 0.50 1 d P A 1
O32 O 0.7681(10) 0.7973(8) -0.0622(8) 0.060(3) Uiso 0.50 1 d P A 1
S9 S 0.6418(8) 0.0542(6) 0.2512(3) 0.086(3) Uani 0.50 1 d PD B 1
O33 O 0.683(2) 0.052(2) 0.287(3) 0.23(2) Uani 0.50 1 d P B 1
O34 O 0.6251(15) 0.1106(10) 0.2115(13) 0.107(6) Uani 0.50 1 d P B 1
O35 O 0.704(4) -0.0049(19) 0.203(2) 0.28(2) Uani 0.50 1 d P B 1
O36 O 0.5347(19) 0.016(2) 0.2808(17) 0.192(12) Uani 0.50 1 d PD B 1
S10 S 1.0913(9) 0.7692(7) -0.1474(5) 0.104(3) Uani 0.50 1 d P C 1
O37 O 1.154(2) 0.7831(16) -0.2158(18) 0.169(11) Uani 0.50 1 d P C 1
O38 O 0.9462(14) 0.7546(11) -0.1810(8) 0.098(5) Uani 0.50 1 d P C 1
O39 O 1.1106(12) 0.8803(9) -0.1024(10) 0.093(5) Uani 0.50 1 d P C 1
O40 O 1.118(2) 0.7223(19) -0.101(2) 0.182(13) Uani 0.50 1 d P C 1
O41 O 0.321(2) 0.7890(14) 0.0025(15) 0.129(7) Uani 0.50 1 d P . .
O42 O 0.346(3) 0.868(2) 0.159(2) 0.197(13) Uani 0.50 1 d P . .
O43 O 0.359(5) 0.9451(15) 0.047(2) 0.28(3) Uani 0.50 1 d P . .
S11 S 0.3654(19) 0.875(2) 0.054(2) 0.094(7) Uani 0.25 1 d PD D 1
O44 O 0.489(3) 0.877(2) 0.074(3) 0.138(18) Uani 0.25 1 d PD D 1
S11A S 0.330(2) 0.883(3) 0.0786(19) 0.101(9) Uani 0.25 1 d P D 2
O44A O 0.215(3) 0.885(3) 0.0680(19) 0.094(11) Uani 0.25 1 d P D 2
O100 O 0.7478(13) 0.8804(9) 0.0162(9) 0.067(3) Uiso 0.50 1 d P E 2
O101 O 1.0480(12) 0.8036(9) -0.1241(9) 0.049(3) Uani 0.50 1 d P F 2
O102 O 0.4279(17) 0.8731(10) 0.0114(12) 0.076(4) Uani 0.50 1 d P D 3

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
C1 0.027(3) 0.031(3) 0.032(3) 0.017(3) 0.002(3) 0.003(3)
C2 0.028(3) 0.032(3) 0.030(3) 0.014(3) -0.003(3) 0.001(3)
C3 0.028(3) 0.032(3) 0.036(4) 0.010(3) -0.006(3) 0.008(3)
C4 0.033(3) 0.036(3) 0.042(4) 0.020(3) 0.006(3) 0.014(3)
C5 0.034(3) 0.024(3) 0.034(4) 0.009(3) 0.003(3) 0.005(3)
C6 0.027(3) 0.026(3) 0.030(3) 0.010(3) -0.002(2) 0.006(3)
C7 0.025(3) 0.023(3) 0.039(4) 0.005(3) 0.001(3) -0.003(2)
C8 0.022(3) 0.038(4) 0.034(4) 0.016(3) 0.004(3) -0.005(3)
C9 0.020(3) 0.026(3) 0.037(4) 0.011(3) 0.000(3) -0.004(2)
C10 0.027(3) 0.032(3) 0.040(4) 0.008(3) 0.005(3) -0.007(3)
C11 0.029(3) 0.037(4) 0.035(4) 0.006(3) -0.004(3) -0.013(3)
C12 0.033(3) 0.038(4) 0.027(3) 0.013(3) -0.006(3) -0.005(3)
C13 0.025(3) 0.036(4) 0.043(4) 0.020(3) -0.002(3) -0.008(3)
C14 0.021(3) 0.042(4) 0.045(4) 0.022(3) 0.000(3) 0.002(3)
C15 0.020(3) 0.041(4) 0.032(3) 0.018(3) 0.002(2) 0.007(3)
C16 0.014(3) 0.034(3) 0.045(4) 0.018(3) -0.002(3) 0.003(2)
C17 0.020(3) 0.039(4) 0.044(4) 0.018(3) -0.001(3) 0.004(3)
C18 0.025(3) 0.042(4) 0.040(4) 0.022(3) 0.002(3) 0.006(3)
C19 0.023(3) 0.043(4) 0.041(4) 0.024(3) 0.004(3) 0.004(3)
C20 0.022(3) 0.040(4) 0.032(3) 0.018(3) 0.001(3) 0.009(3)
C21 0.026(3) 0.043(4) 0.038(4) 0.019(3) 0.006(3) 0.012(3)
C22 0.031(3) 0.035(3) 0.034(4) 0.007(3) 0.010(3) 0.014(3)
C23 0.026(3) 0.028(3) 0.025(3) 0.008(2) 0.002(2) 0.009(3)
C24 0.036(4) 0.036(4) 0.031(4) 0.015(3) 0.002(3) 0.008(3)
C25 0.035(4) 0.031(3) 0.034(4) 0.007(3) 0.002(3) 0.000(3)
C26 0.032(3) 0.043(4) 0.030(4) 0.006(3) -0.008(3) 0.007(3)
C27 0.032(3) 0.035(3) 0.023(3) 0.008(3) 0.007(3) 0.010(3)
C28 0.038(4) 0.041(4) 0.024(3) 0.005(3) 0.002(3) 0.012(3)
C29 0.031(3) 0.044(4) 0.017(3) 0.007(3) 0.003(2) 0.006(3)
C30 0.039(4) 0.039(4) 0.016(3) 0.011(3) 0.002(3) 0.007(3)
C31 0.039(4) 0.041(4) 0.025(3) 0.004(3) 0.003(3) 0.006(3)
C32 0.034(4) 0.050(4) 0.026(3) 0.010(3) 0.003(3) 0.008(3)
C33 0.037(4) 0.048(4) 0.024(3) 0.009(3) 0.002(3) 0.015(3)
C34 0.034(3) 0.041(4) 0.016(3) 0.012(3) -0.001(2) 0.007(3)
C35 0.043(4) 0.038(4) 0.023(3) 0.008(3) -0.006(3) 0.009(3)
S1 0.0330(9) 0.0413(10) 0.0566(12) 0.0183(9) 0.0135(8) 0.0156(8)
S2 0.0607(13) 0.0450(11) 0.0332(10) 0.0032(8) 0.0029(9) -0.0156(10)
S3 0.0522(12) 0.0652(13) 0.0367(11) 0.0238(9) 0.0080(9) 0.0017(10)
S4 0.0377(11) 0.0781(15) 0.0480(12) 0.0286(11) -0.0007(9) -0.0162(10)
S5 0.0337(10) 0.0627(13) 0.0552(13) -0.0014(10) -0.0066(9) 0.0046(9)
O1 0.028(2) 0.039(2) 0.034(2) 0.010(2) 0.0053(19) 0.008(2)
O2 0.037(3) 0.044(3) 0.032(3) 0.012(2) 0.007(2) 0.007(2)
O3 0.031(2) 0.051(3) 0.039(3) 0.027(2) 0.007(2) 0.007(2)
O4 0.035(2) 0.042(3) 0.039(3) 0.020(2) 0.002(2) -0.003(2)
O5 0.031(2) 0.047(3) 0.037(3) 0.017(2) -0.001(2) 0.007(2)
O6 0.056(3) 0.083(4) 0.069(4) 0.031(3) 0.013(3) 0.047(3)
O7 0.055(3) 0.049(3) 0.095(5) 0.032(3) 0.039(3) 0.023(3)
O8 0.050(3) 0.058(3) 0.051(3) 0.008(3) 0.014(3) 0.012(3)
O9 0.185(9) 0.129(7) 0.048(4) -0.013(4) -0.004(5) 0.099(7)
O10 0.116(6) 0.128(7) 0.045(4) -0.015(4) 0.011(4) -0.090(5)
O11 0.091(5) 0.064(4) 0.036(3) 0.013(3) 0.007(3) 0.010(3)
O12 0.145(7) 0.100(6) 0.087(5) 0.037(5) 0.077(5) 0.042(5)
O13 0.056(4) 0.190(9) 0.061(4) 0.074(5) -0.001(3) 0.009(5)
O14 0.067(4) 0.078(4) 0.052(4) 0.039(3) 0.001(3) -0.012(3)
O15 0.058(4) 0.149(8) 0.134(7) 0.060(6) 0.055(5) 0.036(5)
O16 0.056(4) 0.170(8) 0.133(7) 0.128(7) -0.012(4) -0.029(5)
O17 0.092(5) 0.108(6) 0.070(5) 0.028(4) -0.002(4) -0.059(5)
O18 0.051(4) 0.081(5) 0.180(9) -0.012(5) -0.043(5) 0.009(4)
O19 0.054(4) 0.117(6) 0.062(4) 0.027(4) -0.031(3) 0.006(4)
O20 0.039(3) 0.195(9) 0.063(4) 0.035(5) 0.008(3) 0.027(4)
S6 0.0414(10) 0.0494(11) 0.0579(12) 0.0294(9) 0.0196(9) 0.0206(9)
O21 0.272(14) 0.144(9) 0.146(9) 0.083(7) 0.153(10) 0.128(10)
O22 0.117(9) 0.36(2) 0.198(13) -0.121(14) -0.067(9) 0.137(13)
O23 0.212(11) 0.118(7) 0.245(12) 0.142(8) 0.174(10) 0.121(8)
O24 0.090(5) 0.077(4) 0.079(5) 0.036(4) 0.039(4) 0.049(4)
S7 0.0610(14) 0.0649(14) 0.0621(15) 0.0217(12) 0.0025(11) 0.0198(12)
O25 0.50(3) 0.180(14) 0.120(10) 0.078(10) 0.103(16) 0.058(18)
O26 0.097(8) 0.60(4) 0.085(7) -0.034(13) -0.029(6) 0.147(14)
O27 0.064(5) 0.167(9) 0.092(6) 0.005(6) -0.033(4) 0.007(5)
O28 0.184(13) 0.32(2) 0.217(15) -0.083(14) -0.033(11) 0.196(15)
S8 0.064(3) 0.039(2) 0.0300(19) 0.0031(15) -0.0164(18) -0.0032(19)
O29 0.059(9) 0.22(2) 0.067(10) 0.001(12) 0.000(8) -0.026(12)
O30 0.057(7) 0.068(7) 0.022(5) 0.009(5) -0.018(5) -0.045(6)
O31 0.21(2) 0.043(7) 0.071(10) 0.018(7) 0.051(11) 0.013(10)
S9 0.163(7) 0.123(5) 0.0094(19) 0.022(2) 0.020(3) 0.099(5)
O33 0.113(18) 0.14(2) 0.53(7) 0.19(4) 0.18(3) 0.080(17)
O34 0.108(13) 0.062(9) 0.168(17) 0.062(10) 0.038(12) 0.022(9)
O35 0.58(7) 0.19(2) 0.24(3) 0.12(2) 0.26(4) 0.30(4)
O36 0.27(4) 0.23(3) 0.12(2) 0.08(2) 0.00(2) 0.11(3)
S10 0.102(6) 0.086(5) 0.067(4) -0.026(4) 0.020(4) -0.022(4)
O37 0.147(19) 0.125(17) 0.16(2) -0.015(16) 0.034(17) -0.028(14)
O38 0.104(11) 0.105(11) 0.040(7) 0.017(7) -0.006(7) -0.043(9)
O39 0.073(9) 0.051(8) 0.095(11) -0.034(7) 0.003(8) -0.028(7)
O40 0.13(2) 0.12(2) 0.24(3) 0.01(2) -0.05(2) 0.000(16)
O41 0.138(17) 0.094(13) 0.164(19) 0.026(13) 0.049(15) 0.055(13)
O42 0.16(2) 0.24(3) 0.23(3) 0.13(3) -0.04(2) 0.06(2)
O43 0.54(8) 0.062(13) 0.20(3) -0.012(16) -0.16(4) 0.11(3)
S11 0.051(14) 0.112(14) 0.14(2) 0.061(16) -0.002(11) 0.036(13)
O44 0.22(5) 0.09(2) 0.13(3) 0.07(2) -0.06(3) 0.05(3)
S11A 0.049(11) 0.19(2) 0.103(15) 0.089(15) 0.006(8) 0.043(11)
O44A 0.072(18) 0.16(3) 0.08(2) 0.04(2) 0.023(16) 0.09(2)
O101 0.079(9) 0.039(7) 0.045(7) 0.031(6) 0.014(7) 0.022(7)
O102 0.083(11) 0.061(9) 0.108(13) 0.040(8) 0.003(10) 0.044(9)

_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
C1 C6 1.381(9) . ?
C1 O1 1.389(7) . ?
C1 C2 1.386(9) . ?
C2 C3 1.411(9) . ?
C2 C35 1.527(9) . ?
C3 C4 1.370(9) . ?
C4 C5 1.382(9) . ?
C4 S1 1.756(7) . ?
C5 C6 1.383(9) . ?
C6 C7 1.535(8) . ?
C7 C9 1.496(9) . ?
C8 C13 1.367(9) . ?
C8 O2 1.384(8) . ?
C8 C9 1.402(9) . ?
C9 C10 1.390(9) . ?
C10 C11 1.384(10) . ?
C11 C12 1.372(10) . ?
C11 S2 1.747(7) . ?
C12 C13 1.402(9) . ?
C13 C14 1.525(9) . ?
C14 C16 1.517(9) . ?
C15 O3 1.365(8) . ?
C15 C20 1.393(9) . ?
C15 C16 1.396(9) . ?
C16 C17 1.379(9) . ?
C17 C18 1.416(9) . ?
C18 C19 1.393(10) . ?
C18 S3 1.724(7) . ?
C19 C20 1.392(9) . ?
C20 C21 1.511(9) . ?
C21 C23 1.523(8) . ?
C22 C27 1.372(9) . ?
C22 O4 1.403(8) . ?
C22 C23 1.404(9) . ?
C23 C24 1.370(9) . ?
C24 C25 1.365(9) . ?
C25 C26 1.392(10) . ?
C25 S4 1.742(7) . ?
C26 C27 1.379(9) . ?
C27 C28 1.514(9) . ?
C28 C30 1.526(9) . ?
C29 O5 1.366(8) . ?
C29 C30 1.382(9) . ?
C29 C34 1.416(9) . ?
C30 C31 1.365(9) . ?
C31 C32 1.434(10) . ?
C32 C33 1.376(10) . ?
C32 S5 1.747(7) . ?
C33 C34 1.386(9) . ?
C34 C35 1.509(9) . ?
S1 O7 1.414(6) . ?
S1 O8 1.441(6) . ?
S1 O6 1.537(5) . ?
S2 O10 1.421(7) . ?
S2 O9 1.430(8) . ?
S2 O11 1.506(6) . ?
S3 O14 1.425(6) . ?
S3 O13 1.435(7) . ?
S3 O12 1.537(8) . ?
S4 O17 1.412(7) . ?
S4 O16 1.421(7) . ?
S4 O15 1.495(8) . ?
S5 O18 1.417(8) . ?
S5 O19 1.442(7) . ?
S5 O20 1.477(7) . ?
S6 O21 1.302(8) . ?
S6 O23 1.389(8) . ?
S6 O22 1.439(11) . ?
S6 O24 1.498(6) . ?
S7 O28 1.350(11) . ?
S7 O26 1.353(11) . ?
S7 O27 1.388(8) . ?
S7 O25 1.408(14) . ?
S8 O32 1.391(12) . ?
S8 O29 1.437(16) . ?
S8 O31 1.495(16) . ?
S8 O30 1.442(11) . ?
S9 O33 0.77(5) . ?
S9 O34 1.283(17) . ?
S9 O36 1.395(18) . ?
S9 O35 1.43(2) . ?
O33 O35 1.48(5) . ?
O33 O36 1.68(3) . ?
S10 O40 1.27(3) . ?
S10 O37 1.37(3) . ?
S10 O39 1.671(15) . ?
S10 O38 1.72(2) . ?
O41 S11 1.35(4) . ?
O41 O102 1.54(3) . ?
O41 S11A 1.64(4) . ?
O42 S11A 1.39(4) . ?
O42 S11 1.72(4) . ?
O43 S11 1.17(4) . ?
O43 S11A 1.19(5) . ?
O43 O102 1.57(4) . ?
O43 O44A 1.79(6) . ?
S11 O44 1.478(19) . ?
S11A O44A 1.37(3) . ?

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
C6 C1 O1 120.9(5) . . ?
C6 C1 C2 122.8(6) . . ?
O1 C1 C2 116.3(5) . . ?
C1 C2 C3 116.8(6) . . ?
C1 C2 C35 121.7(6) . . ?
C3 C2 C35 121.2(6) . . ?
C4 C3 C2 120.0(6) . . ?
C3 C4 C5 121.5(6) . . ?
C3 C4 S1 120.0(5) . . ?
C5 C4 S1 118.4(5) . . ?
C4 C5 C6 119.5(6) . . ?
C1 C6 C5 118.4(6) . . ?
C1 C6 C7 122.8(6) . . ?
C5 C6 C7 118.6(5) . . ?
C9 C7 C6 117.0(5) . . ?
C13 C8 O2 120.7(6) . . ?
C13 C8 C9 123.0(6) . . ?
O2 C8 C9 116.3(6) . . ?
C10 C9 C8 117.8(6) . . ?
C10 C9 C7 120.7(6) . . ?
C8 C9 C7 121.4(6) . . ?
C11 C10 C9 119.5(6) . . ?
C12 C11 C10 121.7(6) . . ?
C12 C11 S2 119.4(5) . . ?
C10 C11 S2 118.8(6) . . ?
C11 C12 C13 119.8(6) . . ?
C8 C13 C12 118.1(6) . . ?
C8 C13 C14 121.7(6) . . ?
C12 C13 C14 120.2(6) . . ?
C16 C14 C13 113.4(5) . . ?
O3 C15 C20 121.1(6) . . ?
O3 C15 C16 117.2(6) . . ?
C20 C15 C16 121.7(6) . . ?
C17 C16 C15 118.9(6) . . ?
C17 C16 C14 119.8(6) . . ?
C15 C16 C14 121.2(6) . . ?
C16 C17 C18 119.7(6) . . ?
C19 C18 C17 120.5(6) . . ?
C19 C18 S3 120.3(5) . . ?
C17 C18 S3 119.1(5) . . ?
C18 C19 C20 119.6(6) . . ?
C15 C20 C19 119.1(6) . . ?
C15 C20 C21 121.6(6) . . ?
C19 C20 C21 119.2(6) . . ?
C20 C21 C23 116.4(5) . . ?
C27 C22 O4 119.5(6) . . ?
C27 C22 C23 123.2(6) . . ?
O4 C22 C23 117.3(6) . . ?
C24 C23 C22 117.1(6) . . ?
C24 C23 C21 121.4(6) . . ?
C22 C23 C21 121.4(5) . . ?
C25 C24 C23 121.0(6) . . ?
C24 C25 C26 120.3(6) . . ?
C24 C25 S4 121.1(5) . . ?
C26 C25 S4 118.4(5) . . ?
C27 C26 C25 120.4(6) . . ?
C22 C27 C26 117.3(6) . . ?
C22 C27 C28 122.7(6) . . ?
C26 C27 C28 119.8(6) . . ?
C27 C28 C30 114.5(5) . . ?
O5 C29 C30 117.9(6) . . ?
O5 C29 C34 120.1(6) . . ?
C30 C29 C34 121.7(6) . . ?
C31 C30 C29 119.7(6) . . ?
C31 C30 C28 119.9(6) . . ?
C29 C30 C28 120.5(6) . . ?
C30 C31 C32 119.2(6) . . ?
C33 C32 C31 120.9(6) . . ?
C33 C32 S5 120.4(5) . . ?
C31 C32 S5 118.7(5) . . ?
C32 C33 C34 119.9(6) . . ?
C33 C34 C29 118.6(6) . . ?
C33 C34 C35 119.3(6) . . ?
C29 C34 C35 122.0(6) . . ?
C34 C35 C2 116.1(5) . . ?
O7 S1 O8 116.4(4) . . ?
O7 S1 O6 110.0(4) . . ?
O8 S1 O6 104.8(3) . . ?
O7 S1 C4 110.0(3) . . ?
O8 S1 C4 109.1(3) . . ?
O6 S1 C4 106.1(3) . . ?
O10 S2 O9 118.2(7) . . ?
O10 S2 O11 104.4(5) . . ?
O9 S2 O11 110.2(5) . . ?
O10 S2 C11 109.5(4) . . ?
O9 S2 C11 107.5(4) . . ?
O11 S2 C11 106.5(3) . . ?
O14 S3 O13 116.0(5) . . ?
O14 S3 O12 108.9(5) . . ?
O13 S3 O12 106.7(6) . . ?
O14 S3 C18 111.1(3) . . ?
O13 S3 C18 106.9(4) . . ?
O12 S3 C18 106.8(4) . . ?
O17 S4 O16 114.9(6) . . ?
O17 S4 O15 110.3(6) . . ?
O16 S4 O15 106.6(6) . . ?
O17 S4 C25 109.0(4) . . ?
O16 S4 C25 109.0(4) . . ?
O15 S4 C25 106.9(4) . . ?
O18 S5 O19 111.7(5) . . ?
O18 S5 O20 113.1(6) . . ?
O19 S5 O20 106.8(5) . . ?
O18 S5 C32 109.6(4) . . ?
O19 S5 C32 107.3(4) . . ?
O20 S5 C32 108.0(4) . . ?
O21 S6 O23 112.0(6) . . ?
O21 S6 O22 112.8(11) . . ?
O23 S6 O22 104.5(11) . . ?
O21 S6 O24 118.6(6) . . ?
O23 S6 O24 109.3(5) . . ?
O22 S6 O24 98.1(5) . . ?
O28 S7 O26 115.3(11) . . ?
O28 S7 O27 118.9(8) . . ?
O26 S7 O27 109.0(6) . . ?
O28 S7 O25 94.9(12) . . ?
O26 S7 O25 101.5(14) . . ?
O27 S7 O25 115.4(9) . . ?
O32 S8 O29 117.2(9) . . ?
O32 S8 O31 105.2(9) . . ?
O29 S8 O31 100.1(13) . . ?
O32 S8 O30 112.3(7) . . ?
O29 S8 O30 107.1(9) . . ?
O31 S8 O30 114.6(8) . . ?
O33 S9 O34 141(3) . . ?
O33 S9 O36 97(2) . . ?
O34 S9 O36 108.0(15) . . ?
O33 S9 O35 79(3) . . ?
O34 S9 O35 112.1(14) . . ?
O36 S9 O35 119(2) . . ?
S9 O33 O35 70(4) . . ?
S9 O33 O36 55.7(18) . . ?
O35 O33 O36 100(3) . . ?
S9 O35 O33 30.5(15) . . ?
S9 O36 O33 27.1(16) . . ?
O40 S10 O37 121(2) . . ?
O40 S10 O39 119.0(14) . . ?
O37 S10 O39 93.3(13) . . ?
O40 S10 O38 121.0(15) . . ?
O37 S10 O38 105.5(15) . . ?
O39 S10 O38 90.7(10) . . ?
S11 O41 O102 40.6(13) . . ?
S11 O41 S11A 20.0(13) . . ?
O102 O41 S11A 60.5(12) . . ?
S11A O42 S11 18.3(12) . . ?
S11 O43 S11A 29.0(16) . . ?
S11 O43 O102 40.4(18) . . ?
S11A O43 O102 69.4(17) . . ?
S11 O43 O44A 73(3) . . ?
S11A O43 O44A 50(2) . . ?
O102 O43 O44A 107.6(19) . . ?
O43 S11 O41 132(3) . . ?
O43 S11 O44 112(3) . . ?
O41 S11 O44 101(2) . . ?
O43 S11 O42 111(3) . . ?
O41 S11 O42 106(2) . . ?
O44 S11 O42 86(2) . . ?
O43 S11A O44A 89(3) . . ?
O43 S11A O42 138(4) . . ?
O44A S11A O42 107(2) . . ?
O43 S11A O41 108(3) . . ?
O44A S11A O41 98(3) . . ?
O42 S11A O41 108(3) . . ?
S11A O44A O43 41.7(18) . . ?
O41 O102 O43 96(2) . . ?

_diffrn_measured_fraction_theta_max    0.991
_diffrn_reflns_theta_full              27.50
_diffrn_measured_fraction_theta_full   0.991
_refine_diff_density_max    1.869
_refine_diff_density_min   -1.153
_refine_diff_density_rms    0.198