# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Pradyut Ghosh'
_publ_contact_author_email       ICPG@IACS.RES.IN

_publ_section_title              
;
"Anion Complexation of Pentafluorophenyl-Substituted
Tripodal Urea Receptor in solution and the Solid State: Selectivity
toward Phosphate
;
loop_
_publ_author_name
'Pradyut Ghosh'
'M Arunachalam'
'P S Lakshminarayanan'
'I Ravikumar'
;
E.Suresh
;

# Attachment 'Revised_Complex_1.cif'

data_94psm
_database_code_depnum_ccdc_archive 'CCDC 679393'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H54 F16 N8 O3'
_chemical_formula_weight         1034.94

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'
F F 0.0171 0.0103 '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                   12.9366(13)
_cell_length_b                   13.3131(13)
_cell_length_c                   15.2703(15)
_cell_angle_alpha                108.729(2)
_cell_angle_beta                 92.717(2)
_cell_angle_gamma                108.518(2)
_cell_volume                     2328.8(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5420
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      24.6

_exptl_crystal_description       BLOCKS
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.37
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1072
_exptl_absorpt_coefficient_mu    0.138
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.9255
_exptl_absorpt_correction_T_max  0.9507
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER SMART APEX CCD DIFFRACTOMETER'
_diffrn_measurement_method       'OMEGA-PHI SCAN'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16364
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.43
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8118
_reflns_number_gt                6755
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER SMART'
_computing_cell_refinement       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP, MERCURY'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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^)+(0.0600P)^2^+1.5215P] 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         8118
_refine_ls_number_parameters     659
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0551
_refine_ls_wR_factor_ref         0.1329
_refine_ls_wR_factor_gt          0.1268
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.095
_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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
F1 F 0.14023(13) -0.08646(12) 0.15241(11) 0.0303(4) Uani 1 d . . .
F2 F 0.26205(13) -0.18127(13) 0.03980(12) 0.0354(4) Uani 1 d . . .
F3 F 0.39519(13) -0.06745(14) -0.05466(11) 0.0364(4) Uani 1 d . . .
F4 F 0.40500(13) 0.14704(14) -0.03490(11) 0.0351(4) Uani 1 d . . .
F5 F 0.27579(12) 0.23972(12) 0.07112(10) 0.0274(4) Uani 1 d . . .
F6 F 0.34476(13) 0.22535(14) 0.30516(10) 0.0329(4) Uani 1 d . . .
F7 F 0.53887(14) 0.20092(16) 0.34242(12) 0.0432(4) Uani 1 d . . .
F8 F 0.66163(13) 0.31099(16) 0.51736(12) 0.0431(5) Uani 1 d . . .
F9 F 0.58970(13) 0.45044(15) 0.65271(11) 0.0359(4) Uani 1 d . . .
F10 F 0.40271(12) 0.48339(12) 0.61462(10) 0.0280(4) Uani 1 d . . .
F11 F 0.22614(12) 0.79117(12) 0.38145(10) 0.0272(3) Uani 1 d . . .
F12 F 0.35136(14) 0.95666(12) 0.32764(11) 0.0348(4) Uani 1 d . . .
F13 F 0.46075(13) 0.90852(13) 0.18105(11) 0.0336(4) Uani 1 d . . .
F14 F 0.44079(12) 0.68907(13) 0.08755(10) 0.0308(4) Uani 1 d . . .
F15 F 0.30391(12) 0.52068(12) 0.13241(10) 0.0272(4) Uani 1 d . . .
F16 F 0.15239(11) 0.34619(11) 0.27709(9) 0.0192(3) Uani 1 d . . .
O1 O -0.03124(14) -0.02702(14) 0.10025(12) 0.0228(4) Uani 1 d . . .
O2 O 0.19537(14) 0.32830(15) 0.56573(12) 0.0229(4) Uani 1 d . . .
O3 O 0.03957(14) 0.63006(15) 0.26471(12) 0.0243(4) Uani 1 d . . .
N1 N -0.12099(16) 0.27771(16) 0.33636(14) 0.0179(4) Uani 1 d . . .
N2 N -0.03556(18) 0.14144(19) 0.19701(16) 0.0236(5) Uani 1 d . . .
N3 N 0.12920(18) 0.12716(19) 0.16136(15) 0.0212(5) Uani 1 d . . .
N4 N 0.08419(17) 0.34207(19) 0.45336(16) 0.0217(5) Uani 1 d . . .
N5 N 0.26347(17) 0.36249(18) 0.43822(16) 0.0203(5) Uani 1 d . . .
N6 N 0.00680(17) 0.46970(18) 0.29879(15) 0.0196(5) Uani 1 d . . .
N7 N 0.17901(17) 0.56171(19) 0.27507(15) 0.0201(5) Uani 1 d . . .
N8 N 0.21369(17) 0.27841(16) 0.79986(14) 0.0183(4) Uani 1 d . . .
C1 C -0.1938(2) 0.1879(2) 0.25240(18) 0.0231(6) Uani 1 d . . .
H1A H -0.2044 0.2205 0.2058 0.028 Uiso 1 calc R . .
H1B H -0.2655 0.1554 0.2684 0.028 Uiso 1 calc R . .
C2 C -0.1478(2) 0.0949(2) 0.21083(18) 0.0225(6) Uani 1 d . . .
H2A H -0.1500 0.0528 0.2525 0.027 Uiso 1 calc R . .
H2B H -0.1934 0.0429 0.1512 0.027 Uiso 1 calc R . .
C3 C 0.0161(2) 0.0724(2) 0.14891(16) 0.0194(5) Uani 1 d . . .
C4 C 0.1971(2) 0.0773(2) 0.10963(17) 0.0201(5) Uani 1 d . . .
C5 C 0.1990(2) -0.0290(2) 0.10250(17) 0.0228(6) Uani 1 d . . .
C6 C 0.2642(2) -0.0771(2) 0.04746(18) 0.0250(6) Uani 1 d . . .
C7 C 0.3342(2) -0.0193(2) 0.00063(17) 0.0248(6) Uani 1 d . . .
C8 C 0.3389(2) 0.0893(2) 0.01109(18) 0.0245(6) Uani 1 d . . .
C9 C 0.2711(2) 0.1348(2) 0.06392(17) 0.0200(5) Uani 1 d . . .
C10 C -0.1149(2) 0.2393(2) 0.41628(17) 0.0202(5) Uani 1 d . . .
H10A H -0.1097 0.1645 0.3940 0.024 Uiso 1 calc R . .
H10B H -0.1824 0.2335 0.4426 0.024 Uiso 1 calc R . .
C11 C -0.0172(2) 0.3185(2) 0.49216(18) 0.0235(6) Uani 1 d . . .
H11A H -0.0292 0.3889 0.5232 0.028 Uiso 1 calc R . .
H11B H -0.0105 0.2845 0.5386 0.028 Uiso 1 calc R . .
C12 C 0.1803(2) 0.3432(2) 0.49150(16) 0.0182(5) Uani 1 d . . .
C13 C 0.3632(2) 0.3502(2) 0.45939(17) 0.0202(5) Uani 1 d . . .
C14 C 0.4039(2) 0.2817(2) 0.39187(17) 0.0237(6) Uani 1 d . . .
C15 C 0.5031(2) 0.2684(2) 0.4097(2) 0.0288(6) Uani 1 d . . .
C16 C 0.5655(2) 0.3243(2) 0.4985(2) 0.0287(6) Uani 1 d . . .
C17 C 0.5284(2) 0.3935(2) 0.56698(18) 0.0262(6) Uani 1 d . . .
C18 C 0.4299(2) 0.4074(2) 0.54743(18) 0.0227(6) Uani 1 d . . .
C19 C -0.1523(2) 0.3783(2) 0.35957(18) 0.0205(5) Uani 1 d . . .
H19A H -0.1222 0.4257 0.4246 0.025 Uiso 1 calc R . .
H19B H -0.2322 0.3553 0.3524 0.025 Uiso 1 calc R . .
C20 C -0.1104(2) 0.4464(2) 0.29701(18) 0.0216(5) Uani 1 d . . .
H20A H -0.1494 0.4039 0.2333 0.026 Uiso 1 calc R . .
H20B H -0.1244 0.5170 0.3190 0.026 Uiso 1 calc R . .
C21 C 0.0712(2) 0.5581(2) 0.27802(16) 0.0188(5) Uani 1 d . . .
C22 C 0.2547(2) 0.6492(2) 0.25474(17) 0.0193(5) Uani 1 d . . .
C23 C 0.2722(2) 0.7623(2) 0.30485(17) 0.0223(6) Uani 1 d . . .
C24 C 0.3387(2) 0.8488(2) 0.27931(18) 0.0241(6) Uani 1 d . . .
C25 C 0.3949(2) 0.8242(2) 0.20581(18) 0.0251(6) Uani 1 d . . .
C26 C 0.3850(2) 0.7140(2) 0.15850(17) 0.0230(6) Uani 1 d . . .
C27 C 0.3146(2) 0.6279(2) 0.18249(17) 0.0211(5) Uani 1 d . . .
C28 C 0.1139(2) 0.2284(2) 0.72243(17) 0.0184(5) Uani 1 d . . .
H28A H 0.0638 0.2692 0.7418 0.022 Uiso 1 calc R . .
H28B H 0.1388 0.2418 0.6669 0.022 Uiso 1 calc R . .
C29 C 0.0495(2) 0.1026(2) 0.69561(17) 0.0206(5) Uani 1 d . . .
H29A H 0.0936 0.0594 0.6644 0.025 Uiso 1 calc R . .
H29B H 0.0339 0.0854 0.7518 0.025 Uiso 1 calc R . .
C30 C -0.0580(2) 0.0685(2) 0.63119(19) 0.0278(6) Uani 1 d . . .
H30A H -0.0421 0.0898 0.5769 0.033 Uiso 1 calc R . .
H30B H -0.1029 0.1097 0.6638 0.033 Uiso 1 calc R . .
C31 C -0.1230(2) -0.0574(2) 0.5986(2) 0.0369(7) Uani 1 d . . .
H31A H -0.0806 -0.0985 0.5631 0.055 Uiso 1 calc R . .
H31B H -0.1914 -0.0743 0.5600 0.055 Uiso 1 calc R . .
H31C H -0.1380 -0.0793 0.6521 0.055 Uiso 1 calc R . .
C32 C 0.1782(2) 0.2773(2) 0.89356(17) 0.0203(5) Uani 1 d . . .
H32A H 0.1416 0.1991 0.8879 0.024 Uiso 1 calc R . .
H32B H 0.2442 0.3083 0.9405 0.024 Uiso 1 calc R . .
C33 C 0.1020(2) 0.3421(2) 0.92880(18) 0.0253(6) Uani 1 d . . .
H33A H 0.0401 0.3195 0.8796 0.030 Uiso 1 calc R . .
H33B H 0.1416 0.4227 0.9456 0.030 Uiso 1 calc R . .
C34 C 0.0596(2) 0.3180(2) 1.01422(18) 0.0251(6) Uani 1 d . . .
H34A H 0.0218 0.2371 0.9974 0.030 Uiso 1 calc R . .
H34B H 0.1217 0.3419 1.0635 0.030 Uiso 1 calc R . .
C35 C -0.0193(2) 0.3795(3) 1.0505(2) 0.0354(7) Uani 1 d . . .
H35A H 0.0201 0.4598 1.0736 0.053 Uiso 1 calc R . .
H35B H -0.0498 0.3572 1.1003 0.053 Uiso 1 calc R . .
H35C H -0.0779 0.3604 1.0004 0.053 Uiso 1 calc R . .
C36 C 0.2749(2) 0.39819(19) 0.80405(17) 0.0197(5) Uani 1 d . . .
H36A H 0.2233 0.4384 0.8114 0.024 Uiso 1 calc R . .
H36B H 0.3000 0.3944 0.7446 0.024 Uiso 1 calc R . .
C37 C 0.3739(2) 0.4664(2) 0.88226(18) 0.0252(6) Uani 1 d . . .
H37A H 0.4122 0.4171 0.8900 0.030 Uiso 1 calc R . .
H37B H 0.3483 0.4955 0.9406 0.030 Uiso 1 calc R . .
C38 C 0.4543(2) 0.5651(2) 0.86200(19) 0.0268(6) Uani 1 d . . .
H38A H 0.5152 0.6062 0.9141 0.032 Uiso 1 calc R . .
H38B H 0.4844 0.5350 0.8066 0.032 Uiso 1 calc R . .
C39 C 0.4032(3) 0.6478(2) 0.8466(2) 0.0366(7) Uani 1 d . . .
H39A H 0.3506 0.6110 0.7894 0.055 Uiso 1 calc R . .
H39B H 0.4602 0.7122 0.8424 0.055 Uiso 1 calc R . .
H39C H 0.3665 0.6723 0.8982 0.055 Uiso 1 calc R . .
C40 C 0.2871(2) 0.2079(2) 0.77889(17) 0.0203(5) Uani 1 d . . .
H40A H 0.2444 0.1315 0.7748 0.024 Uiso 1 calc R . .
H40B H 0.3472 0.2388 0.8313 0.024 Uiso 1 calc R . .
C41 C 0.3363(2) 0.2012(2) 0.68936(18) 0.0226(6) Uani 1 d . . .
H41A H 0.4079 0.2611 0.7037 0.027 Uiso 1 calc R . .
H41B H 0.2884 0.2121 0.6451 0.027 Uiso 1 calc R . .
C42 C 0.3494(2) 0.0864(2) 0.64537(19) 0.0280(6) Uani 1 d . . .
H42A H 0.3884 0.0714 0.6927 0.034 Uiso 1 calc R . .
H42B H 0.2767 0.0277 0.6241 0.034 Uiso 1 calc R . .
C43 C 0.4120(3) 0.0808(3) 0.5631(2) 0.0394(7) Uani 1 d . . .
H43A H 0.3746 0.0973 0.5166 0.059 Uiso 1 calc R . .
H43B H 0.4151 0.0062 0.5363 0.059 Uiso 1 calc R . .
H43C H 0.4857 0.1353 0.5846 0.059 Uiso 1 calc R . .
H5C H 0.239(2) 0.354(2) 0.385(2) 0.016(7) Uiso 1 d . . .
H7C H 0.193(2) 0.503(3) 0.273(2) 0.027(8) Uiso 1 d . . .
H6C H 0.031(2) 0.416(2) 0.2933(18) 0.017(7) Uiso 1 d . . .
H2C H 0.004(2) 0.207(3) 0.236(2) 0.023(7) Uiso 1 d . . .
H3C H 0.150(2) 0.195(3) 0.189(2) 0.025(8) Uiso 1 d . . .
H4C H 0.079(2) 0.342(2) 0.400(2) 0.027(8) Uiso 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
F1 0.0390(9) 0.0234(8) 0.0352(9) 0.0209(7) 0.0102(7) 0.0088(7)
F2 0.0409(10) 0.0201(8) 0.0448(10) 0.0086(7) -0.0005(8) 0.0144(7)
F3 0.0306(9) 0.0396(10) 0.0332(9) 0.0023(8) 0.0067(7) 0.0154(8)
F4 0.0328(9) 0.0405(10) 0.0339(9) 0.0197(8) 0.0152(7) 0.0075(8)
F5 0.0331(9) 0.0194(8) 0.0341(9) 0.0175(7) 0.0080(7) 0.0066(6)
F6 0.0294(9) 0.0409(10) 0.0229(8) 0.0057(7) 0.0031(7) 0.0110(7)
F7 0.0385(10) 0.0548(11) 0.0413(10) 0.0123(9) 0.0157(8) 0.0264(9)
F8 0.0287(9) 0.0707(13) 0.0457(11) 0.0298(10) 0.0084(8) 0.0283(9)
F9 0.0257(8) 0.0531(11) 0.0287(9) 0.0189(8) -0.0029(7) 0.0104(8)
F10 0.0288(8) 0.0271(8) 0.0235(8) 0.0055(7) 0.0017(6) 0.0076(7)
F11 0.0356(9) 0.0241(8) 0.0257(8) 0.0110(7) 0.0120(7) 0.0120(7)
F12 0.0480(10) 0.0169(8) 0.0347(9) 0.0071(7) 0.0095(8) 0.0070(7)
F13 0.0355(9) 0.0262(8) 0.0365(9) 0.0188(7) 0.0088(7) -0.0005(7)
F14 0.0299(9) 0.0318(9) 0.0280(8) 0.0116(7) 0.0129(7) 0.0052(7)
F15 0.0293(8) 0.0203(8) 0.0306(8) 0.0078(7) 0.0094(7) 0.0074(6)
F16 0.0219(7) 0.0174(7) 0.0201(7) 0.0088(6) 0.0029(6) 0.0072(6)
O1 0.0298(10) 0.0145(9) 0.0210(9) 0.0050(8) 0.0034(8) 0.0052(8)
O2 0.0237(9) 0.0280(10) 0.0211(9) 0.0151(8) 0.0032(7) 0.0080(8)
O3 0.0268(10) 0.0230(10) 0.0332(10) 0.0181(8) 0.0085(8) 0.0134(8)
N1 0.0210(11) 0.0157(10) 0.0190(11) 0.0088(9) 0.0033(8) 0.0065(8)
N2 0.0246(12) 0.0151(11) 0.0241(12) 0.0031(10) 0.0043(10) 0.0017(10)
N3 0.0254(12) 0.0126(11) 0.0238(12) 0.0065(10) 0.0063(9) 0.0041(9)
N4 0.0211(12) 0.0300(13) 0.0158(11) 0.0132(10) 0.0031(9) 0.0063(9)
N5 0.0186(11) 0.0268(12) 0.0182(12) 0.0141(10) 0.0006(9) 0.0059(9)
N6 0.0228(12) 0.0170(11) 0.0264(12) 0.0129(9) 0.0073(9) 0.0109(9)
N7 0.0219(12) 0.0187(11) 0.0285(12) 0.0168(10) 0.0087(9) 0.0096(9)
N8 0.0240(11) 0.0152(10) 0.0178(10) 0.0088(9) 0.0042(9) 0.0068(9)
C1 0.0200(13) 0.0233(14) 0.0268(14) 0.0111(11) 0.0012(11) 0.0069(11)
C2 0.0229(14) 0.0192(13) 0.0217(13) 0.0062(11) -0.0007(11) 0.0045(11)
C3 0.0273(14) 0.0202(14) 0.0140(12) 0.0105(11) 0.0042(10) 0.0084(11)
C4 0.0228(13) 0.0176(13) 0.0168(12) 0.0061(10) -0.0015(10) 0.0038(10)
C5 0.0263(14) 0.0214(13) 0.0208(13) 0.0115(11) 0.0032(11) 0.0046(11)
C6 0.0302(15) 0.0168(13) 0.0258(14) 0.0065(11) -0.0030(11) 0.0076(11)
C7 0.0233(14) 0.0282(15) 0.0182(13) 0.0002(11) 0.0011(11) 0.0115(12)
C8 0.0206(13) 0.0300(15) 0.0203(13) 0.0113(12) 0.0032(11) 0.0031(11)
C9 0.0224(13) 0.0171(13) 0.0193(13) 0.0087(10) -0.0018(10) 0.0038(10)
C10 0.0192(13) 0.0211(13) 0.0257(13) 0.0146(11) 0.0067(10) 0.0072(10)
C11 0.0238(14) 0.0288(14) 0.0228(13) 0.0142(12) 0.0052(11) 0.0102(11)
C12 0.0215(13) 0.0150(12) 0.0175(13) 0.0082(10) 0.0000(10) 0.0037(10)
C13 0.0181(13) 0.0228(13) 0.0233(13) 0.0169(11) 0.0044(10) 0.0031(11)
C14 0.0236(14) 0.0251(14) 0.0206(13) 0.0116(11) 0.0022(11) 0.0029(11)
C15 0.0269(15) 0.0336(16) 0.0334(16) 0.0177(13) 0.0144(12) 0.0130(12)
C16 0.0182(14) 0.0394(16) 0.0365(16) 0.0240(14) 0.0060(12) 0.0096(12)
C17 0.0229(14) 0.0315(15) 0.0239(14) 0.0166(12) 0.0000(11) 0.0028(12)
C18 0.0231(14) 0.0222(14) 0.0230(14) 0.0121(11) 0.0061(11) 0.0037(11)
C19 0.0199(13) 0.0195(13) 0.0238(13) 0.0095(11) 0.0057(10) 0.0069(10)
C20 0.0212(13) 0.0227(13) 0.0260(14) 0.0123(11) 0.0059(11) 0.0105(11)
C21 0.0238(14) 0.0178(13) 0.0170(12) 0.0078(10) 0.0046(10) 0.0084(11)
C22 0.0191(13) 0.0213(13) 0.0229(13) 0.0141(11) 0.0021(10) 0.0079(10)
C23 0.0222(13) 0.0273(14) 0.0201(13) 0.0102(11) 0.0039(11) 0.0103(11)
C24 0.0293(15) 0.0161(13) 0.0250(14) 0.0077(11) 0.0020(11) 0.0056(11)
C25 0.0231(14) 0.0243(14) 0.0268(14) 0.0159(12) 0.0026(11) 0.0000(11)
C26 0.0188(13) 0.0293(15) 0.0195(13) 0.0104(11) 0.0037(10) 0.0050(11)
C27 0.0214(13) 0.0185(13) 0.0224(13) 0.0067(11) 0.0020(11) 0.0064(10)
C28 0.0210(13) 0.0196(13) 0.0176(12) 0.0101(10) 0.0040(10) 0.0072(10)
C29 0.0236(14) 0.0175(13) 0.0235(13) 0.0108(11) 0.0054(11) 0.0070(11)
C30 0.0285(15) 0.0244(14) 0.0301(15) 0.0112(12) -0.0004(12) 0.0078(12)
C31 0.0334(17) 0.0269(16) 0.0435(18) 0.0130(14) -0.0054(14) 0.0027(13)
C32 0.0259(14) 0.0178(13) 0.0184(13) 0.0107(11) 0.0035(10) 0.0050(11)
C33 0.0310(15) 0.0266(14) 0.0214(14) 0.0100(11) 0.0065(11) 0.0124(12)
C34 0.0313(15) 0.0223(14) 0.0190(13) 0.0076(11) 0.0064(11) 0.0054(11)
C35 0.0390(17) 0.0400(18) 0.0249(15) 0.0088(13) 0.0123(13) 0.0128(14)
C36 0.0268(14) 0.0129(12) 0.0221(13) 0.0099(10) 0.0046(11) 0.0067(10)
C37 0.0301(15) 0.0208(14) 0.0246(14) 0.0093(11) 0.0042(11) 0.0078(11)
C38 0.0247(14) 0.0241(14) 0.0271(14) 0.0083(12) 0.0027(11) 0.0039(11)
C39 0.0376(17) 0.0232(15) 0.0452(18) 0.0176(14) -0.0008(14) 0.0013(13)
C40 0.0209(13) 0.0175(13) 0.0240(13) 0.0093(11) 0.0021(10) 0.0068(10)
C41 0.0239(14) 0.0219(13) 0.0249(14) 0.0116(11) 0.0052(11) 0.0082(11)
C42 0.0250(14) 0.0252(14) 0.0315(15) 0.0064(12) 0.0071(12) 0.0093(12)
C43 0.0345(17) 0.0452(19) 0.0382(17) 0.0080(15) 0.0106(14) 0.0197(15)

_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
F1 C5 1.343(3) . ?
F2 C6 1.344(3) . ?
F3 C7 1.335(3) . ?
F4 C8 1.342(3) . ?
F5 C9 1.347(3) . ?
F6 C14 1.343(3) . ?
F7 C15 1.339(3) . ?
F8 C16 1.342(3) . ?
F9 C17 1.342(3) . ?
F10 C18 1.339(3) . ?
F11 C23 1.340(3) . ?
F12 C24 1.339(3) . ?
F13 C25 1.350(3) . ?
F14 C26 1.342(3) . ?
F15 C27 1.343(3) . ?
O1 C3 1.220(3) . ?
O2 C12 1.229(3) . ?
O3 C21 1.222(3) . ?
N1 C19 1.461(3) . ?
N1 C1 1.465(3) . ?
N1 C10 1.474(3) . ?
N2 C3 1.354(3) . ?
N2 C2 1.442(3) . ?
N2 H2C 0.85(3) . ?
N3 C3 1.384(3) . ?
N3 C4 1.391(3) . ?
N3 H3C 0.81(3) . ?
N4 C12 1.342(3) . ?
N4 C11 1.450(3) . ?
N4 H4C 0.81(3) . ?
N5 C13 1.387(3) . ?
N5 C12 1.388(3) . ?
N5 H5C 0.81(3) . ?
N6 C21 1.349(3) . ?
N6 C20 1.445(3) . ?
N6 H6C 0.84(3) . ?
N7 C21 1.384(3) . ?
N7 C22 1.395(3) . ?
N7 H7C 0.85(3) . ?
N8 C40 1.512(3) . ?
N8 C36 1.517(3) . ?
N8 C28 1.520(3) . ?
N8 C32 1.526(3) . ?
C1 C2 1.513(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C4 C9 1.390(3) . ?
C4 C5 1.392(4) . ?
C5 C6 1.376(4) . ?
C6 C7 1.378(4) . ?
C7 C8 1.383(4) . ?
C8 C9 1.370(4) . ?
C10 C11 1.510(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C13 C14 1.388(4) . ?
C13 C18 1.395(4) . ?
C14 C15 1.377(4) . ?
C15 C16 1.382(4) . ?
C16 C17 1.372(4) . ?
C17 C18 1.376(4) . ?
C19 C20 1.524(3) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C22 C27 1.385(3) . ?
C22 C23 1.390(4) . ?
C23 C24 1.382(4) . ?
C24 C25 1.373(4) . ?
C25 C26 1.373(4) . ?
C26 C27 1.384(4) . ?
C28 C29 1.520(3) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.513(4) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C31 1.515(4) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 C33 1.517(4) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C34 1.527(3) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.520(4) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 C37 1.520(4) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 C38 1.526(4) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 C39 1.522(4) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 C41 1.524(3) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 C42 1.528(4) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 C43 1.521(4) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C19 N1 C1 110.45(19) . . ?
C19 N1 C10 112.57(19) . . ?
C1 N1 C10 112.69(19) . . ?
C3 N2 C2 120.5(2) . . ?
C3 N2 H2C 118.5(18) . . ?
C2 N2 H2C 117.1(18) . . ?
C3 N3 C4 122.3(2) . . ?
C3 N3 H3C 115(2) . . ?
C4 N3 H3C 121(2) . . ?
C12 N4 C11 124.6(2) . . ?
C12 N4 H4C 118(2) . . ?
C11 N4 H4C 117(2) . . ?
C13 N5 C12 121.2(2) . . ?
C13 N5 H5C 122.1(18) . . ?
C12 N5 H5C 111.7(19) . . ?
C21 N6 C20 121.3(2) . . ?
C21 N6 H6C 116.9(18) . . ?
C20 N6 H6C 118.1(18) . . ?
C21 N7 C22 119.5(2) . . ?
C21 N7 H7C 118.0(19) . . ?
C22 N7 H7C 120.9(19) . . ?
C40 N8 C36 110.89(18) . . ?
C40 N8 C28 110.27(18) . . ?
C36 N8 C28 106.92(17) . . ?
C40 N8 C32 106.44(18) . . ?
C36 N8 C32 111.38(18) . . ?
C28 N8 C32 110.98(18) . . ?
N1 C1 C2 112.4(2) . . ?
N1 C1 H1A 109.1 . . ?
C2 C1 H1A 109.1 . . ?
N1 C1 H1B 109.1 . . ?
C2 C1 H1B 109.1 . . ?
H1A C1 H1B 107.9 . . ?
N2 C2 C1 110.9(2) . . ?
N2 C2 H2A 109.5 . . ?
C1 C2 H2A 109.5 . . ?
N2 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
O1 C3 N2 124.1(2) . . ?
O1 C3 N3 123.6(2) . . ?
N2 C3 N3 112.4(2) . . ?
C9 C4 N3 120.5(2) . . ?
C9 C4 C5 115.9(2) . . ?
N3 C4 C5 123.5(2) . . ?
F1 C5 C6 117.5(2) . . ?
F1 C5 C4 120.9(2) . . ?
C6 C5 C4 121.6(2) . . ?
F2 C6 C5 120.3(2) . . ?
F2 C6 C7 118.7(2) . . ?
C5 C6 C7 121.0(2) . . ?
F3 C7 C6 120.7(2) . . ?
F3 C7 C8 120.7(2) . . ?
C6 C7 C8 118.6(2) . . ?
F4 C8 C9 120.2(2) . . ?
F4 C8 C7 119.9(2) . . ?
C9 C8 C7 119.8(2) . . ?
F5 C9 C8 118.4(2) . . ?
F5 C9 C4 118.5(2) . . ?
C8 C9 C4 123.0(2) . . ?
N1 C10 C11 112.5(2) . . ?
N1 C10 H10A 109.1 . . ?
C11 C10 H10A 109.1 . . ?
N1 C10 H10B 109.1 . . ?
C11 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
N4 C11 C10 111.0(2) . . ?
N4 C11 H11A 109.4 . . ?
C10 C11 H11A 109.4 . . ?
N4 C11 H11B 109.4 . . ?
C10 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
O2 C12 N4 124.6(2) . . ?
O2 C12 N5 122.1(2) . . ?
N4 C12 N5 113.2(2) . . ?
N5 C13 C14 121.0(2) . . ?
N5 C13 C18 122.9(2) . . ?
C14 C13 C18 116.0(2) . . ?
F6 C14 C15 118.0(2) . . ?
F6 C14 C13 119.2(2) . . ?
C15 C14 C13 122.8(2) . . ?
F7 C15 C14 120.7(3) . . ?
F7 C15 C16 119.9(2) . . ?
C14 C15 C16 119.4(2) . . ?
F8 C16 C17 120.4(2) . . ?
F8 C16 C15 120.1(3) . . ?
C17 C16 C15 119.5(2) . . ?
F9 C17 C16 119.9(2) . . ?
F9 C17 C18 119.8(2) . . ?
C16 C17 C18 120.3(2) . . ?
F10 C18 C17 117.5(2) . . ?
F10 C18 C13 120.5(2) . . ?
C17 C18 C13 121.9(2) . . ?
N1 C19 C20 111.7(2) . . ?
N1 C19 H19A 109.3 . . ?
C20 C19 H19A 109.3 . . ?
N1 C19 H19B 109.3 . . ?
C20 C19 H19B 109.3 . . ?
H19A C19 H19B 108.0 . . ?
N6 C20 C19 109.7(2) . . ?
N6 C20 H20A 109.7 . . ?
C19 C20 H20A 109.7 . . ?
N6 C20 H20B 109.7 . . ?
C19 C20 H20B 109.7 . . ?
H20A C20 H20B 108.2 . . ?
O3 C21 N6 124.2(2) . . ?
O3 C21 N7 122.3(2) . . ?
N6 C21 N7 113.5(2) . . ?
C27 C22 C23 116.5(2) . . ?
C27 C22 N7 121.9(2) . . ?
C23 C22 N7 121.7(2) . . ?
F11 C23 C24 117.6(2) . . ?
F11 C23 C22 120.5(2) . . ?
C24 C23 C22 121.9(2) . . ?
F12 C24 C25 119.8(2) . . ?
F12 C24 C23 120.3(2) . . ?
C25 C24 C23 119.8(2) . . ?
F13 C25 C26 120.1(2) . . ?
F13 C25 C24 120.1(2) . . ?
C26 C25 C24 119.8(2) . . ?
F14 C26 C25 120.4(2) . . ?
F14 C26 C27 119.9(2) . . ?
C25 C26 C27 119.7(2) . . ?
F15 C27 C26 118.1(2) . . ?
F15 C27 C22 119.8(2) . . ?
C26 C27 C22 122.1(2) . . ?
C29 C28 N8 116.15(19) . . ?
C29 C28 H28A 108.3 . . ?
N8 C28 H28A 108.3 . . ?
C29 C28 H28B 108.3 . . ?
N8 C28 H28B 108.3 . . ?
H28A C28 H28B 107.4 . . ?
C30 C29 C28 110.5(2) . . ?
C30 C29 H29A 109.5 . . ?
C28 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 108.1 . . ?
C29 C30 C31 112.6(2) . . ?
C29 C30 H30A 109.1 . . ?
C31 C30 H30A 109.1 . . ?
C29 C30 H30B 109.1 . . ?
C31 C30 H30B 109.1 . . ?
H30A C30 H30B 107.8 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C33 C32 N8 116.0(2) . . ?
C33 C32 H32A 108.3 . . ?
N8 C32 H32A 108.3 . . ?
C33 C32 H32B 108.3 . . ?
N8 C32 H32B 108.3 . . ?
H32A C32 H32B 107.4 . . ?
C32 C33 C34 109.8(2) . . ?
C32 C33 H33A 109.7 . . ?
C34 C33 H33A 109.7 . . ?
C32 C33 H33B 109.7 . . ?
C34 C33 H33B 109.7 . . ?
H33A C33 H33B 108.2 . . ?
C35 C34 C33 111.4(2) . . ?
C35 C34 H34A 109.3 . . ?
C33 C34 H34A 109.3 . . ?
C35 C34 H34B 109.3 . . ?
C33 C34 H34B 109.3 . . ?
H34A C34 H34B 108.0 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N8 C36 C37 115.22(19) . . ?
N8 C36 H36A 108.5 . . ?
C37 C36 H36A 108.5 . . ?
N8 C36 H36B 108.5 . . ?
C37 C36 H36B 108.5 . . ?
H36A C36 H36B 107.5 . . ?
C36 C37 C38 112.0(2) . . ?
C36 C37 H37A 109.2 . . ?
C38 C37 H37A 109.2 . . ?
C36 C37 H37B 109.2 . . ?
C38 C37 H37B 109.2 . . ?
H37A C37 H37B 107.9 . . ?
C39 C38 C37 114.3(2) . . ?
C39 C38 H38A 108.7 . . ?
C37 C38 H38A 108.7 . . ?
C39 C38 H38B 108.7 . . ?
C37 C38 H38B 108.7 . . ?
H38A C38 H38B 107.6 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N8 C40 C41 115.5(2) . . ?
N8 C40 H40A 108.4 . . ?
C41 C40 H40A 108.4 . . ?
N8 C40 H40B 108.4 . . ?
C41 C40 H40B 108.4 . . ?
H40A C40 H40B 107.5 . . ?
C40 C41 C42 110.5(2) . . ?
C40 C41 H41A 109.5 . . ?
C42 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C42 C41 H41B 109.5 . . ?
H41A C41 H41B 108.1 . . ?
C43 C42 C41 112.7(2) . . ?
C43 C42 H42A 109.1 . . ?
C41 C42 H42A 109.1 . . ?
C43 C42 H42B 109.1 . . ?
C41 C42 H42B 109.1 . . ?
H42A C42 H42B 107.8 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.063

# Attachment 'hsouream_R3.cif'

data_hsouream
_database_code_depnum_ccdc_archive 'CCDC 697104'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C86 H108 F30 N16 O10 S'
_chemical_formula_weight         2127.94

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'
F F 0.0171 0.0103 '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                   21.2559(15)
_cell_length_b                   19.5053(13)
_cell_length_c                   23.6564(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.3770(10)
_cell_angle_gamma                90.00
_cell_volume                     9764.8(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6500
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      23.5

_exptl_crystal_description       PLATES
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4408
_exptl_absorpt_coefficient_mu    0.155
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9267
_exptl_absorpt_correction_T_max  0.9609
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER APEX II CCD AREA DETECTOR'
_diffrn_measurement_method       'OMEGA SCAN'
_diffrn_detector_area_resol_mean 3
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24105
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_sigmaI/netI    0.0441
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.61
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8582
_reflns_number_gt                7052
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER APEX II'
_computing_cell_refinement       'BRUKER APEX II'
_computing_data_reduction        'BRUKER AXS SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'BRUKER SHELXTL'
_computing_publication_material  'MERCURY 2.2'

_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. It should be noted that the
Principal mean square atomic displacements U values for F6 and F8 indicates
that there is a disorder. However we could not able to model the disorder as
the principal mean square atomic displacements U values for the rest of the
phenyl ring was in agreement with the model. As a result the fluorine atoms
were left as non-disordered(and planar to the ring).
;

_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^)+(0.0663P)^2^+49.1031P] 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         8582
_refine_ls_number_parameters     691
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0787
_refine_ls_wR_factor_ref         0.1893
_refine_ls_wR_factor_gt          0.1798
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.007
_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
S1 S 0.0000 0.90492(6) 0.2500 0.0292(3) Uani 1 2 d S . .
F1 F 0.08529(11) 0.71132(15) 0.26576(10) 0.0497(7) Uani 1 1 d . . .
F2 F 0.09819(12) 0.57692(17) 0.24435(11) 0.0622(8) Uani 1 1 d . . .
F3 F 0.04802(13) 0.48143(14) 0.31164(13) 0.0607(8) Uani 1 1 d . . .
F4 F -0.01629(13) 0.52305(12) 0.39877(12) 0.0533(7) Uani 1 1 d . . .
F5 F -0.03638(11) 0.65654(12) 0.41626(9) 0.0391(6) Uani 1 1 d . . .
F7 F 0.2170(2) 0.6822(2) 0.05467(13) 0.1013(14) Uani 1 1 d . . .
F6 F 0.1224(3) 0.87520(15) 0.1270(2) 0.155(3) Uani 1 1 d . . .
F8 F 0.1475(3) 0.7982(2) 0.03800(15) 0.163(3) Uani 1 1 d . . .
C15 C 0.1569(3) 0.8187(2) 0.1362(2) 0.076(2) Uani 1 1 d . . .
C14 C 0.1690(4) 0.7796(3) 0.0908(2) 0.085(2) Uani 1 1 d . . .
F9 F 0.25902(15) 0.64496(16) 0.16095(14) 0.0715(9) Uani 1 1 d . . .
F10 F 0.23237(12) 0.71940(12) 0.25046(10) 0.0453(6) Uani 1 1 d . . .
F11 F -0.11018(11) 1.00470(14) 0.42437(9) 0.0459(6) Uani 1 1 d . . .
F12 F -0.23479(13) 0.98795(15) 0.43263(11) 0.0552(7) Uani 1 1 d . . .
F13 F -0.31828(11) 1.00349(14) 0.33980(12) 0.0533(7) Uani 1 1 d . . .
F14 F -0.27584(12) 1.03653(15) 0.23811(11) 0.0554(7) Uani 1 1 d . . .
F15 F -0.15166(11) 1.05989(13) 0.23134(10) 0.0436(6) Uani 1 1 d . . .
O1 O 0.05996(13) 0.75222(13) 0.44400(10) 0.0324(6) Uani 1 1 d . . .
O2 O 0.26177(13) 0.85432(15) 0.27951(11) 0.0374(7) Uani 1 1 d . . .
O3 O -0.04183(13) 1.12119(15) 0.39456(12) 0.0403(7) Uani 1 1 d . . .
O4 O 0.0475(2) 0.9024(2) 0.19937(19) 0.0222(10) Uani 0.50 1 d P . .
O5A O 0.0440(2) 0.9559(3) 0.2697(2) 0.0257(11) Uani 0.50 1 d P . .
O5 O 0.0420(2) 0.9244(3) 0.2987(2) 0.0234(10) Uani 0.50 1 d P . .
O6 O 0.0233(2) 0.8370(2) 0.24806(19) 0.0212(10) Uani 0.50 1 d P . .
N1 N 0.13005(15) 0.97433(16) 0.41620(13) 0.0326(7) Uani 1 1 d . . .
N2 N 0.03350(19) 0.85587(18) 0.40607(16) 0.0410(9) Uani 1 1 d . . .
N3 N 0.01757(16) 0.75878(17) 0.35197(14) 0.0327(8) Uani 1 1 d . . .
N4 N 0.18064(18) 0.90696(18) 0.31772(16) 0.0390(9) Uani 1 1 d . . .
N5 N 0.1626(2) 0.8426(2) 0.23636(19) 0.0514(12) Uani 1 1 d . . .
N6 N 0.03841(15) 1.06470(17) 0.35640(14) 0.0304(7) Uani 1 1 d . . .
N7 N -0.06366(16) 1.0448(2) 0.32265(15) 0.0376(9) Uani 1 1 d . . .
N8 N 0.08741(13) 0.31279(15) 0.09523(12) 0.0234(6) Uani 1 1 d . . .
C1 C 0.1253(2) 0.9174(2) 0.45499(17) 0.0470(12) Uani 1 1 d . . .
H1A H 0.1422 0.9312 0.4928 0.056 Uiso 1 1 calc R . .
H1B H 0.1506 0.8795 0.4433 0.056 Uiso 1 1 calc R . .
C2 C 0.0576(3) 0.8934(2) 0.45700(18) 0.0566(15) Uani 1 1 d . . .
H2A H 0.0553 0.8642 0.4899 0.068 Uiso 1 1 calc R . .
H2B H 0.0309 0.9330 0.4615 0.068 Uiso 1 1 calc R . .
C3 C 0.03867(17) 0.78769(19) 0.40402(16) 0.0291(8) Uani 1 1 d . . .
C4 C 0.02613(17) 0.68894(19) 0.34291(15) 0.0291(8) Uani 1 1 d . . .
C5 C 0.05986(18) 0.6652(2) 0.29900(16) 0.0359(10) Uani 1 1 d . . .
C6 C 0.06713(19) 0.5965(3) 0.28803(17) 0.0423(11) Uani 1 1 d . . .
C7 C 0.0420(2) 0.5488(2) 0.32217(19) 0.0408(10) Uani 1 1 d . . .
C8 C 0.00914(19) 0.5702(2) 0.36592(18) 0.0377(10) Uani 1 1 d . . .
C9 C 0.00007(18) 0.6389(2) 0.37563(16) 0.0327(9) Uani 1 1 d . . .
C10 C 0.1947(2) 0.9853(2) 0.3994(2) 0.0452(11) Uani 1 1 d . . .
H10A H 0.2228 0.9930 0.4335 0.054 Uiso 1 1 calc R . .
H10B H 0.1946 1.0269 0.3769 0.054 Uiso 1 1 calc R . .
C11 C 0.2214(2) 0.9290(2) 0.36663(18) 0.0445(11) Uani 1 1 d . . .
H11A H 0.2613 0.9442 0.3541 0.053 Uiso 1 1 calc R . .
H11B H 0.2301 0.8901 0.3916 0.053 Uiso 1 1 calc R . .
C12 C 0.20539(19) 0.86740(19) 0.27854(17) 0.0330(9) Uani 1 1 d . . .
C13 C 0.1783(2) 0.8021(2) 0.19154(18) 0.0372(10) Uani 1 1 d . . .
C16 C 0.2039(3) 0.7217(3) 0.0986(2) 0.0631(16) Uani 1 1 d . . .
C17 C 0.2257(2) 0.7027(2) 0.15295(19) 0.0427(10) Uani 1 1 d . . .
C18 C 0.21284(18) 0.7424(2) 0.19861(16) 0.0315(9) Uani 1 1 d . . .
C19 C 0.10879(19) 1.0382(2) 0.44108(16) 0.0339(9) Uani 1 1 d . . .
H19A H 0.1429 1.0570 0.4665 0.041 Uiso 1 1 calc R . .
H19B H 0.0738 1.0282 0.4633 0.041 Uiso 1 1 calc R . .
H20A H 0.0735 1.1314 0.4145 0.041 Uiso 1 1 d R . .
H20B H 0.1242 1.1034 0.3762 0.041 Uiso 1 1 d R . .
C20 C 0.08824(19) 1.0907(2) 0.39623(17) 0.0347(9) Uani 1 1 d . . .
C21 C -0.02248(19) 1.0793(2) 0.36128(16) 0.0320(9) Uani 1 1 d . . .
C22 C -0.12811(18) 1.0370(2) 0.32848(17) 0.0332(9) Uani 1 1 d . . .
C23 C -0.1508(2) 1.0176(2) 0.37924(17) 0.0366(10) Uani 1 1 d . . .
C24 C -0.2140(2) 1.0071(2) 0.38278(18) 0.0402(10) Uani 1 1 d . . .
C25 C -0.2567(2) 1.0139(2) 0.33591(19) 0.0415(10) Uani 1 1 d . . .
C26 C -0.23511(19) 1.0311(2) 0.28453(18) 0.0388(10) Uani 1 1 d . . .
C27 C -0.17171(19) 1.0430(2) 0.28160(17) 0.0353(9) Uani 1 1 d . . .
C28 C 0.01977(17) 0.29398(18) 0.07425(15) 0.0260(8) Uani 1 1 d . . .
H28A H 0.0161 0.2940 0.0331 0.031 Uiso 1 1 calc R . .
H28B H 0.0119 0.2475 0.0864 0.031 Uiso 1 1 calc R . .
C29 C -0.03153(17) 0.33988(19) 0.09368(15) 0.0278(8) Uani 1 1 d . . .
H29A H -0.0229 0.3872 0.0846 0.033 Uiso 1 1 calc R . .
H29B H -0.0324 0.3362 0.1345 0.033 Uiso 1 1 calc R . .
C30 C -0.09539(17) 0.3183(2) 0.06398(16) 0.0313(9) Uani 1 1 d . . .
H30A H -0.0967 0.3299 0.0240 0.038 Uiso 1 1 calc R . .
H30B H -0.0998 0.2690 0.0669 0.038 Uiso 1 1 calc R . .
C31 C -0.15065(19) 0.3528(2) 0.08943(18) 0.0415(10) Uani 1 1 d . . .
H31A H -0.1507 0.3397 0.1285 0.062 Uiso 1 1 calc R . .
H31B H -0.1896 0.3387 0.0689 0.062 Uiso 1 1 calc R . .
H31C H -0.1464 0.4017 0.0869 0.062 Uiso 1 1 calc R . .
C32 C 0.09645(18) 0.3209(2) 0.15932(14) 0.0284(8) Uani 1 1 d . . .
H32A H 0.1383 0.3396 0.1694 0.034 Uiso 1 1 calc R . .
H32B H 0.0661 0.3544 0.1703 0.034 Uiso 1 1 calc R . .
C33 C 0.0895(2) 0.2569(2) 0.19351(16) 0.0359(9) Uani 1 1 d . . .
H33A H 0.1228 0.2247 0.1869 0.043 Uiso 1 1 calc R . .
H33B H 0.0491 0.2354 0.1823 0.043 Uiso 1 1 calc R . .
C34 C 0.0936(2) 0.2763(2) 0.25656(17) 0.0397(10) Uani 1 1 d . . .
H34A H 0.1324 0.3016 0.2664 0.048 Uiso 1 1 calc R . .
H34B H 0.0585 0.3061 0.2631 0.048 Uiso 1 1 calc R . .
C35 C 0.0922(3) 0.2145(2) 0.29417(18) 0.0502(12) Uani 1 1 d . . .
H35A H 0.0553 0.1876 0.2828 0.075 Uiso 1 1 calc R . .
H35B H 0.0909 0.2290 0.3328 0.075 Uiso 1 1 calc R . .
H35C H 0.1294 0.1874 0.2910 0.075 Uiso 1 1 calc R . .
C36 C 0.12786(17) 0.25459(19) 0.07537(15) 0.0259(8) Uani 1 1 d . . .
H36A H 0.1138 0.2121 0.0913 0.031 Uiso 1 1 calc R . .
H36B H 0.1201 0.2510 0.0344 0.031 Uiso 1 1 calc R . .
C37 C 0.19812(17) 0.2610(2) 0.09046(16) 0.0307(8) Uani 1 1 d . . .
H37A H 0.2061 0.2786 0.1288 0.037 Uiso 1 1 calc R . .
H37B H 0.2155 0.2934 0.0649 0.037 Uiso 1 1 calc R . .
C38 C 0.23050(19) 0.1922(2) 0.08629(18) 0.0385(10) Uani 1 1 d . . .
H38A H 0.2120 0.1597 0.1110 0.046 Uiso 1 1 calc R . .
H38B H 0.2231 0.1753 0.0477 0.046 Uiso 1 1 calc R . .
C39 C 0.3011(2) 0.1961(3) 0.1026(2) 0.0493(12) Uani 1 1 d . . .
H39A H 0.3204 0.2243 0.0758 0.074 Uiso 1 1 calc R . .
H39B H 0.3189 0.1508 0.1025 0.074 Uiso 1 1 calc R . .
H39C H 0.3088 0.2156 0.1399 0.074 Uiso 1 1 calc R . .
C40 C 0.10661(17) 0.38134(18) 0.07254(15) 0.0266(8) Uani 1 1 d . . .
H40A H 0.1514 0.3876 0.0833 0.032 Uiso 1 1 calc R . .
H40B H 0.0844 0.4169 0.0914 0.032 Uiso 1 1 calc R . .
C41 C 0.09484(18) 0.39255(19) 0.00901(15) 0.0299(8) Uani 1 1 d . . .
H41A H 0.0511 0.4054 -0.0006 0.036 Uiso 1 1 calc R . .
H41B H 0.1027 0.3503 -0.0108 0.036 Uiso 1 1 calc R . .
C42 C 0.1382(2) 0.4491(2) -0.00998(17) 0.0358(9) Uani 1 1 d . . .
H42A H 0.1817 0.4339 -0.0028 0.043 Uiso 1 1 calc R . .
H42B H 0.1295 0.4554 -0.0506 0.043 Uiso 1 1 calc R . .
C43 C 0.1316(2) 0.5175(2) 0.01896(19) 0.0457(11) Uani 1 1 d . . .
H43A H 0.0894 0.5345 0.0104 0.069 Uiso 1 1 calc R . .
H43B H 0.1611 0.5496 0.0055 0.069 Uiso 1 1 calc R . .
H43C H 0.1401 0.5120 0.0593 0.069 Uiso 1 1 calc R . .
H4C H 0.143(2) 0.913(2) 0.3164(18) 0.037(12) Uiso 1 1 d . . .
H7C H -0.049(2) 1.018(2) 0.3038(19) 0.038(13) Uiso 1 1 d . . .
H6C H 0.0454(19) 1.030(2) 0.3367(18) 0.032(11) Uiso 1 1 d . . .
H3C H 0.014(2) 0.782(2) 0.3246(19) 0.038(12) Uiso 1 1 d . . .
H5C H 0.129(2) 0.853(3) 0.233(2) 0.051(16) Uiso 1 1 d . . .
H2C H 0.018(2) 0.874(3) 0.378(2) 0.057(16) 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 0.0357(7) 0.0170(6) 0.0322(7) 0.000 -0.0114(6) 0.000
F1 0.0365(13) 0.0793(19) 0.0348(13) 0.0181(13) 0.0110(11) 0.0014(13)
F2 0.0450(16) 0.099(2) 0.0426(15) -0.0115(15) 0.0052(12) 0.0294(15)
F3 0.0546(17) 0.0492(17) 0.076(2) -0.0230(14) -0.0058(14) 0.0130(13)
F4 0.0592(17) 0.0315(14) 0.0700(18) 0.0075(12) 0.0093(14) -0.0110(12)
F5 0.0472(14) 0.0359(13) 0.0363(12) 0.0062(10) 0.0155(11) -0.0037(11)
F7 0.148(4) 0.115(3) 0.0448(18) -0.0398(19) 0.031(2) -0.056(3)
F6 0.255(6) 0.0257(16) 0.150(4) -0.015(2) -0.162(4) 0.027(2)
F8 0.341(8) 0.068(2) 0.058(2) 0.0202(19) -0.097(3) -0.058(4)
C15 0.124(5) 0.018(2) 0.071(4) 0.005(2) -0.062(4) -0.004(3)
C14 0.161(7) 0.043(3) 0.042(3) 0.007(2) -0.041(4) -0.039(4)
F9 0.0666(19) 0.067(2) 0.081(2) -0.0335(17) 0.0061(16) 0.0290(16)
F10 0.0613(17) 0.0392(14) 0.0351(13) 0.0058(11) 0.0026(11) 0.0197(12)
F11 0.0448(14) 0.0646(17) 0.0287(12) -0.0089(11) 0.0064(11) 0.0049(12)
F12 0.0520(16) 0.0760(19) 0.0404(14) -0.0020(13) 0.0194(12) -0.0036(14)
F13 0.0323(14) 0.0650(18) 0.0639(17) 0.0069(14) 0.0122(12) 0.0025(12)
F14 0.0362(14) 0.0738(19) 0.0548(16) 0.0174(14) -0.0039(12) 0.0013(13)
F15 0.0407(13) 0.0561(16) 0.0346(13) 0.0060(11) 0.0075(10) -0.0001(11)
O1 0.0462(16) 0.0263(14) 0.0245(13) 0.0068(11) 0.0022(12) 0.0001(12)
O2 0.0288(15) 0.0518(18) 0.0319(15) -0.0041(13) 0.0040(12) 0.0005(13)
O3 0.0393(16) 0.0430(17) 0.0406(16) -0.0177(14) 0.0146(13) 0.0040(13)
O4 0.022(2) 0.025(3) 0.021(2) -0.005(2) 0.0109(19) 0.002(2)
O5A 0.038(3) 0.019(3) 0.020(3) 0.000(2) 0.004(2) -0.007(2)
O5 0.025(3) 0.021(3) 0.025(3) -0.001(2) 0.005(2) 0.002(2)
O6 0.019(2) 0.020(2) 0.025(2) 0.001(2) 0.002(2) 0.0018(17)
N1 0.0324(18) 0.0335(18) 0.0311(17) -0.0100(14) -0.0014(14) 0.0056(14)
N2 0.061(2) 0.033(2) 0.032(2) 0.0112(16) 0.0174(18) 0.0106(17)
N3 0.0388(19) 0.0315(19) 0.0277(18) 0.0168(15) 0.0028(15) -0.0006(15)
N4 0.0257(19) 0.037(2) 0.052(2) -0.0137(17) -0.0071(16) 0.0090(16)
N5 0.033(2) 0.043(2) 0.073(3) -0.026(2) -0.022(2) 0.0177(18)
N6 0.0310(18) 0.0297(18) 0.0317(18) -0.0061(15) 0.0095(14) 0.0036(14)
N7 0.0321(19) 0.050(2) 0.0323(18) -0.0161(17) 0.0088(15) 0.0136(17)
N8 0.0238(15) 0.0284(16) 0.0189(14) -0.0015(12) 0.0070(12) 0.0020(12)
C1 0.074(3) 0.039(3) 0.027(2) -0.0090(18) -0.003(2) 0.018(2)
C2 0.118(5) 0.026(2) 0.032(2) 0.0067(18) 0.039(3) 0.015(3)
C3 0.030(2) 0.029(2) 0.030(2) 0.0110(17) 0.0120(16) 0.0010(16)
C4 0.0249(19) 0.033(2) 0.0278(19) 0.0069(16) -0.0039(15) -0.0007(16)
C5 0.024(2) 0.056(3) 0.027(2) 0.0104(19) -0.0012(16) 0.0007(18)
C6 0.027(2) 0.067(3) 0.032(2) -0.010(2) -0.0020(17) 0.018(2)
C7 0.036(2) 0.039(2) 0.046(3) -0.009(2) -0.0035(19) 0.0074(19)
C8 0.035(2) 0.036(2) 0.041(2) 0.0023(19) 0.0005(19) -0.0030(18)
C9 0.032(2) 0.036(2) 0.030(2) 0.0016(17) 0.0022(17) -0.0003(17)
C10 0.034(2) 0.051(3) 0.049(3) -0.012(2) -0.008(2) 0.001(2)
C11 0.035(2) 0.056(3) 0.041(2) -0.011(2) -0.0003(19) 0.000(2)
C12 0.032(2) 0.026(2) 0.039(2) 0.0008(17) -0.0053(17) 0.0062(17)
C13 0.042(2) 0.025(2) 0.042(2) -0.0051(18) -0.0114(19) 0.0015(18)
C16 0.095(4) 0.063(4) 0.033(3) -0.016(2) 0.013(3) -0.039(3)
C17 0.043(3) 0.041(2) 0.046(3) -0.009(2) 0.012(2) 0.001(2)
C18 0.034(2) 0.032(2) 0.029(2) 0.0062(16) 0.0046(16) 0.0006(17)
C19 0.035(2) 0.032(2) 0.034(2) -0.0119(17) 0.0001(17) -0.0004(17)
C20 0.035(2) 0.028(2) 0.043(2) -0.0050(18) 0.0136(18) -0.0080(17)
C21 0.039(2) 0.032(2) 0.0274(19) -0.0011(16) 0.0112(17) 0.0062(17)
C22 0.032(2) 0.032(2) 0.037(2) -0.0120(17) 0.0088(17) 0.0105(17)
C23 0.040(2) 0.039(2) 0.030(2) -0.0100(18) 0.0031(18) 0.0096(19)
C24 0.042(2) 0.044(3) 0.037(2) -0.0032(19) 0.0156(19) 0.0065(19)
C25 0.034(2) 0.039(2) 0.053(3) -0.002(2) 0.008(2) 0.0057(19)
C26 0.034(2) 0.037(2) 0.045(2) 0.0043(19) 0.0026(19) 0.0064(18)
C27 0.038(2) 0.034(2) 0.035(2) -0.0028(18) 0.0084(18) 0.0112(18)
C28 0.0279(19) 0.0257(19) 0.0247(18) 0.0019(15) 0.0041(15) 0.0007(15)
C29 0.030(2) 0.029(2) 0.0261(18) 0.0016(15) 0.0070(15) 0.0030(16)
C30 0.030(2) 0.031(2) 0.033(2) 0.0050(17) 0.0057(16) 0.0023(16)
C31 0.031(2) 0.053(3) 0.041(2) 0.009(2) 0.0079(18) 0.0085(19)
C32 0.0260(19) 0.040(2) 0.0196(17) -0.0027(16) 0.0027(14) 0.0049(16)
C33 0.040(2) 0.041(2) 0.028(2) 0.0017(17) 0.0121(17) 0.0087(19)
C34 0.049(3) 0.041(2) 0.031(2) 0.0019(18) 0.0126(18) 0.007(2)
C35 0.079(3) 0.045(3) 0.028(2) 0.0033(19) 0.011(2) 0.012(2)
C36 0.0308(19) 0.0268(19) 0.0207(17) 0.0000(15) 0.0057(15) 0.0036(15)
C37 0.031(2) 0.037(2) 0.0259(19) -0.0010(16) 0.0122(16) 0.0009(17)
C38 0.032(2) 0.042(2) 0.042(2) -0.0020(19) 0.0073(18) 0.0073(18)
C39 0.035(2) 0.059(3) 0.054(3) -0.012(2) 0.008(2) 0.016(2)
C40 0.0266(19) 0.0243(19) 0.0291(19) -0.0031(15) 0.0037(15) -0.0027(15)
C41 0.035(2) 0.026(2) 0.029(2) 0.0000(15) 0.0032(16) -0.0009(16)
C42 0.042(2) 0.032(2) 0.035(2) 0.0037(17) 0.0092(18) -0.0046(18)
C43 0.058(3) 0.032(2) 0.048(3) 0.010(2) 0.010(2) -0.007(2)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O5A 1.413(5) 1 ?
S1 O5A 1.413(5) . ?
S1 O5A 1.413(5) 2 ?
S1 O6 1.417(5) 2 ?
S1 O6 1.417(5) . ?
S1 O6 1.417(5) 1 ?
S1 O5 1.441(5) 2 ?
S1 O5 1.441(5) . ?
S1 O5 1.441(5) 1 ?
S1 O4 1.638(4) . ?
S1 O4 1.638(4) 1 ?
S1 O4 1.638(4) 2 ?
F1 C5 1.342(5) . ?
F2 C6 1.333(5) . ?
F3 C7 1.346(5) . ?
F4 C8 1.349(5) . ?
F5 C9 1.335(4) . ?
F7 C16 1.343(6) . ?
F6 C15 1.330(6) . ?
F8 C14 1.338(6) . ?
C15 C14 1.360(9) . ?
C15 C13 1.384(6) . ?
C14 C16 1.355(9) . ?
F9 C17 1.334(5) . ?
F10 C18 1.335(4) . ?
F11 C23 1.333(5) . ?
F12 C24 1.350(5) . ?
F13 C25 1.336(5) . ?
F14 C26 1.337(5) . ?
F15 C27 1.341(5) . ?
O1 C3 1.224(4) . ?
O2 C12 1.223(5) . ?
O3 C21 1.232(4) . ?
O4 O4 0.000(13) 1 ?
O5A O5A 0.000(10) 1 ?
O5A O5 0.923(6) 1 ?
O5A O5 0.923(6) . ?
O5 O5 0.0000 1 ?
O5 O5A 0.923(6) 1 ?
O6 O6 0.000(9) 1 ?
O6 O6 1.005(8) 2 ?
N1 C1 1.450(6) . ?
N1 C19 1.466(5) . ?
N1 C10 1.482(6) . ?
N2 C3 1.336(5) . ?
N2 C2 1.461(6) . ?
N2 H2C 0.80(5) . ?
N3 C3 1.390(5) . ?
N3 C4 1.394(5) . ?
N3 H3C 0.79(5) . ?
N4 C12 1.350(5) . ?
N4 C11 1.444(5) . ?
N4 H4C 0.80(5) . ?
N5 C12 1.373(5) . ?
N5 C13 1.387(6) . ?
N5 H5C 0.75(5) . ?
N6 C21 1.341(5) . ?
N6 C20 1.442(5) . ?
N6 H6C 0.84(4) . ?
N7 C21 1.381(5) . ?
N7 C22 1.398(5) . ?
N7 H7C 0.77(5) . ?
N8 C40 1.511(5) . ?
N8 C32 1.518(4) . ?
N8 C28 1.521(5) . ?
N8 C36 1.525(4) . ?
C1 C2 1.517(7) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C4 C9 1.393(5) . ?
C4 C5 1.396(6) . ?
C5 C6 1.376(6) . ?
C6 C7 1.372(7) . ?
C7 C8 1.366(6) . ?
C8 C9 1.377(6) . ?
C10 C11 1.486(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C13 C18 1.378(6) . ?
C16 C17 1.377(7) . ?
C17 C18 1.378(6) . ?
C19 C20 1.510(6) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9697 . ?
C20 H20B 0.9687 . ?
C22 C27 1.382(6) . ?
C22 C23 1.389(6) . ?
C23 C24 1.369(6) . ?
C24 C25 1.372(6) . ?
C25 C26 1.380(6) . ?
C26 C27 1.376(6) . ?
C28 C29 1.515(5) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.528(5) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C31 1.526(5) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 C33 1.502(5) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C34 1.534(5) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.500(6) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 C37 1.508(5) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 C38 1.516(5) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 C39 1.516(6) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 C41 1.516(5) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 C42 1.531(5) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 C43 1.513(6) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5A S1 O5A 0.0(5) 1 . ?
O5A S1 O5A 90.7(5) 1 2 ?
O5A S1 O5A 90.7(5) . 2 ?
O5A S1 O6 150.4(3) 1 2 ?
O5A S1 O6 150.4(3) . 2 ?
O5A S1 O6 116.4(3) 2 2 ?
O5A S1 O6 116.4(3) 1 . ?
O5A S1 O6 116.4(3) . . ?
O5A S1 O6 150.4(3) 2 . ?
O6 S1 O6 41.5(3) 2 . ?
O5A S1 O6 116.4(3) 1 1 ?
O5A S1 O6 116.4(3) . 1 ?
O5A S1 O6 150.4(3) 2 1 ?
O6 S1 O6 41.5(3) 2 1 ?
O6 S1 O6 0.0(4) . 1 ?
O5A S1 O5 114.8(3) 1 2 ?
O5A S1 O5 114.8(3) . 2 ?
O5A S1 O5 37.7(2) 2 2 ?
O6 S1 O5 94.6(3) 2 2 ?
O6 S1 O5 114.4(3) . 2 ?
O6 S1 O5 114.4(3) 1 2 ?
O5A S1 O5 37.7(2) 1 . ?
O5A S1 O5 37.7(2) . . ?
O5A S1 O5 114.8(3) 2 . ?
O6 S1 O5 114.4(3) 2 . ?
O6 S1 O5 94.6(3) . . ?
O6 S1 O5 94.6(3) 1 . ?
O5 S1 O5 149.4(4) 2 . ?
O5A S1 O5 37.7(2) 1 1 ?
O5A S1 O5 37.7(2) . 1 ?
O5A S1 O5 114.8(3) 2 1 ?
O6 S1 O5 114.4(3) 2 1 ?
O6 S1 O5 94.6(3) . 1 ?
O6 S1 O5 94.6(3) 1 1 ?
O5 S1 O5 149.4(4) 2 1 ?
O5 S1 O5 0.0(4) . 1 ?
O5A S1 O4 80.1(3) 1 . ?
O5A S1 O4 80.1(3) . . ?
O5A S1 O4 102.3(3) 2 . ?
O6 S1 O4 103.7(2) 2 . ?
O6 S1 O4 72.9(2) . . ?
O6 S1 O4 72.9(2) 1 . ?
O5 S1 O4 78.6(3) 2 . ?
O5 S1 O4 102.4(3) . . ?
O5 S1 O4 102.4(3) 1 . ?
O5A S1 O4 80.1(3) 1 1 ?
O5A S1 O4 80.1(3) . 1 ?
O5A S1 O4 102.3(3) 2 1 ?
O6 S1 O4 103.7(2) 2 1 ?
O6 S1 O4 72.9(2) . 1 ?
O6 S1 O4 72.9(2) 1 1 ?
O5 S1 O4 78.6(3) 2 1 ?
O5 S1 O4 102.4(3) . 1 ?
O5 S1 O4 102.4(3) 1 1 ?
O4 S1 O4 0.0(4) . 1 ?
O5A S1 O4 102.3(3) 1 2 ?
O5A S1 O4 102.3(3) . 2 ?
O5A S1 O4 80.1(3) 2 2 ?
O6 S1 O4 72.9(2) 2 2 ?
O6 S1 O4 103.7(2) . 2 ?
O6 S1 O4 103.7(2) 1 2 ?
O5 S1 O4 102.4(3) 2 2 ?
O5 S1 O4 78.6(3) . 2 ?
O5 S1 O4 78.6(3) 1 2 ?
O4 S1 O4 176.6(3) . 2 ?
O4 S1 O4 176.6(3) 1 2 ?
F6 C15 C14 118.5(5) . . ?
F6 C15 C13 118.4(5) . . ?
C14 C15 C13 123.1(5) . . ?
F8 C14 C16 119.1(6) . . ?
F8 C14 C15 120.8(6) . . ?
C16 C14 C15 120.1(5) . . ?
O4 O4 S1 0(10) 1 . ?
O5A O5A O5 0(10) 1 1 ?
O5A O5A O5 0(10) 1 . ?
O5 O5A O5 0.0(9) 1 . ?
O5A O5A S1 0(10) 1 . ?
O5 O5A S1 72.8(5) 1 . ?
O5 O5A S1 72.8(5) . . ?
O5 O5 O5A 0(10) 1 1 ?
O5 O5 O5A 0(10) 1 . ?
O5A O5 O5A 0.0(7) 1 . ?
O5 O5 S1 0(10) 1 . ?
O5A O5 S1 69.5(4) 1 . ?
O5A O5 S1 69.5(4) . . ?
O6 O6 O6 0(10) 1 2 ?
O6 O6 S1 0(10) 1 . ?
O6 O6 S1 69.24(17) 2 . ?
C1 N1 C19 110.7(3) . . ?
C1 N1 C10 113.7(3) . . ?
C19 N1 C10 108.3(3) . . ?
C3 N2 C2 120.4(4) . . ?
C3 N2 H2C 117(4) . . ?
C2 N2 H2C 123(4) . . ?
C3 N3 C4 119.8(3) . . ?
C3 N3 H3C 119(3) . . ?
C4 N3 H3C 116(3) . . ?
C12 N4 C11 118.5(4) . . ?
C12 N4 H4C 120(3) . . ?
C11 N4 H4C 120(3) . . ?
C12 N5 C13 124.5(4) . . ?
C12 N5 H5C 123(4) . . ?
C13 N5 H5C 112(4) . . ?
C21 N6 C20 121.6(3) . . ?
C21 N6 H6C 116(3) . . ?
C20 N6 H6C 119(3) . . ?
C21 N7 C22 123.6(3) . . ?
C21 N7 H7C 117(3) . . ?
C22 N7 H7C 115(3) . . ?
C40 N8 C32 104.4(3) . . ?
C40 N8 C28 112.1(3) . . ?
C32 N8 C28 112.2(3) . . ?
C40 N8 C36 111.7(3) . . ?
C32 N8 C36 111.3(3) . . ?
C28 N8 C36 105.2(3) . . ?
N1 C1 C2 112.2(4) . . ?
N1 C1 H1A 109.2 . . ?
C2 C1 H1A 109.2 . . ?
N1 C1 H1B 109.2 . . ?
C2 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
N2 C2 C1 112.9(3) . . ?
N2 C2 H2A 109.0 . . ?
C1 C2 H2A 109.0 . . ?
N2 C2 H2B 109.0 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
O1 C3 N2 124.1(4) . . ?
O1 C3 N3 121.4(3) . . ?
N2 C3 N3 114.5(3) . . ?
C9 C4 N3 122.4(4) . . ?
C9 C4 C5 116.1(4) . . ?
N3 C4 C5 121.5(3) . . ?
F1 C5 C6 119.0(4) . . ?
F1 C5 C4 118.5(4) . . ?
C6 C5 C4 122.6(4) . . ?
F2 C6 C7 120.7(4) . . ?
F2 C6 C5 119.8(4) . . ?
C7 C6 C5 119.4(4) . . ?
F3 C7 C8 120.1(4) . . ?
F3 C7 C6 120.2(4) . . ?
C8 C7 C6 119.6(4) . . ?
F4 C8 C7 119.3(4) . . ?
F4 C8 C9 119.8(4) . . ?
C7 C8 C9 120.8(4) . . ?
F5 C9 C8 118.1(4) . . ?
F5 C9 C4 120.5(3) . . ?
C8 C9 C4 121.4(4) . . ?
N1 C10 C11 116.2(4) . . ?
N1 C10 H10A 108.2 . . ?
C11 C10 H10A 108.2 . . ?
N1 C10 H10B 108.2 . . ?
C11 C10 H10B 108.2 . . ?
H10A C10 H10B 107.4 . . ?
N4 C11 C10 114.1(4) . . ?
N4 C11 H11A 108.7 . . ?
C10 C11 H11A 108.7 . . ?
N4 C11 H11B 108.7 . . ?
C10 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
O2 C12 N4 123.4(4) . . ?
O2 C12 N5 121.4(4) . . ?
N4 C12 N5 115.2(4) . . ?
C18 C13 C15 115.9(4) . . ?
C18 C13 N5 123.4(4) . . ?
C15 C13 N5 120.6(4) . . ?
F7 C16 C14 121.6(5) . . ?
F7 C16 C17 119.4(6) . . ?
C14 C16 C17 118.9(5) . . ?
F9 C17 C16 119.2(4) . . ?
F9 C17 C18 120.4(4) . . ?
C16 C17 C18 120.4(4) . . ?
F10 C18 C13 120.8(4) . . ?
F10 C18 C17 117.6(4) . . ?
C13 C18 C17 121.5(4) . . ?
N1 C19 C20 112.0(3) . . ?
N1 C19 H19A 109.2 . . ?
C20 C19 H19A 109.2 . . ?
N1 C19 H19B 109.2 . . ?
C20 C19 H19B 109.2 . . ?
H19A C19 H19B 107.9 . . ?
N6 C20 C19 111.5(3) . . ?
N6 C20 H20A 109.3 . . ?
C19 C20 H20A 109.1 . . ?
N6 C20 H20B 109.6 . . ?
C19 C20 H20B 109.2 . . ?
H20A C20 H20B 108.1 . . ?
O3 C21 N6 125.4(4) . . ?
O3 C21 N7 121.2(4) . . ?
N6 C21 N7 113.3(3) . . ?
C27 C22 C23 117.1(4) . . ?
C27 C22 N7 120.1(4) . . ?
C23 C22 N7 122.6(4) . . ?
F11 C23 C24 119.3(4) . . ?
F11 C23 C22 119.5(4) . . ?
C24 C23 C22 121.1(4) . . ?
F12 C24 C23 119.9(4) . . ?
F12 C24 C25 119.2(4) . . ?
C23 C24 C25 121.0(4) . . ?
F13 C25 C24 120.5(4) . . ?
F13 C25 C26 120.4(4) . . ?
C24 C25 C26 119.1(4) . . ?
F14 C26 C27 120.5(4) . . ?
F14 C26 C25 119.9(4) . . ?
C27 C26 C25 119.6(4) . . ?
F15 C27 C26 118.7(4) . . ?
F15 C27 C22 119.2(4) . . ?
C26 C27 C22 122.1(4) . . ?
C29 C28 N8 116.3(3) . . ?
C29 C28 H28A 108.2 . . ?
N8 C28 H28A 108.2 . . ?
C29 C28 H28B 108.2 . . ?
N8 C28 H28B 108.2 . . ?
H28A C28 H28B 107.4 . . ?
C28 C29 C30 109.3(3) . . ?
C28 C29 H29A 109.8 . . ?
C30 C29 H29A 109.8 . . ?
C28 C29 H29B 109.8 . . ?
C30 C29 H29B 109.8 . . ?
H29A C29 H29B 108.3 . . ?
C31 C30 C29 112.4(3) . . ?
C31 C30 H30A 109.1 . . ?
C29 C30 H30A 109.1 . . ?
C31 C30 H30B 109.1 . . ?
C29 C30 H30B 109.1 . . ?
H30A C30 H30B 107.9 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C33 C32 N8 116.2(3) . . ?
C33 C32 H32A 108.2 . . ?
N8 C32 H32A 108.2 . . ?
C33 C32 H32B 108.2 . . ?
N8 C32 H32B 108.2 . . ?
H32A C32 H32B 107.4 . . ?
C32 C33 C34 108.6(3) . . ?
C32 C33 H33A 110.0 . . ?
C34 C33 H33A 110.0 . . ?
C32 C33 H33B 110.0 . . ?
C34 C33 H33B 110.0 . . ?
H33A C33 H33B 108.4 . . ?
C35 C34 C33 112.1(4) . . ?
C35 C34 H34A 109.2 . . ?
C33 C34 H34A 109.2 . . ?
C35 C34 H34B 109.2 . . ?
C33 C34 H34B 109.2 . . ?
H34A C34 H34B 107.9 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C37 C36 N8 116.1(3) . . ?
C37 C36 H36A 108.3 . . ?
N8 C36 H36A 108.3 . . ?
C37 C36 H36B 108.3 . . ?
N8 C36 H36B 108.3 . . ?
H36A C36 H36B 107.4 . . ?
C36 C37 C38 110.9(3) . . ?
C36 C37 H37A 109.5 . . ?
C38 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C38 C37 H37B 109.5 . . ?
H37A C37 H37B 108.1 . . ?
C39 C38 C37 112.6(4) . . ?
C39 C38 H38A 109.1 . . ?
C37 C38 H38A 109.1 . . ?
C39 C38 H38B 109.1 . . ?
C37 C38 H38B 109.1 . . ?
H38A C38 H38B 107.8 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N8 C40 C41 117.1(3) . . ?
N8 C40 H40A 108.0 . . ?
C41 C40 H40A 108.0 . . ?
N8 C40 H40B 108.0 . . ?
C41 C40 H40B 108.0 . . ?
H40A C40 H40B 107.3 . . ?
C40 C41 C42 110.3(3) . . ?
C40 C41 H41A 109.6 . . ?
C42 C41 H41A 109.6 . . ?
C40 C41 H41B 109.6 . . ?
C42 C41 H41B 109.6 . . ?
H41A C41 H41B 108.1 . . ?
C43 C42 C41 114.7(3) . . ?
C43 C42 H42A 108.6 . . ?
C41 C42 H42A 108.6 . . ?
C43 C42 H42B 108.6 . . ?
C41 C42 H42B 108.6 . . ?
H42A C42 H42B 107.6 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N7 H7C O5A 0.77(5) 2.13(5) 2.851(7) 156(4) 2
N7 H7C O4 0.77(5) 2.25(5) 2.852(6) 135(4) 2
N7 H7C O5A 0.77(5) 2.52(5) 3.217(6) 151(4) 1
N6 H6C O5A 0.84(4) 2.14(4) 2.962(6) 164(4) 1
N6 H6C O5 0.84(4) 2.25(4) 3.062(6) 163(4) 1
N5 H5C O6 0.75(5) 2.32(5) 3.001(6) 153(5) 1
N5 H5C O4 0.75(5) 2.07(5) 2.778(6) 158(5) 1
N4 H4C O5A 0.80(5) 2.44(5) 3.165(6) 152(4) 1
N4 H4C O5 0.80(5) 2.16(5) 2.958(6) 171(4) 1
N3 H3C O6 0.79(5) 2.12(5) 2.880(6) 164(4) 2
N3 H3C O6 0.79(5) 2.13(5) 2.905(6) 168(4) 1
N2 H2C O4 0.80(5) 2.26(5) 3.034(6) 163(5) 2
N2 H2C O5 0.80(5) 2.21(5) 2.892(7) 143(5) 1

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.171
_refine_diff_density_min         -1.035
_refine_diff_density_rms         0.066