#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:45:29 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178962 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/91/4119158.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4119158
loop_
_publ_author_name
'Natalie D. Suhan'
'Stephen J. Loeb'
'S. Holger Eichhorn'
_publ_contact_author
;
 Stephen J. Loeb
 Department of Chemistry and Biochemistry
 University of Windsor
 Windsor, Ontario, Canada
 N9B 3P4
 
;
_publ_contact_author_email       loeb@uwindsor.ca
_publ_contact_author_fax         '+ 519 973-7098 '
_publ_contact_author_phone       '+ 519 253-3000 ext 3529'
_publ_section_title
;
 Mesomorphic [2]Rotaxanes: Sheltering Ionic Cores with Interlocking
 Components
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              400
_journal_page_last               408
_journal_paper_doi               10.1021/ja309558p
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C74 H77 F12 N5 O29 S4'
_chemical_formula_weight         1856.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.939(3)
_cell_angle_beta                 90.035(3)
_cell_angle_gamma                91.766(3)
_cell_formula_units_Z            2
_cell_length_a                   12.442(3)
_cell_length_b                   16.488(4)
_cell_length_c                   20.443(5)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.5
_cell_measurement_theta_min      1.5
_cell_volume                     4049.9(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL XPREP'
_computing_molecular_graphics    'Bruker SHELXTL XP'
_computing_publication_material  'Bruker SHELXTL XCIF'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-1 CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            38473
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.231
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.863733
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            prism
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       orange
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.011
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1118
_refine_ls_number_reflns         14147
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0808
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0929P)²+16.0303P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2165
_refine_ls_wR_factor_ref         0.2277
_reflns_number_gt                11136
_reflns_number_total             14147
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja309558p_si_003.cif
_cod_data_source_block           NS4TT
_cod_original_cell_volume        4049.8(17)
_cod_database_code               4119158
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
O1 O 1.1673(3) 0.2114(2) 0.35049(19) 0.0395(9) Uani 1 1 d .
O2 O 1.1062(3) 0.1941(2) 0.44894(19) 0.0436(10) Uani 1 1 d .
O3 O 0.8571(3) 0.4120(2) 0.57942(19) 0.0467(10) Uani 1 1 d .
O4 O 0.7834(3) 0.4943(2) 0.52096(19) 0.0441(9) Uani 1 1 d .
N1 N 0.8994(3) 0.4029(2) 0.24645(18) 0.0224(8) Uani 1 1 d .
N2 N 0.5593(3) 0.1098(2) 0.02693(18) 0.0208(8) Uani 1 1 d .
C1 C 1.0439(4) 0.3460(3) 0.3546(2) 0.0242(10) Uani 1 1 d .
H1A H 1.0875 0.3254 0.3162 0.029 Uiso 1 1 calc R
C2 C 1.0439(4) 0.3069(3) 0.4079(2) 0.0249(10) Uani 1 1 d .
C3 C 0.9819(4) 0.3382(3) 0.4646(2) 0.0267(10) Uani 1 1 d .
H3A H 0.9826 0.3125 0.5012 0.032 Uiso 1 1 calc R
C4 C 0.9187(4) 0.4070(3) 0.4679(2) 0.0266(10) Uani 1 1 d .
C5 C 0.9183(4) 0.4450(3) 0.4149(2) 0.0260(10) Uani 1 1 d .
H5A H 0.8754 0.4924 0.4175 0.031 Uiso 1 1 calc R
C6 C 0.9809(4) 0.4141(3) 0.3577(2) 0.0237(10) Uani 1 1 d .
C7 C 1.1081(4) 0.2318(3) 0.4054(2) 0.0279(10) Uani 1 1 d .
C8 C 1.2409(5) 0.1438(4) 0.3456(3) 0.0454(14) Uani 1 1 d .
H8A H 1.2800 0.1344 0.3028 0.068 Uiso 1 1 calc R
H8B H 1.2003 0.0924 0.3471 0.068 Uiso 1 1 calc R
H8C H 1.2921 0.1589 0.3835 0.068 Uiso 1 1 calc R
C9 C 0.8515(4) 0.4368(3) 0.5296(3) 0.0345(12) Uani 1 1 d .
C10 C 0.7097(6) 0.5235(5) 0.5758(3) 0.0591(18) Uani 1 1 d .
H10A H 0.6629 0.5650 0.5648 0.089 Uiso 1 1 calc R
H10B H 0.7503 0.5495 0.6174 0.089 Uiso 1 1 calc R
H10C H 0.6658 0.4760 0.5824 0.089 Uiso 1 1 calc R
C11 C 0.9766(4) 0.4536(3) 0.2989(2) 0.0261(10) Uani 1 1 d .
H11A H 0.9526 0.5121 0.3147 0.031 Uiso 1 1 calc R
H11B H 1.0491 0.4548 0.2791 0.031 Uiso 1 1 calc R
C12 C 0.7940(4) 0.4013(3) 0.2595(2) 0.0280(10) Uani 1 1 d .
H12A H 0.7679 0.4360 0.3006 0.034 Uiso 1 1 calc R
C13 C 0.7230(4) 0.3503(3) 0.2147(2) 0.0277(10) Uani 1 1 d .
H13A H 0.6486 0.3497 0.2249 0.033 Uiso 1 1 calc R
C14 C 0.7603(3) 0.2995(3) 0.1541(2) 0.0205(9) Uani 1 1 d .
C15 C 0.8678(4) 0.3052(3) 0.1409(2) 0.0270(10) Uani 1 1 d .
H15A H 0.8953 0.2737 0.0989 0.032 Uiso 1 1 calc R
C16 C 0.9367(4) 0.3563(3) 0.1880(2) 0.0292(10) Uani 1 1 d .
H16A H 1.0115 0.3582 0.1788 0.035 Uiso 1 1 calc R
C17 C 0.6864(3) 0.2369(3) 0.1078(2) 0.0199(9) Uani 1 1 d .
C18 C 0.5762(4) 0.2332(3) 0.1164(2) 0.0240(10) Uani 1 1 d .
H18A H 0.5430 0.2757 0.1499 0.029 Uiso 1 1 calc R
C19 C 0.5140(4) 0.1681(3) 0.0765(2) 0.0259(10) Uani 1 1 d .
H19A H 0.4389 0.1646 0.0843 0.031 Uiso 1 1 calc R
C20 C 0.6646(4) 0.1150(3) 0.0156(2) 0.0258(10) Uani 1 1 d .
H20A H 0.6953 0.0743 -0.0206 0.031 Uiso 1 1 calc R
C21 C 0.7293(4) 0.1771(3) 0.0546(2) 0.0239(10) Uani 1 1 d .
H21A H 0.8040 0.1794 0.0453 0.029 Uiso 1 1 calc R
C22 C 0.4945(4) 0.0375(3) -0.0149(2) 0.0233(9) Uani 1 1 d .
H22A H 0.5205 0.0234 -0.0621 0.028 Uiso 1 1 calc R
H22B H 0.4181 0.0524 -0.0152 0.028 Uiso 1 1 calc R
O5 O 0.2179(2) 0.0033(2) -0.07532(16) 0.0268(7) Uani 1 1 d .
O6 O 0.2770(2) 0.0696(2) 0.06775(15) 0.0251(7) Uani 1 1 d .
O7 O 0.4103(2) 0.0544(2) 0.17335(16) 0.0270(7) Uani 1 1 d .
O8 O 0.3525(2) -0.0510(2) -0.17357(15) 0.0259(7) Uani 1 1 d .
C23 C 0.2502(3) -0.0823(3) -0.1838(2) 0.0223(9) Uani 1 1 d .
C24 C 0.2138(4) -0.1412(3) -0.2424(2) 0.0256(10) Uani 1 1 d .
H24A H 0.2621 -0.1612 -0.2785 0.031 Uiso 1 1 calc R
C25 C 0.1081(4) -0.1705(3) -0.2482(3) 0.0320(11) Uani 1 1 d .
H25A H 0.0848 -0.2103 -0.2885 0.038 Uiso 1 1 calc R
C26 C 0.0364(4) -0.1436(3) -0.1971(3) 0.0331(11) Uani 1 1 d .
H26A H -0.0360 -0.1644 -0.2016 0.040 Uiso 1 1 calc R
C27 C 0.0719(4) -0.0846(3) -0.1379(2) 0.0291(11) Uani 1 1 d .
H27A H 0.0230 -0.0653 -0.1020 0.035 Uiso 1 1 calc R
C28 C 0.1762(4) -0.0545(3) -0.1314(2) 0.0237(10) Uani 1 1 d .
C29 C 0.1439(4) 0.0398(3) -0.0232(2) 0.0293(11) Uani 1 1 d .
H29A H 0.1126 -0.0039 -0.0029 0.035 Uiso 1 1 calc R
H29B H 0.0846 0.0656 -0.0423 0.035 Uiso 1 1 calc R
C30 C 0.2048(4) 0.1056(3) 0.0296(2) 0.0277(10) Uani 1 1 d .
H30A H 0.2461 0.1430 0.0072 0.033 Uiso 1 1 calc R
H30B H 0.1531 0.1401 0.0607 0.033 Uiso 1 1 calc R
C31 C 0.2336(4) 0.0622(3) 0.1311(2) 0.0263(10) Uani 1 1 d .
H31A H 0.1623 0.0328 0.1233 0.032 Uiso 1 1 calc R
H31B H 0.2241 0.1188 0.1615 0.032 Uiso 1 1 calc R
C32 C 0.3079(4) 0.0141(3) 0.1633(2) 0.0262(10) Uani 1 1 d .
H32A H 0.2784 0.0100 0.2073 0.031 Uiso 1 1 calc R
H32B H 0.3140 -0.0435 0.1339 0.031 Uiso 1 1 calc R
C33 C 0.4766(4) 0.0200(3) 0.2157(2) 0.0273(10) Uani 1 1 d .
H33A H 0.4925 -0.0389 0.1924 0.033 Uiso 1 1 calc R
H33B H 0.4383 0.0201 0.2582 0.033 Uiso 1 1 calc R
C34 C 0.4215(3) -0.0705(3) -0.2315(2) 0.0254(10) Uani 1 1 d .
H34A H 0.3853 -0.0578 -0.2707 0.030 Uiso 1 1 calc R
H34B H 0.4370 -0.1311 -0.2436 0.030 Uiso 1 1 calc R
O101 O -0.3985(3) 0.7997(2) 0.0567(2) 0.0448(10) Uani 1 1 d .
O102 O -0.3445(3) 0.7697(2) 0.15212(18) 0.0357(8) Uani 1 1 d .
O103 O -0.6237(3) 0.5756(2) -0.10260(18) 0.0432(9) Uani 1 1 d .
O104 O -0.7252(3) 0.4914(2) -0.05619(19) 0.0437(9) Uani 1 1 d .
N101 N -0.6632(3) 0.5907(2) 0.23969(18) 0.0230(8) Uani 1 1 d .
N102 N -0.9563(3) 0.8879(2) 0.47135(18) 0.0205(8) Uani 1 1 d .
C101 C -0.5255(4) 0.6484(3) 0.0239(2) 0.0266(10) Uani 1 1 d .
H10D H -0.5100 0.6734 -0.0122 0.032 Uiso 1 1 calc R
C102 C -0.4962(4) 0.6425(3) 0.1388(2) 0.0247(10) Uani 1 1 d .
H10E H -0.4595 0.6627 0.1809 0.030 Uiso 1 1 calc R
C103 C -0.4756(4) 0.6798(3) 0.0863(2) 0.0254(10) Uani 1 1 d .
C104 C -0.5979(4) 0.5805(3) 0.0138(2) 0.0268(10) Uani 1 1 d .
C105 C -0.6210(4) 0.5452(3) 0.0671(2) 0.0257(10) Uani 1 1 d .
H10F H -0.6719 0.4997 0.0606 0.031 Uiso 1 1 calc R
C106 C -0.5707(4) 0.5755(3) 0.1298(2) 0.0228(9) Uani 1 1 d .
C107 C -0.4028(4) 0.7562(3) 0.0956(2) 0.0287(10) Uani 1 1 d .
C108 C -0.2722(4) 0.8427(4) 0.1663(3) 0.0425(13) Uani 1 1 d .
H10G H -0.2335 0.8469 0.2089 0.064 Uiso 1 1 calc R
H10H H -0.3136 0.8933 0.1702 0.064 Uiso 1 1 calc R
H10I H -0.2205 0.8372 0.1294 0.064 Uiso 1 1 calc R
C109 C -0.6487(4) 0.5503(3) -0.0545(3) 0.0311(11) Uani 1 1 d .
C110 C -0.7830(6) 0.4607(4) -0.1200(3) 0.0610(18) Uani 1 1 d .
H11C H -0.8373 0.4182 -0.1156 0.092 Uiso 1 1 calc R
H11D H -0.7323 0.4357 -0.1556 0.092 Uiso 1 1 calc R
H11E H -0.8182 0.5075 -0.1317 0.092 Uiso 1 1 calc R
C111 C -0.5949(4) 0.5358(3) 0.1871(2) 0.0280(10) Uani 1 1 d .
H11F H -0.6326 0.4808 0.1690 0.034 Uiso 1 1 calc R
H11G H -0.5265 0.5258 0.2082 0.034 Uiso 1 1 calc R
C112 C -0.6190(4) 0.6322(3) 0.2996(2) 0.0305(11) Uani 1 1 d .
H11H H -0.5458 0.6247 0.3091 0.037 Uiso 1 1 calc R
C113 C -0.6795(4) 0.6852(3) 0.3468(2) 0.0281(10) Uani 1 1 d .
H11I H -0.6473 0.7147 0.3886 0.034 Uiso 1 1 calc R
C114 C -0.7862(4) 0.6966(3) 0.3350(2) 0.0217(9) Uani 1 1 d .
C115 C -0.8302(4) 0.6513(3) 0.2730(2) 0.0261(10) Uani 1 1 d .
H11J H -0.9035 0.6573 0.2626 0.031 Uiso 1 1 calc R
C116 C -0.7670(4) 0.5979(3) 0.2271(2) 0.0270(10) Uani 1 1 d .
H11K H -0.7979 0.5657 0.1857 0.032 Uiso 1 1 calc R
C117 C -0.8503(4) 0.7594(3) 0.3845(2) 0.0207(9) Uani 1 1 d .
C118 C -0.8018(4) 0.8074(3) 0.4438(2) 0.0283(10) Uani 1 1 d .
H11L H -0.7311 0.7958 0.4555 0.034 Uiso 1 1 calc R
C119 C -0.8562(4) 0.8716(3) 0.4852(2) 0.0278(10) Uani 1 1 d .
H11M H -0.8215 0.9051 0.5249 0.033 Uiso 1 1 calc R
C120 C -1.0084(4) 0.8401(3) 0.4167(2) 0.0265(10) Uani 1 1 d .
H12B H -1.0808 0.8510 0.4078 0.032 Uiso 1 1 calc R
C121 C -0.9565(4) 0.7751(3) 0.3735(2) 0.0275(10) Uani 1 1 d .
H12C H -0.9943 0.7406 0.3355 0.033 Uiso 1 1 calc R
C122 C -1.0087(4) 0.9624(3) 0.5149(2) 0.0231(9) Uani 1 1 d .
H12D H -0.9778 0.9755 0.5612 0.028 Uiso 1 1 calc R
H12E H -1.0867 0.9501 0.5178 0.028 Uiso 1 1 calc R
O105 O -1.2783(2) 1.0149(2) 0.57760(16) 0.0267(7) Uani 1 1 d .
O106 O -1.2310(2) 0.9411(2) 0.43378(15) 0.0256(7) Uani 1 1 d .
O107 O -1.0997(2) 0.9394(2) 0.32158(16) 0.0268(7) Uani 1 1 d .
O108 O -1.1406(2) 1.0601(2) 0.67787(15) 0.0253(7) Uani 1 1 d .
C123 C -1.2403(3) 1.0932(3) 0.6889(2) 0.0224(9) Uani 1 1 d .
C124 C -1.2715(4) 1.1490(3) 0.7493(2) 0.0274(10) Uani 1 1 d .
H12F H -1.2217 1.1662 0.7859 0.033 Uiso 1 1 calc R
C125 C -1.3738(4) 1.1789(3) 0.7560(3) 0.0329(11) Uani 1 1 d .
H12G H -1.3949 1.2150 0.7979 0.039 Uiso 1 1 calc R
C126 C -1.4461(4) 1.1574(3) 0.7031(3) 0.0325(11) Uani 1 1 d .
H12H H -1.5157 1.1802 0.7076 0.039 Uiso 1 1 calc R
C127 C -1.4161(4) 1.1018(3) 0.6426(3) 0.0300(11) Uani 1 1 d .
H12I H -1.4662 1.0857 0.6061 0.036 Uiso 1 1 calc R
C128 C -1.3150(4) 1.0700(3) 0.6353(2) 0.0242(10) Uani 1 1 d .
C129 C -1.3573(4) 0.9779(3) 0.5271(2) 0.0269(10) Uani 1 1 d .
H12J H -1.3841 1.0208 0.5055 0.032 Uiso 1 1 calc R
H12K H -1.4190 0.9548 0.5479 0.032 Uiso 1 1 calc R
C130 C -1.3053(4) 0.9086(3) 0.4749(2) 0.0273(10) Uani 1 1 d .
H13B H -1.2669 0.8721 0.4981 0.033 Uiso 1 1 calc R
H13C H -1.3618 0.8738 0.4455 0.033 Uiso 1 1 calc R
C131 C -1.2740(4) 0.9409(3) 0.3694(2) 0.0272(10) Uani 1 1 d .
H13D H -1.3426 0.9706 0.3751 0.033 Uiso 1 1 calc R
H13E H -1.2886 0.8823 0.3427 0.033 Uiso 1 1 calc R
C132 C -1.1958(4) 0.9832(3) 0.3329(2) 0.0268(10) Uani 1 1 d .
H13F H -1.2273 0.9857 0.2890 0.032 Uiso 1 1 calc R
H13G H -1.1806 1.0414 0.3600 0.032 Uiso 1 1 calc R
C133 C -1.0282(4) 0.9737(3) 0.2808(2) 0.0298(11) Uani 1 1 d .
H13H H -1.0067 1.0320 0.3052 0.036 Uiso 1 1 calc R
H13I H -1.0654 0.9754 0.2384 0.036 Uiso 1 1 calc R
C134 C -1.0696(4) 1.0775(3) 0.7358(2) 0.0303(11) Uani 1 1 d .
H13J H -1.1070 1.0639 0.7745 0.036 Uiso 1 1 calc R
H13K H -1.0485 1.1379 0.7488 0.036 Uiso 1 1 calc R
S1 S 1.26812(10) 0.33441(8) 0.20281(7) 0.0330(3) Uani 1 1 d .
F1 F 1.4509(3) 0.3696(2) 0.2669(2) 0.0597(10) Uani 1 1 d .
F2 F 1.4100(3) 0.2385(2) 0.23620(18) 0.0555(9) Uani 1 1 d .
F3 F 1.3314(3) 0.3169(2) 0.32085(17) 0.0516(9) Uani 1 1 d .
O9 O 1.3292(3) 0.3293(3) 0.1423(2) 0.0475(10) Uani 1 1 d .
O10 O 1.1870(3) 0.2697(2) 0.1991(2) 0.0486(10) Uani 1 1 d .
O11 O 1.2348(3) 0.4174(2) 0.2366(2) 0.0429(9) Uani 1 1 d .
C35 C 1.3697(4) 0.3141(3) 0.2600(3) 0.0387(13) Uani 1 1 d .
S2 S 0.58117(10) 0.17849(8) 0.42626(6) 0.0300(3) Uani 1 1 d .
F4 F 0.6010(5) 0.2948(3) 0.3621(2) 0.0962(16) Uani 1 1 d .
F5 F 0.4826(5) 0.3183(3) 0.4394(3) 0.107(2) Uani 1 1 d .
F6 F 0.6486(5) 0.3332(3) 0.4665(3) 0.1111(19) Uani 1 1 d .
O12 O 0.5600(3) 0.1817(3) 0.49614(18) 0.0440(9) Uani 1 1 d .
O13 O 0.4988(3) 0.1381(3) 0.3797(2) 0.0593(12) Uani 1 1 d .
O14 O 0.6870(3) 0.1562(3) 0.4056(2) 0.0507(11) Uani 1 1 d .
C36 C 0.5782(6) 0.2874(4) 0.4240(4) 0.0590(18) Uani 1 1 d .
S101 S 0.06074(9) 0.80021(8) 0.07047(6) 0.0276(3) Uani 1 1 d .
F101 F 0.1957(3) 0.6843(3) 0.0157(2) 0.0718(12) Uani 1 1 d .
F102 F 0.1670(4) 0.6958(2) 0.12157(19) 0.0685(11) Uani 1 1 d .
F103 F 0.0490(4) 0.6369(2) 0.0476(2) 0.0783(13) Uani 1 1 d .
O109 O 0.0238(3) 0.7934(2) 0.00233(17) 0.0327(8) Uani 1 1 d .
O110 O -0.0229(3) 0.8021(3) 0.1189(2) 0.0478(10) Uani 1 1 d .
O111 O 0.1483(3) 0.8587(2) 0.09229(19) 0.0438(9) Uani 1 1 d .
C135 C 0.1213(5) 0.6986(4) 0.0636(3) 0.0414(13) Uani 1 1 d .
S102 S -0.28215(15) 0.63950(12) 0.31346(9) 0.0616(5) Uani 1 1 d .
F104 F -0.3235(11) 0.5828(6) 0.4136(4) 0.222(5) Uani 1 1 d .
F105 F -0.4020(6) 0.6935(4) 0.4168(3) 0.124(2) Uani 1 1 d .
F106 F -0.2464(8) 0.6986(7) 0.4393(5) 0.232(6) Uani 1 1 d .
O112 O -0.3678(5) 0.5983(8) 0.2805(3) 0.183(6) Uani 1 1 d .
O113 O -0.1864(4) 0.5972(4) 0.3026(4) 0.097(2) Uani 1 1 d .
O114 O -0.2624(11) 0.7244(6) 0.3107(6) 0.220(7) Uani 1 1 d .
C136 C -0.3136(9) 0.6554(6) 0.3995(4) 0.089(3) Uani 1 1 d .
N1S N -0.0978(5) 0.5481(4) -0.0984(3) 0.0635(15) Uani 1 1 d .
C1S C -0.1386(5) 0.6002(4) -0.0591(3) 0.0481(15) Uani 1 1 d .
C2S C -0.1929(5) 0.6649(4) -0.0113(3) 0.0513(15) Uani 1 1 d .
H2SA H -0.1401 0.7075 0.0129 0.077 Uiso 1 1 calc R
H2SB H -0.2314 0.6405 0.0212 0.077 Uiso 1 1 calc R
H2SC H -0.2443 0.6911 -0.0353 0.077 Uiso 1 1 calc R
O1W O -0.0636(4) 0.7042(4) 0.2186(3) 0.0784(15) Uani 1 1 d .
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_3
C7 O1 C8 117.0(4) .
C9 O4 C10 115.4(5) .
C16 N1 C12 120.0(4) .
C16 N1 C11 119.7(4) .
C12 N1 C11 120.1(4) .
C20 N2 C19 120.0(4) .
C20 N2 C22 118.9(4) .
C19 N2 C22 121.1(4) .
C6 C1 C2 120.3(4) .
C3 C2 C1 119.7(4) .
C3 C2 C7 118.5(4) .
C1 C2 C7 121.8(4) .
C2 C3 C4 120.1(4) .
C5 C4 C3 120.1(4) .
C5 C4 C9 122.2(4) .
C3 C4 C9 117.7(4) .
C4 C5 C6 120.3(4) .
C1 C6 C5 119.6(4) .
C1 C6 C11 120.4(4) .
C5 C6 C11 120.0(4) .
O2 C7 O1 124.2(4) .
O2 C7 C2 123.7(4) .
O1 C7 C2 112.1(4) .
O3 C9 O4 124.7(5) .
O3 C9 C4 124.7(5) .
O4 C9 C4 110.6(4) .
N1 C11 C6 108.9(4) .
N1 C12 C13 121.2(4) .
C12 C13 C14 119.9(4) .
C15 C14 C13 117.5(4) .
C15 C14 C17 121.6(4) .
C13 C14 C17 120.7(4) .
C14 C15 C16 120.6(4) .
N1 C16 C15 120.7(4) .
C18 C17 C21 117.2(4) .
C18 C17 C14 123.5(4) .
C21 C17 C14 119.2(4) .
C17 C18 C19 120.6(4) .
N2 C19 C18 120.2(4) .
N2 C20 C21 121.7(4) .
C20 C21 C17 120.2(4) .
N2 C22 C22 108.9(4) 2_655
C28 O5 C29 117.0(3) .
C30 O6 C31 113.4(3) .
C32 O7 C33 111.6(3) .
C23 O8 C34 116.0(3) .
O8 C23 C24 124.5(4) .
O8 C23 C28 117.5(4) .
C24 C23 C28 118.0(4) .
C25 C24 C23 120.6(4) .
C26 C25 C24 121.3(5) .
C25 C26 C27 118.7(4) .
C28 C27 C26 120.7(5) .
C27 C28 O5 124.7(4) .
C27 C28 C23 120.6(4) .
O5 C28 C23 114.7(4) .
O5 C29 C30 107.7(4) .
O6 C30 C29 112.2(4) .
O6 C31 C32 109.7(4) .
O7 C32 C31 110.3(4) .
O7 C33 C34 109.7(4) 2_655
O8 C34 C33 109.4(4) 2_655
C107 O102 C108 116.1(4) .
C109 O104 C110 116.1(4) .
C116 N101 C112 120.5(4) .
C116 N101 C111 120.0(4) .
C112 N101 C111 119.6(4) .
C119 N102 C120 120.5(4) .
C119 N102 C122 119.5(4) .
C120 N102 C122 119.9(4) .
C103 C101 C104 120.3(4) .
C103 C102 C106 120.1(4) .
C101 C103 C102 120.1(4) .
C101 C103 C107 118.1(4) .
C102 C103 C107 121.7(4) .
C101 C104 C105 119.3(4) .
C101 C104 C109 117.3(4) .
C105 C104 C109 123.4(4) .
C104 C105 C106 121.1(4) .
C105 C106 C102 119.0(4) .
C105 C106 C111 120.7(4) .
C102 C106 C111 120.3(4) .
O101 C107 O102 124.5(5) .
O101 C107 C103 123.8(5) .
O102 C107 C103 111.7(4) .
O103 C109 O104 123.8(5) .
O103 C109 C104 124.2(5) .
O104 C109 C104 112.0(4) .
N101 C111 C106 111.4(4) .
N101 C112 C113 120.0(4) .
C112 C113 C114 121.4(5) .
C113 C114 C115 117.2(4) .
C113 C114 C117 121.3(4) .
C115 C114 C117 121.4(4) .
C116 C115 C114 119.7(4) .
N101 C116 C115 121.1(4) .
C121 C117 C118 116.9(4) .
C121 C117 C114 123.2(4) .
C118 C117 C114 119.8(4) .
C119 C118 C117 119.9(4) .
N102 C119 C118 121.5(4) .
N102 C120 C121 119.8(4) .
C120 C121 C117 121.1(4) .
N102 C122 C122 109.6(4) 2_376
C128 O105 C129 116.4(3) .
C131 O106 C130 113.2(3) .
C132 O107 C133 111.3(3) .
C123 O108 C134 115.9(3) .
O108 C123 C124 124.2(4) .
O108 C123 C128 117.1(4) .
C124 C123 C128 118.6(4) .
C125 C124 C123 120.3(5) .
C124 C125 C126 121.0(5) .
C125 C126 C127 119.2(5) .
C128 C127 C126 120.6(5) .
C127 C128 O105 124.7(4) .
C127 C128 C123 120.2(4) .
O105 C128 C123 115.1(4) .
O105 C129 C130 108.0(4) .
O106 C130 C129 111.9(4) .
O106 C131 C132 109.6(4) .
O107 C132 C131 110.5(4) .
O107 C133 C134 110.9(4) 2_376
O108 C134 C133 109.8(4) 2_376
O10 S1 O9 116.0(3) .
O10 S1 O11 114.3(2) .
O9 S1 O11 114.8(2) .
O10 S1 C35 104.7(3) .
O9 S1 C35 101.7(2) .
O11 S1 C35 103.0(2) .
F3 C35 F1 108.2(5) .
F3 C35 F2 107.0(5) .
F1 C35 F2 107.1(4) .
F3 C35 S1 112.6(4) .
F1 C35 S1 110.6(4) .
F2 C35 S1 111.1(4) .
O14 S2 O13 114.9(3) .
O14 S2 O12 114.2(2) .
O13 S2 O12 115.1(2) .
O14 S2 C36 102.9(3) .
O13 S2 C36 104.0(3) .
O12 S2 C36 103.5(3) .
F6 C36 F5 108.5(6) .
F6 C36 F4 108.4(7) .
F5 C36 F4 107.3(6) .
F6 C36 S2 110.8(5) .
F5 C36 S2 111.4(6) .
F4 C36 S2 110.3(5) .
O111 S101 O110 115.6(2) .
O111 S101 O109 114.5(2) .
O110 S101 O109 114.8(2) .
O111 S101 C135 103.2(3) .
O110 S101 C135 103.3(3) .
O109 S101 C135 102.9(2) .
F103 C135 F102 107.6(5) .
F103 C135 F101 107.6(5) .
F102 C135 F101 108.4(5) .
F103 C135 S101 111.3(4) .
F102 C135 S101 111.2(4) .
F101 C135 S101 110.6(4) .
O112 S102 O113 115.8(5) .
O112 S102 O114 117.9(8) .
O113 S102 O114 109.0(6) .
O112 S102 C136 104.6(5) .
O113 S102 C136 107.4(5) .
O114 S102 C136 100.2(6) .
F106 C136 F105 103.5(9) .
F106 C136 F104 107.6(11) .
F105 C136 F104 106.9(10) .
F106 C136 S102 114.9(10) .
F105 C136 S102 114.2(7) .
F104 C136 S102 109.2(7) .
N1S C1S C2S 178.1(7) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 C7 1.318(6) .
O1 C8 1.448(6) .
O2 C7 1.210(6) .
O3 C9 1.194(6) .
O4 C9 1.335(6) .
O4 C10 1.442(7) .
N1 C16 1.336(6) .
N1 C12 1.339(6) .
N1 C11 1.503(6) .
N2 C20 1.335(6) .
N2 C19 1.342(6) .
N2 C22 1.488(6) .
C1 C6 1.377(6) .
C1 C2 1.402(6) .
C2 C3 1.386(6) .
C2 C7 1.483(7) .
C3 C4 1.387(7) .
C4 C5 1.384(7) .
C4 C9 1.497(7) .
C5 C6 1.397(7) .
C6 C11 1.509(6) .
C12 C13 1.371(7) .
C13 C14 1.393(6) .
C14 C15 1.370(6) .
C14 C17 1.498(6) .
C15 C16 1.381(7) .
C17 C18 1.383(6) .
C17 C21 1.386(6) .
C18 C19 1.383(6) .
C20 C21 1.364(6) .
C22 C22 1.523(9) 2_655
O5 C28 1.378(6) .
O5 C29 1.432(5) .
O6 C30 1.427(6) .
O6 C31 1.435(5) .
O7 C32 1.409(5) .
O7 C33 1.426(5) .
O8 C23 1.354(5) .
O8 C34 1.438(5) .
C23 C24 1.397(6) .
C23 C28 1.407(6) .
C24 C25 1.381(7) .
C25 C26 1.367(7) .
C26 C27 1.404(7) .
C27 C28 1.369(6) .
C29 C30 1.503(7) .
C31 C32 1.493(7) .
C33 C34 1.484(7) 2_655
C34 C33 1.484(7) 2_655
O101 C107 1.201(6) .
O102 C107 1.329(6) .
O102 C108 1.447(6) .
O103 C109 1.200(6) .
O104 C109 1.333(6) .
O104 C110 1.452(7) .
N101 C116 1.331(6) .
N101 C112 1.347(6) .
N101 C111 1.499(6) .
N102 C119 1.327(6) .
N102 C120 1.344(6) .
N102 C122 1.488(5) .
C101 C103 1.386(7) .
C101 C104 1.388(7) .
C102 C103 1.388(6) .
C102 C106 1.396(6) .
C103 C107 1.498(7) .
C104 C105 1.387(7) .
C104 C109 1.489(7) .
C105 C106 1.390(7) .
C106 C111 1.508(6) .
C112 C113 1.366(7) .
C113 C114 1.376(7) .
C114 C115 1.396(6) .
C114 C117 1.497(6) .
C115 C116 1.375(6) .
C117 C121 1.384(7) .
C117 C118 1.391(6) .
C118 C119 1.371(7) .
C120 C121 1.378(7) .
C122 C122 1.528(9) 2_376
O105 C128 1.378(5) .
O105 C129 1.429(5) .
O106 C131 1.420(5) .
O106 C130 1.431(5) .
O107 C132 1.405(5) .
O107 C133 1.420(6) .
O108 C123 1.366(5) .
O108 C134 1.440(5) .
C123 C124 1.400(6) .
C123 C128 1.403(6) .
C124 C125 1.373(7) .
C125 C126 1.375(8) .
C126 C127 1.395(7) .
C127 C128 1.371(7) .
C129 C130 1.511(7) .
C131 C132 1.489(7) .
C133 C134 1.491(7) 2_376
C134 C133 1.491(7) 2_376
S1 O10 1.434(4) .
S1 O9 1.438(4) .
S1 O11 1.439(4) .
S1 C35 1.817(6) .
F1 C35 1.324(6) .
F2 C35 1.329(6) .
F3 C35 1.323(6) .
S2 O14 1.414(4) .
S2 O13 1.424(4) .
S2 O12 1.440(4) .
S2 C36 1.810(7) .
F4 C36 1.332(8) .
F5 C36 1.314(8) .
F6 C36 1.309(9) .
S101 O111 1.424(4) .
S101 O110 1.432(4) .
S101 O109 1.442(4) .
S101 C135 1.830(6) .
F101 C135 1.329(7) .
F102 C135 1.327(6) .
F103 C135 1.312(7) .
S102 O112 1.330(8) .
S102 O113 1.388(5) .
S102 O114 1.429(9) .
S102 C136 1.756(9) .
F104 C136 1.305(12) .
F105 C136 1.287(11) .
F106 C136 1.238(11) .
N1S C1S 1.146(8) .
C1S C2S 1.434(9) .
