#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:00:53 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178929 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/58/4115891.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_4115891
loop_
_publ_author_name
'Jaheon Kim'
'In-Sun Jung'
'Soo-Young Kim'
'Eunsung Lee'
'Jin-Koo Kang'
'Shigeru Sakamoto'
'Kentaro Yamaguchi'
'Kimoon Kim'
_publ_contact_author
;
Kimoon Kim
National Creative Research Initiative Center
for Smart Supramolecules and Department of Chemistry,
Pohang University of Science and Technology
San 31 Hyojadong, Pohang 790-784,South Korea
;
_publ_contact_author_email       kkim@postech.ac.kr
_publ_contact_author_fax         '82 562 279 8129'
_publ_contact_author_phone       '82 562 279 2113'
_publ_section_title
;
 New Cucurbituril Homologues: Syntheses, Isolation, Characterization, and
 X-ray Crystal Structures of Cucurbit[n]uril (n= 5, 7, and 8)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              540
_journal_page_last               541
_journal_paper_doi               10.1021/ja993376p
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C80 H144 Cl2 N40 O50 S'
_chemical_formula_weight         2569.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.9620(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.8327(3)
_cell_length_b                   18.5925(2)
_cell_length_c                   22.4398(6)
_cell_measurement_reflns_used    5786
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      24.08
_cell_measurement_theta_min      1.85
_cell_volume                     5700.7(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker XP in SHELXTL'
_computing_publication_material  'Bruker XCIF in SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       'omega and phi scana'
_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  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22492
_diffrn_reflns_theta_full        24.08
_diffrn_reflns_theta_max         24.08
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.186
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_description       block
_exptl_crystal_F_000             2708
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.723
_refine_diff_density_min         -1.001
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       0.0048(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1055
_refine_ls_number_reflns         8887
_refine_ls_number_restraints     226
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1255
_refine_ls_R_factor_gt           0.1023
_refine_ls_shift/su_max          0.536
_refine_ls_shift/su_mean         0.034
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1808P)²+11.3868P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2811
_refine_ls_wR_factor_ref         0.3113
_reflns_number_gt                6744
_reflns_number_total             8887
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja993376p_1.cif
_cod_data_source_block           2
_cod_database_code               4115891
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
O1 O 0.5758(2) 0.3385(2) 0.23505(15) 0.0589(9) Uani 1 1 d . . .
O2 O 0.5253(3) 0.5344(2) 0.2565(2) 0.0894(14) Uani 1 1 d . . .
O3 O 0.3550(3) 0.69230(19) 0.17208(16) 0.0606(9) Uani 1 1 d . . .
O4 O 0.1784(3) 0.7122(2) 0.02962(17) 0.0702(11) Uani 1 1 d . . .
O5 O 0.8992(3) 0.4299(2) 0.09444(16) 0.0711(11) Uani 1 1 d . . .
O6 O 0.8699(3) 0.6299(3) 0.1318(2) 0.0963(16) Uani 1 1 d . . .
O7 O 0.7008(3) 0.7733(2) 0.04335(17) 0.0638(10) Uani 1 1 d . . .
O8 O 0.5171(3) 0.7890(3) -0.10810(17) 0.0852(14) Uani 1 1 d . . .
N1 N 0.7093(3) 0.2954(2) 0.19565(17) 0.0496(9) Uani 1 1 d . . .
N2 N 0.7244(3) 0.3984(2) 0.24662(17) 0.0501(9) Uani 1 1 d . . .
N3 N 0.6923(3) 0.5251(2) 0.26035(17) 0.0531(10) Uani 1 1 d . . .
N4 N 0.6211(3) 0.6309(2) 0.23812(18) 0.0537(10) Uani 1 1 d . . .
N5 N 0.5188(3) 0.7242(2) 0.18502(17) 0.0509(10) Uani 1 1 d . . .
N6 N 0.4140(3) 0.7859(2) 0.11984(16) 0.0509(10) Uani 1 1 d . . .
N7 N 0.3020(3) 0.7944(2) 0.02495(17) 0.0502(10) Uani 1 1 d . . .
N8 N 0.2178(3) 0.7541(2) -0.06056(17) 0.0559(10) Uani 1 1 d . . .
N9 N 0.8383(3) 0.3319(2) 0.13959(17) 0.0540(10) Uani 1 1 d . . .
N10 N 0.8502(3) 0.4366(2) 0.18815(17) 0.0502(9) Uani 1 1 d . . .
N11 N 0.8261(3) 0.5622(2) 0.2093(2) 0.0581(11) Uani 1 1 d . . .
N12 N 0.7594(3) 0.6703(2) 0.19120(19) 0.0585(11) Uani 1 1 d . . .
N13 N 0.6576(3) 0.7629(2) 0.13824(19) 0.0566(10) Uani 1 1 d . . .
N14 N 0.5495(3) 0.8108(2) 0.06451(16) 0.0514(10) Uani 1 1 d . . .
N15 N 0.4376(3) 0.8217(2) -0.02904(17) 0.0547(10) Uani 1 1 d . . .
N16 N 0.3495(3) 0.7880(2) -0.11575(16) 0.0528(10) Uani 1 1 d . . .
C1 C 0.6610(3) 0.3437(3) 0.22648(19) 0.0459(11) Uani 1 1 d . . .
C2 C 0.7011(4) 0.4540(3) 0.2873(2) 0.0561(12) Uani 1 1 d . . .
H2A H 0.7523 0.4551 0.3227 0.067 Uiso 1 1 calc R . .
H2B H 0.6393 0.4418 0.3010 0.067 Uiso 1 1 calc R . .
C3 C 0.6046(4) 0.5612(3) 0.2522(2) 0.0555(12) Uani 1 1 d . . .
C4 C 0.5472(4) 0.6859(3) 0.2416(2) 0.0603(13) Uani 1 1 d . . .
H4A H 0.4891 0.6632 0.2534 0.072 Uiso 1 1 calc R . .
H4B H 0.5726 0.7205 0.2731 0.072 Uiso 1 1 calc R . .
C5 C 0.4218(4) 0.7302(3) 0.1596(2) 0.0486(11) Uani 1 1 d . . .
C6 C 0.3206(4) 0.8123(3) 0.0887(2) 0.0546(12) Uani 1 1 d . . .
H6A H 0.2680 0.7922 0.1082 0.066 Uiso 1 1 calc R . .
H6B H 0.3189 0.8647 0.0930 0.066 Uiso 1 1 calc R . .
C7 C 0.2278(3) 0.7501(3) 0.0009(2) 0.0531(12) Uani 1 1 d . . .
C8 C 0.1343(4) 0.7231(3) -0.0996(2) 0.0636(14) Uani 1 1 d . . .
H8A H 0.0895 0.7022 -0.0745 0.076 Uiso 1 1 calc R . .
H8B H 0.0992 0.7616 -0.1238 0.076 Uiso 1 1 calc R . .
C9 C 0.8121(3) 0.3138(3) 0.19789(19) 0.0469(11) Uani 1 1 d . . .
H9A H 0.8559 0.2766 0.2190 0.056 Uiso 1 1 calc R . .
C10 C 0.8216(3) 0.3862(3) 0.2320(2) 0.0484(11) Uani 1 1 d . . .
H10A H 0.8713 0.3837 0.2688 0.058 Uiso 1 1 calc R . .
C11 C 0.7735(3) 0.5732(3) 0.2596(2) 0.0526(11) Uani 1 1 d . . .
H11A H 0.8181 0.5731 0.2986 0.063 Uiso 1 1 calc R . .
C12 C 0.7250(4) 0.6468(3) 0.2462(2) 0.0543(12) Uani 1 1 d . . .
H12A H 0.7441 0.6810 0.2797 0.065 Uiso 1 1 calc R . .
C13 C 0.5767(4) 0.7836(3) 0.1684(2) 0.0524(12) Uani 1 1 d . . .
H13A H 0.5984 0.8156 0.2032 0.063 Uiso 1 1 calc R . .
C14 C 0.5050(3) 0.8229(3) 0.11844(19) 0.0484(11) Uani 1 1 d . . .
H14A H 0.4997 0.8748 0.1273 0.058 Uiso 1 1 calc R . .
C15 C 0.3377(3) 0.8371(3) -0.0200(2) 0.0484(11) Uani 1 1 d . . .
H15A H 0.3282 0.8891 -0.0132 0.058 Uiso 1 1 calc R . .
C16 C 0.2754(4) 0.8112(3) -0.0801(2) 0.0525(11) Uani 1 1 d . . .
H16A H 0.2340 0.8502 -0.1003 0.063 Uiso 1 1 calc R . .
C17 C 0.8667(3) 0.4025(3) 0.1367(2) 0.0543(12) Uani 1 1 d . . .
C18 C 0.8965(4) 0.5050(3) 0.2066(3) 0.0627(14) Uani 1 1 d . . .
H18A H 0.9364 0.4994 0.2464 0.075 Uiso 1 1 calc R . .
H18B H 0.9402 0.5186 0.1781 0.075 Uiso 1 1 calc R . .
C19 C 0.8232(4) 0.6220(3) 0.1738(3) 0.0662(14) Uani 1 1 d . . .
C20 C 0.7530(4) 0.7439(3) 0.1709(3) 0.0664(14) Uani 1 1 d . . .
H20A H 0.8023 0.7521 0.1447 0.080 Uiso 1 1 calc R . .
H20B H 0.7682 0.7757 0.2059 0.080 Uiso 1 1 calc R . .
C21 C 0.6419(4) 0.7814(3) 0.0789(2) 0.0516(12) Uani 1 1 d . . .
C22 C 0.5220(4) 0.8520(3) 0.0102(2) 0.0584(13) Uani 1 1 d . . .
H22A H 0.5776 0.8541 -0.0119 0.070 Uiso 1 1 calc R . .
H22B H 0.5066 0.9013 0.0211 0.070 Uiso 1 1 calc R . .
C23 C 0.4417(4) 0.7986(3) -0.0867(2) 0.0563(12) Uani 1 1 d . . .
C24 C 0.6726(4) 0.2244(3) 0.1801(2) 0.0571(13) Uani 1 1 d . . .
H24A H 0.6131 0.2167 0.1979 0.069 Uiso 1 1 calc R . .
H24B H 0.7213 0.1891 0.1979 0.069 Uiso 1 1 calc R . .
N1G N 0.2289(9) 0.5434(7) 0.1331(6) 0.071(3) Uani 0.50 1 d PU A 1
H1GA H 0.2743 0.5474 0.1645 0.085 Uiso 0.50 1 calc PR A 1
N2G N 0.1628(10) 0.5440(7) 0.0400(5) 0.063(3) Uani 0.50 1 d PU A 1
H2GA H 0.1604 0.5385 0.0013 0.075 Uiso 0.50 1 calc PR A 1
N3G N 0.8450(11) 0.6402(17) 0.0111(9) 0.093(7) Uani 0.50 1 d PU A 1
H3GA H 0.8632 0.6261 0.0481 0.112 Uiso 0.50 1 calc PR A 1
N4G N 0.7541(18) 0.6531(15) -0.0779(12) 0.090(5) Uani 0.50 1 d PU A 1
H4GA H 0.7010 0.6480 -0.1039 0.108 Uiso 0.50 1 calc PR A 1
C1G C 0.4277(7) 0.5480(7) 0.0850(6) 0.055(3) Uani 0.50 1 d PDU A 1
H1GB H 0.4341 0.5239 0.1222 0.066 Uiso 0.50 1 calc PR A 1
C2G C 0.3361(10) 0.5647(17) 0.0536(9) 0.056(4) Uani 0.50 1 d PDU A 1
C3G C 0.3241(9) 0.5982(12) -0.0032(7) 0.066(4) Uani 0.50 1 d PDU A 1
H3GB H 0.2613 0.6072 -0.0246 0.079 Uiso 0.50 1 calc PR A 1
C4G C 0.4079(8) 0.6176(7) -0.0271(7) 0.069(3) Uani 0.50 1 d PDU A 1
H4GB H 0.4007 0.6418 -0.0643 0.083 Uiso 0.50 1 calc PR A 1
C5G C 0.5845(8) 0.6237(7) -0.0219(6) 0.063(3) Uani 0.50 1 d PDU A 1
H5GA H 0.5768 0.6490 -0.0586 0.076 Uiso 0.50 1 calc PR A 1
C6G C 0.6764(8) 0.6076(7) 0.0078(6) 0.060(3) Uani 0.50 1 d PDU A 1
C7G C 0.6860(8) 0.5666(7) 0.0609(5) 0.068(3) Uani 0.50 1 d PDU A 1
H7GA H 0.7487 0.5516 0.0788 0.082 Uiso 0.50 1 calc PR A 1
C8G C 0.6054(7) 0.5474(6) 0.0879(5) 0.063(2) Uani 0.50 1 d PDU A 1
H8GA H 0.6139 0.5212 0.1242 0.075 Uiso 0.50 1 calc PR A 1
C9G C 0.5113(7) 0.5679(8) 0.0600(6) 0.051(2) Uani 0.50 1 d PDU A 1
C10G C 0.5028(8) 0.6022(9) 0.0028(6) 0.057(3) Uani 0.50 1 d PDU A 1
C11G C 0.2434(17) 0.5527(15) 0.0800(11) 0.052(3) Uani 0.50 1 d PU A 1
C12G C 0.1285(14) 0.5253(17) 0.1365(10) 0.079(7) Uani 0.50 1 d PU A 1
H12A H 0.1033 0.5534 0.1677 0.094 Uiso 0.50 1 calc PR A 1
H12B H 0.1213 0.4739 0.1447 0.094 Uiso 0.50 1 calc PR A 1
C13G C 0.0765(13) 0.5454(14) 0.0731(6) 0.083(6) Uani 0.50 1 d PU A 1
H13A H 0.0269 0.5098 0.0571 0.099 Uiso 0.50 1 calc PR A 1
H13B H 0.0465 0.5932 0.0723 0.099 Uiso 0.50 1 calc PR A 1
C14G C 0.7668(17) 0.6340(18) -0.0142(9) 0.093(7) Uani 0.50 1 d PU A 1
C15G C 0.9096(14) 0.6737(12) -0.0248(11) 0.085(6) Uani 0.50 1 d PU A 1
H15A H 0.9671 0.6434 -0.0263 0.102 Uiso 0.50 1 calc PR A 1
H15B H 0.9315 0.7206 -0.0079 0.102 Uiso 0.50 1 calc PR A 1
C16G C 0.8484(13) 0.6828(10) -0.0898(10) 0.082(4) Uani 0.50 1 d PU A 1
H16A H 0.8427 0.7334 -0.1023 0.098 Uiso 0.50 1 calc PR A 1
H16B H 0.8759 0.6547 -0.1201 0.098 Uiso 0.50 1 calc PR A 1
N1G' N 0.1716(17) 0.5723(9) 0.0694(13) 0.147(9) Uani 0.50 1 d PU B 2
H1GC H 0.1610 0.6022 0.0392 0.176 Uiso 0.50 1 calc PR B 2
N2G' N 0.2487(13) 0.4989(12) 0.1327(9) 0.120(5) Uani 0.50 1 d PU B 2
H2GC H 0.2966 0.4722 0.1499 0.145 Uiso 0.50 1 calc PR B 2
N3G' N 0.752(3) 0.665(3) -0.0930(14) 0.161(14) Uani 0.50 1 d PU B 2
H3GC H 0.7108 0.6749 -0.1251 0.193 Uiso 0.50 1 calc PR B 2
N4G' N 0.8127(15) 0.6533(14) -0.0060(11) 0.101(6) Uani 0.50 1 d PU B 2
H4GC H 0.8075 0.6634 0.0313 0.121 Uiso 0.50 1 calc PR B 2
C1' C 0.3620(11) 0.5894(11) 0.0192(9) 0.085(4) Uani 0.50 1 d PDU B 2
H1'A H 0.3065 0.6031 -0.0081 0.102 Uiso 0.50 1 calc PR B 2
C2' C 0.3518(15) 0.558(2) 0.0742(10) 0.088(6) Uani 0.50 1 d PDU B 2
C3' C 0.4345(10) 0.5384(12) 0.1154(7) 0.095(5) Uani 0.50 1 d PDU B 2
H3'A H 0.4265 0.5171 0.1523 0.113 Uiso 0.50 1 calc PR B 2
C4' C 0.5294(10) 0.5502(9) 0.1019(7) 0.093(4) Uani 0.50 1 d PDU B 2
H4'A H 0.5845 0.5387 0.1303 0.111 Uiso 0.50 1 calc PR B 2
C5' C 0.6313(10) 0.5958(7) 0.0280(6) 0.078(3) Uani 0.50 1 d PDU B 2
H5'A H 0.6891 0.5848 0.0543 0.093 Uiso 0.50 1 calc PR B 2
C6' C 0.6383(12) 0.6275(8) -0.0261(6) 0.073(3) Uani 0.50 1 d PDU B 2
C7' C 0.5549(9) 0.6474(7) -0.0653(8) 0.089(3) Uani 0.50 1 d PDU B 2
H7'A H 0.5605 0.6712 -0.1016 0.106 Uiso 0.50 1 calc PR B 2
C8' C 0.4636(10) 0.6322(7) -0.0507(7) 0.089(3) Uani 0.50 1 d PDU B 2
H8'A H 0.4066 0.6432 -0.0778 0.107 Uiso 0.50 1 calc PR B 2
C9' C 0.4574(10) 0.6003(9) 0.0048(7) 0.068(3) Uani 0.50 1 d PDU B 2
C10' C 0.5411(9) 0.5792(12) 0.0456(7) 0.077(4) Uani 0.50 1 d PDU B 2
C11' C 0.259(2) 0.540(2) 0.092(2) 0.107(8) Uani 0.50 1 d PU B 2
C12' C 0.0975(19) 0.5463(13) 0.1065(15) 0.114(9) Uani 0.50 1 d PU B 2
H12C H 0.0438 0.5212 0.0813 0.137 Uiso 0.50 1 calc PR B 2
H12D H 0.0706 0.5866 0.1268 0.137 Uiso 0.50 1 calc PR B 2
C13' C 0.152(2) 0.497(2) 0.1509(15) 0.134(10) Uani 0.50 1 d PU B 2
H13C H 0.1542 0.5142 0.1923 0.160 Uiso 0.50 1 calc PR B 2
H13D H 0.1245 0.4482 0.1474 0.160 Uiso 0.50 1 calc PR B 2
C14' C 0.7371(15) 0.6394(14) -0.0394(12) 0.087(5) Uani 0.50 1 d PU B 2
C15' C 0.875(3) 0.671(3) -0.081(3) 0.27(3) Uani 0.50 1 d PU B 2
H15C H 0.9007 0.6378 -0.1087 0.321 Uiso 0.50 1 calc PR B 2
H15D H 0.8930 0.7196 -0.0909 0.321 Uiso 0.50 1 calc PR B 2
C16' C 0.919(3) 0.655(3) -0.0230(18) 0.21(2) Uani 0.50 1 d PU B 2
H16C H 0.9525 0.6086 -0.0188 0.257 Uiso 0.50 1 calc PR B 2
H16D H 0.9600 0.6937 -0.0034 0.257 Uiso 0.50 1 calc PR B 2
Cl1 Cl 0.93994(18) 0.65257(19) -0.23301(15) 0.1496(11) Uani 1 1 d . . .
O1W O 0.8459(5) 0.2035(4) 0.3172(3) 0.135(2) Uani 1 1 d . . .
O2W O 0.1036(5) 0.6140(3) 0.2767(3) 0.1180(19) Uani 1 1 d . . .
O3W O 0.6913(5) 0.6374(5) 0.3807(3) 0.149(3) Uani 1 1 d . . .
O4W O -0.0603(5) 0.8129(5) -0.1921(4) 0.164(3) Uani 1 1 d . . .
O5W O 0.6196(4) 0.6240(6) -0.1898(4) 0.201(5) Uani 1 1 d . . .
O6W O 0.1323(6) 0.9113(5) -0.0047(7) 0.237(5) Uani 1 1 d . . .
O7W O 0.9611(10) 0.8705(7) -0.0795(5) 0.245(6) Uani 1 1 d . . .
O8W O 0.8945(14) 0.4333(18) 0.3975(9) 0.221(12) Uani 0.50 1 d P C 1
O8' O 0.9549(17) 0.4967(17) 0.3759(8) 0.230(14) Uani 0.50 1 d P C 1
O9W O 0.9878(11) 0.3036(9) 0.3597(6) 0.135(5) Uani 0.50 1 d P D 2
O9' O 1.070(2) 0.382(2) 0.3496(16) 0.35(2) Uani 0.50 1 d P E 2
O10W O 0.8804(8) 0.8268(8) 0.0315(6) 0.121(4) Uani 0.50 1 d P F 3
O10' O 0.8194(11) 0.8625(8) -0.0092(7) 0.135(4) Uani 0.50 1 d P F 3
O11W O 0.3338(13) 0.5576(11) 0.2630(12) 0.187(9) Uani 0.50 1 d P G 4
O11' O 0.3354(17) 0.497(2) 0.2435(8) 0.264(18) Uani 0.50 1 d P G 4
O12W O 0.3807(14) 1.0030(6) 0.0775(7) 0.103(5) Uani 0.50 1 d P H 5
O12' O 0.458(4) 1.0029(15) 0.1015(17) 0.25(2) Uani 0.50 1 d P H 5
O13W O 0.4227(18) 0.9549(11) -0.1204(12) 0.207(10) Uani 0.50 1 d P I 6
O13' O 0.152(2) 1.0183(13) -0.1906(9) 0.251(13) Uani 0.50 1 d P J 6
O14W O 0.259(2) 0.4091(15) 0.2648(18) 0.292(14) Uani 0.50 1 d P K 7
O14' O 0.9739(19) 0.2603(18) 0.3970(15) 0.263(13) Uani 0.50 1 d P L 7
O15W O 0.243(7) 1.028(2) 0.001(4) 0.69(10) Uani 0.50 1 d P M 8
O15' O 0.385(9) 1.011(4) 0.068(4) 0.76(11) Uani 0.50 1 d P N 8
S1 S 0.2802(10) 1.0182(5) -0.0938(5) 0.215(4) Uani 0.50 1 d PD O 9
O1S O 0.3780(13) 0.9993(9) -0.0791(16) 0.232(14) Uani 0.50 1 d PD O 9
O2S O 0.2832(16) 1.0796(8) -0.1277(12) 0.242(12) Uani 0.50 1 d PD O 9
O3S O 0.214(4) 1.0223(15) -0.053(2) 0.37(3) Uani 0.50 1 d PD O 9
O4S O 0.274(4) 0.9693(14) -0.1423(12) 0.51(4) Uani 0.50 1 d PD O 9
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'
Cl Cl 0.1484 0.1585 '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_1
_geom_angle_site_symmetry_3
C1 N1 C24 122.9(4) . .
C1 N1 C9 112.2(4) . .
C24 N1 C9 122.1(4) . .
C1 N2 C2 122.9(4) . .
C1 N2 C10 112.2(4) . .
C2 N2 C10 124.0(4) . .
C3 N3 C11 111.7(4) . .
C3 N3 C2 121.0(4) . .
C11 N3 C2 123.9(4) . .
C3 N4 C12 111.3(4) . .
C3 N4 C4 120.8(4) . .
C12 N4 C4 122.7(4) . .
C5 N5 C13 111.9(4) . .
C5 N5 C4 121.0(4) . .
C13 N5 C4 120.9(4) . .
C5 N6 C14 113.4(4) . .
C5 N6 C6 123.1(4) . .
C14 N6 C6 122.8(4) . .
C7 N7 C15 112.3(4) . .
C7 N7 C6 122.4(4) . .
C15 N7 C6 122.6(4) . .
C7 N8 C16 112.0(4) . .
C7 N8 C8 122.1(4) . .
C16 N8 C8 122.3(4) . .
C17 N9 C8 122.7(4) . 3_665
C17 N9 C9 112.2(4) . .
C8 N9 C9 121.4(4) 3_665 .
C17 N10 C18 121.5(4) . .
C17 N10 C10 111.8(4) . .
C18 N10 C10 121.5(4) . .
C19 N11 C11 111.5(4) . .
C19 N11 C18 122.2(4) . .
C11 N11 C18 124.0(4) . .
C19 N12 C20 123.2(4) . .
C19 N12 C12 110.9(4) . .
C20 N12 C12 122.7(4) . .
C21 N13 C20 123.4(4) . .
C21 N13 C13 111.9(4) . .
C20 N13 C13 122.6(4) . .
C21 N14 C22 121.5(4) . .
C21 N14 C14 111.2(4) . .
C22 N14 C14 122.0(4) . .
C23 N15 C15 111.9(4) . .
C23 N15 C22 122.9(4) . .
C15 N15 C22 121.8(4) . .
C23 N16 C24 122.7(4) . 3_665
C23 N16 C16 112.5(4) . .
C24 N16 C16 122.5(4) 3_665 .
O1 C1 N1 125.7(5) . .
O1 C1 N2 125.9(4) . .
N1 C1 N2 108.4(4) . .
N2 C2 N3 113.6(4) . .
O2 C3 N4 126.2(5) . .
O2 C3 N3 125.2(5) . .
N4 C3 N3 108.6(4) . .
N5 C4 N4 113.2(4) . .
O3 C5 N6 126.9(5) . .
O3 C5 N5 125.2(5) . .
N6 C5 N5 107.9(4) . .
N7 C6 N6 113.8(4) . .
O4 C7 N7 125.8(5) . .
O4 C7 N8 125.6(5) . .
N7 C7 N8 108.6(4) . .
N9 C8 N8 113.1(4) 3_665 .
N9 C9 N1 113.8(4) . .
N9 C9 C10 103.4(4) . .
N1 C9 C10 103.3(3) . .
N2 C10 N10 114.3(4) . .
N2 C10 C9 103.8(4) . .
N10 C10 C9 103.6(3) . .
N3 C11 N11 114.2(4) . .
N3 C11 C12 103.9(4) . .
N11 C11 C12 103.3(4) . .
N4 C12 N12 113.8(4) . .
N4 C12 C11 103.7(4) . .
N12 C12 C11 104.1(4) . .
N5 C13 N13 114.6(4) . .
N5 C13 C14 103.1(4) . .
N13 C13 C14 103.9(4) . .
N6 C14 N14 115.4(4) . .
N6 C14 C13 102.8(4) . .
N14 C14 C13 102.7(4) . .
N7 C15 N15 115.4(4) . .
N7 C15 C16 103.5(4) . .
N15 C15 C16 103.1(4) . .
N8 C16 N16 114.8(4) . .
N8 C16 C15 102.8(4) . .
N16 C16 C15 103.0(4) . .
O5 C17 N10 126.3(5) . .
O5 C17 N9 125.3(5) . .
N10 C17 N9 108.4(4) . .
N11 C18 N10 112.6(4) . .
O6 C19 N12 125.6(5) . .
O6 C19 N11 124.9(5) . .
N12 C19 N11 109.4(4) . .
N12 C20 N13 113.5(4) . .
O7 C21 N13 125.6(5) . .
O7 C21 N14 125.2(5) . .
N13 C21 N14 109.3(4) . .
N14 C22 N15 112.8(4) . .
O8 C23 N16 125.8(5) . .
O8 C23 N15 125.2(5) . .
N16 C23 N15 109.0(4) . .
N1 C24 N16 113.6(4) . 3_665
C11G N1G C12G 112.3(16) . .
C11G N2G C13G 108.2(14) . .
C14G N3G C15G 113(2) . .
C14G N4G C16G 107(2) . .
C2G C1G C9G 118.7(11) . .
C1G C2G C3G 122.0(12) . .
C1G C2G C11G 122.2(12) . .
C3G C2G C11G 115.7(11) . .
C4G C3G C2G 118.3(12) . .
C3G C4G C10G 122.1(11) . .
C10G C5G C6G 119.4(11) . .
C5G C6G C7G 119.3(11) . .
C5G C6G C14G 121.7(15) . .
C7G C6G C14G 119.0(14) . .
C8G C7G C6G 122.1(11) . .
C7G C8G C9G 119.0(11) . .
C1G C9G C8G 120.7(10) . .
C1G C9G C10G 121.3(10) . .
C8G C9G C10G 117.7(10) . .
C5G C10G C9G 122.0(11) . .
C5G C10G C4G 120.4(10) . .
C9G C10G C4G 117.5(10) . .
N1G C11G N2G 113(2) . .
N1G C11G C2G 131.6(18) . .
N2G C11G C2G 115(2) . .
N1G C12G C13G 102.1(15) . .
N2G C13G C12G 99.2(13) . .
N3G C14G N4G 114.8(19) . .
N3G C14G C6G 130(2) . .
N4G C14G C6G 115.1(18) . .
N3G C15G C16G 105.9(18) . .
N4G C16G C15G 98.8(18) . .
C11' N1G' C12' 107(2) . .
C11' N2G' C13' 116(2) . .
C14' N3G' C15' 100(3) . .
C14' N4G' C16' 127(3) . .
C2' C1' C9' 119.2(16) . .
C11' C2' C1' 124(2) . .
C11' C2' C3' 115.6(19) . .
C1' C2' C3' 120.6(17) . .
C4' C3' C2' 120.5(16) . .
C10' C4' C3' 119.7(14) . .
C6' C5' C10' 122.4(14) . .
C5' C6' C7' 120.8(15) . .
C5' C6' C14' 116.4(16) . .
C7' C6' C14' 122.8(15) . .
C6' C7' C8' 119.7(15) . .
C7' C8' C9' 119.0(14) . .
C8' C9' C10' 122.5(13) . .
C8' C9' C1' 117.0(14) . .
C10' C9' C1' 120.5(13) . .
C4' C10' C9' 119.4(12) . .
C4' C10' C5' 124.9(12) . .
C9' C10' C5' 115.5(13) . .
N2G' C11' C2' 124(3) . .
N2G' C11' N1G' 110(3) . .
C2' C11' N1G' 125(3) . .
N1G' C12' C13' 105(2) . .
N2G' C13' C12' 101(2) . .
N4G' C14' N3G' 104(2) . .
N4G' C14' C6' 130(2) . .
N3G' C14' C6' 121(3) . .
C16' C15' N3G' 115(3) . .
N4G' C16' C15' 87(3) . .
O2S S1 O1S 103.2(16) . .
O2S S1 O3S 113.5(18) . .
O1S S1 O3S 125(3) . .
O2S S1 O4S 96.3(17) . .
O1S S1 O4S 88(2) . .
O3S S1 O4S 125(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 C1 1.226(5) .
O2 C3 1.221(6) .
O3 C5 1.229(6) .
O4 C7 1.231(6) .
O5 C17 1.222(6) .
O6 C19 1.233(7) .
O7 C21 1.235(6) .
O8 C23 1.227(6) .
N1 C1 1.370(6) .
N1 C24 1.436(6) .
N1 C9 1.456(6) .
N2 C1 1.373(6) .
N2 C2 1.448(6) .
N2 C10 1.450(6) .
N3 C3 1.374(6) .
N3 C11 1.438(6) .
N3 C2 1.449(6) .
N4 C3 1.362(7) .
N4 C12 1.452(6) .
N4 C4 1.456(6) .
N5 C5 1.378(6) .
N5 C13 1.447(6) .
N5 C4 1.455(6) .
N6 C5 1.359(6) .
N6 C14 1.439(6) .
N6 C6 1.455(6) .
N7 C7 1.361(6) .
N7 C15 1.431(6) .
N7 C6 1.453(6) .
N8 C7 1.367(6) .
N8 C16 1.437(6) .
N8 C8 1.455(6) .
N9 C17 1.374(7) .
N9 C8 1.451(6) 3_665
N9 C9 1.451(6) .
N10 C17 1.367(6) .
N10 C18 1.456(7) .
N10 C10 1.457(6) .
N11 C19 1.365(7) .
N11 C11 1.448(6) .
N11 C18 1.449(7) .
N12 C19 1.357(7) .
N12 C20 1.441(7) .
N12 C12 1.456(6) .
N13 C21 1.359(6) .
N13 C20 1.449(7) .
N13 C13 1.448(6) .
N14 C21 1.381(7) .
N14 C22 1.439(6) .
N14 C14 1.459(6) .
N15 C23 1.373(6) .
N15 C15 1.456(6) .
N15 C22 1.461(6) .
N16 C23 1.354(6) .
N16 C24 1.448(6) 3_665
N16 C16 1.459(6) .
C8 N9 1.451(6) 3_665
C9 C10 1.544(7) .
C11 C12 1.533(7) .
C13 C14 1.558(7) .
C15 C16 1.560(7) .
C24 N16 1.448(6) 3_665
N1G C11G 1.25(3) .
N1G C12G 1.44(2) .
N2G C11G 1.33(3) .
N2G C13G 1.50(2) .
N3G C14G 1.15(3) .
N3G C15G 1.43(3) .
N4G C14G 1.46(3) .
N4G C16G 1.48(3) .
C1G C2G 1.386(13) .
C1G C9G 1.411(11) .
C2G C3G 1.405(12) .
C2G C11G 1.51(3) .
C3G C4G 1.399(12) .
C4G C10G 1.407(12) .
C5G C10G 1.392(11) .
C5G C6G 1.374(12) .
C6G C7G 1.403(12) .
C6G C14G 1.50(2) .
C7G C8G 1.396(11) .
C8G C9G 1.407(11) .
C9G C10G 1.421(12) .
C12G C13G 1.54(2) .
C15G C16G 1.58(3) .
N1G' C11' 1.37(4) .
N1G' C12' 1.50(2) .
N2G' C11' 1.23(4) .
N2G' C13' 1.45(3) .
N3G' C14' 1.34(3) .
N3G' C15' 1.67(5) .
N4G' C14' 1.21(3) .
N4G' C16' 1.57(4) .
C1' C2' 1.390(14) .
C1' C9' 1.421(13) .
C2' C11' 1.44(4) .
C2' C3' 1.403(14) .
C3' C4' 1.410(12) .
C4' C10' 1.405(12) .
C5' C6' 1.367(13) .
C5' C10' 1.400(12) .
C6' C7' 1.388(13) .
C6' C14' 1.46(2) .
C7' C8' 1.382(12) .
C8' C9' 1.395(12) .
C9' C10' 1.417(13) .
C12' C13' 1.48(4) .
C15' C16' 1.38(6) .
O8W O8' 1.56(4) .
O10W O10' 1.322(18) .
O11W O11' 1.22(4) .
O12W O12' 1.12(5) .
S1 O2S 1.377(15) .
S1 O1S 1.386(15) .
S1 O3S 1.399(16) .
S1 O4S 1.411(17) .
