#------------------------------------------------------------------------------
#$Date: 2017-01-09 05:08:45 +0200 (Mon, 09 Jan 2017) $
#$Revision: 190086 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/67/7226735.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_7226735
loop_
_publ_author_name
'Ovsyannikov, A. S.'
'Lang, M. N.'
'Ferlay, S.'
'Solovieva, S. E.'
'Antipin, I. S.'
'Konovalov, A. I.'
'Kyritsakas, N.'
'Hosseini, M. W.'
_publ_section_title
;
 Molecular tectonics: tetracarboxythiacalix[4]arene derivatives as tectons
 for the formation of hydrogen-bonded networks
;
_journal_issue                   44
_journal_name_full               CrystEngComm
_journal_page_first              8622
_journal_paper_doi               10.1039/C6CE02026G
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         2(C56H70O8S8),2(C10H20N4),CH4O,H2O
_chemical_formula_sum            'C133 H186 N8 O18 S16'
_chemical_formula_weight         2699.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2016-09-20 deposited with the CCDC.
2016-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.1140(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   33.2961(10)
_cell_length_b                   11.7323(3)
_cell_length_c                   20.7114(5)
_cell_measurement_reflns_used    79000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.
_cell_measurement_theta_min      2.5
_cell_volume                     7384.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            79125
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.144
_diffrn_reflns_theta_min         1.333
_exptl_absorpt_coefficient_mu    0.295
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2884
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.617
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Flack x determined using 5702 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.146(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     819
_refine_ls_number_reflns         20081
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0660
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.082
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1284P)²+3.8076P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1821
_refine_ls_wR_factor_ref         0.2051
_reflns_Friedel_coverage         0.834
_reflns_Friedel_fraction_full    0.946
_reflns_Friedel_fraction_max     0.876
_reflns_number_gt                14646
_reflns_number_total             20081
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ce02026g2.cif
_cod_data_source_block           e3770a_b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7226728--7226735.cif.
;
_cod_database_code               7226735
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.983
_shelx_estimated_absorpt_t_max   0.985
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
S1 S 0.62892(4) 0.39833(11) 0.60184(6) 0.0316(3) Uani 1 1 d . . .
C1 C 0.59116(14) 0.4603(4) 0.6319(2) 0.0270(9) Uani 1 1 d . . .
C2 C 0.55801(15) 0.3982(4) 0.6420(2) 0.0266(9) Uani 1 1 d . . .
C3 C 0.53088(14) 0.4594(4) 0.6665(2) 0.0271(9) Uani 1 1 d . . .
C4 C 0.53864(16) 0.5735(4) 0.6845(2) 0.0278(10) Uani 1 1 d . . .
H4 H 0.5200 0.6122 0.7020 0.033 Uiso 1 1 calc R U .
C5 C 0.57277(17) 0.6332(4) 0.6778(3) 0.0317(10) Uani 1 1 d . . .
C6 C 0.59861(17) 0.5748(4) 0.6511(3) 0.0322(10) Uani 1 1 d . . .
H6 H 0.6221 0.6136 0.6456 0.039 Uiso 1 1 calc R U .
S2 S 0.55108(4) 0.25058(10) 0.62257(7) 0.0330(3) Uani 1 1 d . . .
C7 C 0.5627(3) 0.1862(7) 0.7084(5) 0.078(2) Uani 1 1 d . . .
H7A H 0.5380 0.2045 0.7216 0.094 Uiso 1 1 calc R U .
H7B H 0.5631 0.1024 0.7031 0.094 Uiso 1 1 calc R U .
C8 C 0.60371(19) 0.2201(6) 0.7670(3) 0.0473(14) Uani 1 1 d . . .
H8A H 0.6012 0.3021 0.7759 0.057 Uiso 1 1 calc R U .
H8B H 0.6054 0.1784 0.8096 0.057 Uiso 1 1 calc R U .
C9 C 0.6454(3) 0.2042(7) 0.7617(6) 0.083(3) Uani 1 1 d . . .
H9A H 0.6408 0.2181 0.7120 0.099 Uiso 1 1 calc R U .
H9B H 0.6542 0.1234 0.7724 0.099 Uiso 1 1 calc R U .
C10 C 0.6833(2) 0.2779(6) 0.8088(4) 0.0576(17) Uani 1 1 d . . .
O1 O 0.67741(19) 0.3584(6) 0.8405(3) 0.0837(19) Uani 1 1 d . . .
O2 O 0.71827(16) 0.2554(5) 0.8009(3) 0.0673(13) Uani 1 1 d . . .
C11 C 0.5805(2) 0.7608(5) 0.6950(3) 0.0467(14) Uani 1 1 d . . .
C12 C 0.5461(3) 0.8102(6) 0.7190(4) 0.066(2) Uani 1 1 d . . .
H12A H 0.5521 0.8913 0.7300 0.098 Uiso 1 1 calc R U .
H12B H 0.5476 0.7696 0.7613 0.098 Uiso 1 1 calc R U .
H12C H 0.5166 0.8012 0.6811 0.098 Uiso 1 1 calc R U .
C13 C 0.5796(4) 0.8248(7) 0.6334(6) 0.105(4) Uani 1 1 d . . .
H13A H 0.5985 0.7868 0.6141 0.157 Uiso 1 1 calc R U .
H13B H 0.5903 0.9024 0.6479 0.157 Uiso 1 1 calc R U .
H13C H 0.5494 0.8278 0.5972 0.157 Uiso 1 1 calc R U .
C14 C 0.6261(3) 0.7735(8) 0.7558(6) 0.104(4) Uani 1 1 d . . .
H14A H 0.6487 0.7515 0.7395 0.156 Uiso 1 1 calc R U .
H14B H 0.6280 0.7241 0.7952 0.156 Uiso 1 1 calc R U .
H14C H 0.6305 0.8530 0.7718 0.156 Uiso 1 1 calc R U .
S3 S 0.48854(4) 0.39582(11) 0.68503(6) 0.0305(3) Uani 1 1 d . . .
C15 C 0.45168(15) 0.3348(4) 0.6039(3) 0.0274(9) Uani 1 1 d . . .
C16 C 0.43182(14) 0.3940(4) 0.5406(2) 0.0255(9) Uani 1 1 d . . .
C17 C 0.40241(14) 0.3344(4) 0.4811(2) 0.0259(9) Uani 1 1 d . . .
C18 C 0.39278(15) 0.2205(4) 0.4872(3) 0.0298(10) Uani 1 1 d . . .
H18 H 0.3733 0.1811 0.4462 0.036 Uiso 1 1 calc R U .
C19 C 0.41062(16) 0.1629(4) 0.5508(3) 0.0293(10) Uani 1 1 d . . .
C20 C 0.44070(16) 0.2209(4) 0.6088(3) 0.0292(10) Uani 1 1 d . . .
H20 H 0.4541 0.1825 0.6528 0.035 Uiso 1 1 calc R U .
S4 S 0.44334(4) 0.53978(10) 0.53319(7) 0.0343(3) Uani 1 1 d . . .
C21 C 0.4169(2) 0.6064(6) 0.5847(3) 0.0484(14) Uani 1 1 d . . .
H21A H 0.4248 0.5639 0.6296 0.058 Uiso 1 1 calc R U .
H21B H 0.4281 0.6852 0.5968 0.058 Uiso 1 1 calc R U .
C22 C 0.3652(3) 0.6100(8) 0.5444(4) 0.068(2) Uani 1 1 d . . .
H22A H 0.3539 0.5310 0.5343 0.081 Uiso 1 1 calc R U .
H22B H 0.3526 0.6457 0.5753 0.081 Uiso 1 1 calc R U .
C23 C 0.3509(2) 0.6726(7) 0.4789(4) 0.066(2) Uani 1 1 d . . .
H23A H 0.3626 0.6325 0.4482 0.080 Uiso 1 1 calc R U .
H23B H 0.3654 0.7481 0.4899 0.080 Uiso 1 1 calc R U .
C24 C 0.3030(2) 0.6927(8) 0.4360(5) 0.075(2) Uani 1 1 d . . .
O3 O 0.27557(18) 0.6857(8) 0.4656(3) 0.092(2) Uani 1 1 d . . .
H3 H 0.2889 0.6634 0.5076 0.138 Uiso 1 1 calc R U .
O4 O 0.2926(2) 0.7204(7) 0.3750(4) 0.094(2) Uani 1 1 d . . .
C25 C 0.40057(19) 0.0363(5) 0.5546(3) 0.0379(12) Uani 1 1 d . . .
C26 C 0.4111(5) -0.0021(7) 0.6299(5) 0.111(5) Uani 1 1 d . . .
H26A H 0.4035 -0.0829 0.6298 0.166 Uiso 1 1 calc R U .
H26B H 0.3940 0.0433 0.6494 0.166 Uiso 1 1 calc R U .
H26C H 0.4426 0.0084 0.6590 0.166 Uiso 1 1 calc R U .
C27 C 0.4281(4) -0.0308(7) 0.5263(7) 0.107(4) Uani 1 1 d . . .
H27A H 0.4592 -0.0101 0.5522 0.160 Uiso 1 1 calc R U .
H27B H 0.4189 -0.0139 0.4760 0.160 Uiso 1 1 calc R U .
H27C H 0.4244 -0.1124 0.5324 0.160 Uiso 1 1 calc R U .
C28 C 0.3531(3) 0.0106(8) 0.5103(7) 0.123(5) Uani 1 1 d . . .
H28A H 0.3505 -0.0305 0.4676 0.184 Uiso 1 1 calc R U .
H28B H 0.3365 0.0821 0.4969 0.184 Uiso 1 1 calc R U .
H28C H 0.3413 -0.0366 0.5375 0.184 Uiso 1 1 calc R U .
S5 S -0.00203(4) 0.60084(11) 0.18991(6) 0.0337(3) Uani 1 1 d . . .
C29 C 0.03869(15) 0.5364(4) 0.1681(2) 0.0297(10) Uani 1 1 d . . .
C30 C 0.06387(15) 0.5957(4) 0.1393(2) 0.0282(9) Uani 1 1 d . . .
C31 C 0.09645(15) 0.5341(4) 0.1274(2) 0.0291(10) Uani 1 1 d . . .
C32 C 0.10536(16) 0.4212(4) 0.1496(3) 0.0321(10) Uani 1 1 d . . .
H32 H 0.1285 0.3826 0.1432 0.039 Uiso 1 1 calc R U .
C33 C 0.08151(18) 0.3636(4) 0.1807(3) 0.0343(11) Uani 1 1 d . . .
C34 C 0.04777(17) 0.4219(4) 0.1882(3) 0.0319(10) Uani 1 1 d . . .
H34 H 0.0301 0.3834 0.2075 0.038 Uiso 1 1 calc R U .
S6 S 0.05513(4) 0.74270(11) 0.11916(7) 0.0350(3) Uani 1 1 d . . .
C35 C 0.10360(17) 0.7998(4) 0.1910(3) 0.0343(11) Uani 1 1 d . . .
H35A H 0.1296 0.7534 0.1962 0.041 Uiso 1 1 calc R U .
H35B H 0.1088 0.8787 0.1793 0.041 Uiso 1 1 calc R U .
C36 C 0.09846(18) 0.7998(5) 0.2599(3) 0.0414(13) Uani 1 1 d . . .
H36A H 0.0924 0.7211 0.2705 0.050 Uiso 1 1 calc R U .
H36B H 0.0727 0.8474 0.2546 0.050 Uiso 1 1 calc R U .
C37 C 0.13889(19) 0.8447(5) 0.3222(3) 0.0485(14) Uani 1 1 d . . .
H37A H 0.1480 0.9171 0.3078 0.058 Uiso 1 1 calc R U .
H37B H 0.1302 0.8622 0.3615 0.058 Uiso 1 1 calc R U .
C38 C 0.17785(18) 0.7668(6) 0.3497(3) 0.0460(13) Uani 1 1 d . . .
O5 O 0.21145(16) 0.8103(5) 0.4009(3) 0.0728(15) Uani 1 1 d . . .
O6 O 0.17536(15) 0.6687(4) 0.3290(3) 0.0586(12) Uani 1 1 d . . .
C39 C 0.0916(2) 0.2378(4) 0.2031(3) 0.0421(13) Uani 1 1 d . . .
C40 C 0.1379(3) 0.2366(8) 0.2647(5) 0.087(3) Uani 1 1 d . . .
H40A H 0.1464 0.1578 0.2798 0.130 Uiso 1 1 calc R U .
H40B H 0.1373 0.2807 0.3045 0.130 Uiso 1 1 calc R U .
H40C H 0.1592 0.2705 0.2488 0.130 Uiso 1 1 calc R U .
C41 C 0.0607(3) 0.1891(6) 0.2314(5) 0.083(3) Uani 1 1 d . . .
H41A H 0.0309 0.1872 0.1937 0.124 Uiso 1 1 calc R U .
H41B H 0.0610 0.2365 0.2705 0.124 Uiso 1 1 calc R U .
H41C H 0.0700 0.1115 0.2485 0.124 Uiso 1 1 calc R U .
C42 C 0.0925(6) 0.1722(7) 0.1424(7) 0.153(7) Uani 1 1 d . . .
H42A H 0.0911 0.0905 0.1511 0.229 Uiso 1 1 calc R U .
H42B H 0.1198 0.1889 0.1370 0.229 Uiso 1 1 calc R U .
H42C H 0.0673 0.1939 0.0991 0.229 Uiso 1 1 calc R U .
S7 S 0.13092(4) 0.59426(11) 0.08978(6) 0.0320(3) Uani 1 1 d . . .
C43 C 0.09557(15) 0.6595(4) 0.0089(3) 0.0290(10) Uani 1 1 d . . .
C44 C 0.06400(15) 0.6001(4) -0.0482(2) 0.0290(9) Uani 1 1 d . . .
C45 C 0.04109(15) 0.6619(4) -0.1097(2) 0.0277(9) Uani 1 1 d . . .
C46 C 0.05018(17) 0.7765(4) -0.1155(3) 0.0321(10) Uani 1 1 d . . .
H46 H 0.0344 0.8156 -0.1587 0.039 Uiso 1 1 calc R U .
C47 C 0.08183(17) 0.8344(4) -0.0594(3) 0.0315(10) Uani 1 1 d . . .
C48 C 0.10378(16) 0.7742(4) 0.0024(3) 0.0300(10) Uani 1 1 d . . .
H48 H 0.1253 0.8124 0.0418 0.036 Uiso 1 1 calc R U .
S8 S 0.05266(5) 0.45500(11) -0.04018(8) 0.0440(4) Uani 1 1 d . . .
C49 C 0.0772(3) 0.3915(6) -0.0960(4) 0.070(2) Uani 1 1 d . . .
H49A H 0.0663 0.3125 -0.1078 0.084 Uiso 1 1 calc R U .
H49B H 0.0676 0.4351 -0.1407 0.084 Uiso 1 1 calc R U .
C50 C 0.1272(3) 0.3898(7) -0.0610(3) 0.066(2) Uani 1 1 d . . .
H50A H 0.1384 0.4687 -0.0497 0.080 Uiso 1 1 calc R U .
H50B H 0.1387 0.3571 -0.0941 0.080 Uiso 1 1 calc R U .
C51 C 0.1434(2) 0.3188(6) 0.0069(4) 0.0620(19) Uani 1 1 d . . .
H51A H 0.1301 0.3496 0.0382 0.074 Uiso 1 1 calc R U .
H51B H 0.1327 0.2396 -0.0055 0.074 Uiso 1 1 calc R U .
C52 C 0.1921(2) 0.3161(6) 0.0469(4) 0.0535(16) Uani 1 1 d . . .
O7 O 0.2186(2) 0.3438(7) 0.0241(3) 0.0882(19) Uani 1 1 d . . .
O8 O 0.20342(16) 0.2827(5) 0.1127(3) 0.0671(14) Uani 1 1 d . . .
H8D H 0.1903 0.2217 0.1131 0.101 Uiso 1 1 calc R U .
C53 C 0.08960(19) 0.9621(4) -0.0631(3) 0.0361(11) Uani 1 1 d . . .
C54 C 0.0687(5) 1.0070(7) -0.1384(4) 0.112(5) Uani 1 1 d . . .
H54A H 0.0717 1.0902 -0.1379 0.168 Uiso 1 1 calc R U .
H54B H 0.0375 0.9865 -0.1597 0.168 Uiso 1 1 calc R U .
H54C H 0.0836 0.9735 -0.1661 0.168 Uiso 1 1 calc R U .
C55 C 0.0664(4) 1.0221(6) -0.0234(6) 0.094(3) Uani 1 1 d . . .
H55A H 0.0751 0.9871 0.0233 0.140 Uiso 1 1 calc R U .
H55B H 0.0345 1.0152 -0.0500 0.140 Uiso 1 1 calc R U .
H55C H 0.0747 1.1028 -0.0178 0.140 Uiso 1 1 calc R U .
C56 C 0.1380(3) 0.9859(7) -0.0290(8) 0.120(5) Uani 1 1 d . . .
H56A H 0.1441 1.0581 -0.0471 0.180 Uiso 1 1 calc R U .
H56B H 0.1539 0.9241 -0.0401 0.180 Uiso 1 1 calc R U .
H56C H 0.1475 0.9912 0.0224 0.180 Uiso 1 1 calc R U .
C57 C 0.73526(19) 0.6081(6) 0.8338(4) 0.0503(15) Uani 1 1 d . . .
N1 N 0.75307(18) 0.7107(5) 0.8461(3) 0.0533(13) Uani 1 1 d . . .
H1 H 0.7575 0.7459 0.8121 0.064 Uiso 1 1 calc R U .
C58 C 0.7656(2) 0.7676(7) 0.9141(4) 0.0623(19) Uani 1 1 d . . .
H58A H 0.7413 0.8173 0.9132 0.075 Uiso 1 1 calc R U .
H58B H 0.7919 0.8156 0.9241 0.075 Uiso 1 1 calc R U .
C59 C 0.7755(2) 0.6774(7) 0.9713(4) 0.0638(19) Uani 1 1 d . . .
H59A H 0.8026 0.6356 0.9772 0.077 Uiso 1 1 calc R U .
H59B H 0.7804 0.7143 1.0169 0.077 Uiso 1 1 calc R U .
C60 C 0.7381(3) 0.5965(8) 0.9514(4) 0.068(2) Uani 1 1 d . . .
H60A H 0.7461 0.5327 0.9856 0.081 Uiso 1 1 calc R U .
H60B H 0.7123 0.6359 0.9533 0.081 Uiso 1 1 calc R U .
N2 N 0.72665(18) 0.5520(5) 0.8807(3) 0.0548(14) Uani 1 1 d . . .
H2 H 0.7135 0.4853 0.8693 0.066 Uiso 1 1 calc R U .
C61 C 0.7263(2) 0.5520(6) 0.7642(3) 0.0498(14) Uani 1 1 d . . .
H61A H 0.7117 0.6070 0.7253 0.060 Uiso 1 1 calc R U .
H61B H 0.7062 0.4866 0.7574 0.060 Uiso 1 1 calc R U .
C62 C 0.76926(19) 0.5102(5) 0.7611(3) 0.0440(13) Uani 1 1 d . . .
H62A H 0.7870 0.5771 0.7597 0.053 Uiso 1 1 calc R U .
H62B H 0.7864 0.4671 0.8049 0.053 Uiso 1 1 calc R U .
C63 C 0.76199(17) 0.4362(5) 0.6989(3) 0.0413(12) Uani 1 1 d . . .
N3 N 0.74307(16) 0.3375(4) 0.6948(3) 0.0457(11) Uani 1 1 d . . .
H3A H 0.7358 0.3168 0.7295 0.055 Uiso 1 1 calc R U .
C64 C 0.7336(2) 0.2610(6) 0.6360(4) 0.0545(16) Uani 1 1 d . . .
H64A H 0.7065 0.2172 0.6278 0.065 Uiso 1 1 calc R U .
H64B H 0.7581 0.2063 0.6468 0.065 Uiso 1 1 calc R U .
C65 C 0.7276(2) 0.3269(7) 0.5715(4) 0.0584(18) Uani 1 1 d . . .
H65A H 0.7004 0.3733 0.5567 0.070 Uiso 1 1 calc R U .
H65B H 0.7244 0.2740 0.5325 0.070 Uiso 1 1 calc R U .
C66 C 0.7662(2) 0.4030(7) 0.5863(4) 0.0576(17) Uani 1 1 d . . .
H66A H 0.7925 0.3566 0.5935 0.069 Uiso 1 1 calc R U .
H66B H 0.7604 0.4541 0.5454 0.069 Uiso 1 1 calc R U .
N4 N 0.77420(16) 0.4711(5) 0.6501(3) 0.0480(12) Uani 1 1 d . . .
H4A H 0.7876 0.5373 0.6553 0.058 Uiso 1 1 calc R U .
O9 O 0.2715(4) 0.5565(9) 0.5834(6) 0.069(3) Uani 0.5 1 d . . P
C67 C 0.2410(6) 0.9493(14) 0.2644(9) 0.076(5) Uani 0.5 1 d . . P
H67A H 0.2550 0.9713 0.2329 0.114 Uiso 0.5 1 calc R U P
H67B H 0.2600 0.9709 0.3131 0.114 Uiso 0.5 1 calc R U P
H67C H 0.2126 0.9883 0.2498 0.114 Uiso 0.5 1 calc R U P
O10 O 0.2341(3) 0.8275(6) 0.2607(4) 0.0439(19) Uani 0.5 1 d . . P
H10 H 0.2559 0.7954 0.2920 0.066 Uiso 0.5 1 calc R U P
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'
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
C17 S1 C1 107.1(2) 2_656 .
C6 C1 C2 121.1(4) . .
C6 C1 S1 115.2(4) . .
C2 C1 S1 123.5(4) . .
C3 C2 C1 116.7(4) . .
C3 C2 S2 122.7(4) . .
C1 C2 S2 120.6(4) . .
C4 C3 C2 121.1(4) . .
C4 C3 S3 115.2(4) . .
C2 C3 S3 123.4(4) . .
C3 C4 C5 122.0(4) . .
C3 C4 H4 119.0 . .
C5 C4 H4 119.0 . .
C6 C5 C4 117.3(4) . .
C6 C5 C11 120.3(5) . .
C4 C5 C11 122.3(5) . .
C5 C6 C1 121.7(4) . .
C5 C6 H6 119.2 . .
C1 C6 H6 119.2 . .
C2 S2 C7 103.2(3) . .
C8 C7 S2 116.7(5) . .
C8 C7 H7A 108.1 . .
S2 C7 H7A 108.1 . .
C8 C7 H7B 108.1 . .
S2 C7 H7B 108.1 . .
H7A C7 H7B 107.3 . .
C9 C8 C7 120.1(7) . .
C9 C8 H8A 107.3 . .
C7 C8 H8A 107.3 . .
C9 C8 H8B 107.3 . .
C7 C8 H8B 107.3 . .
H8A C8 H8B 106.9 . .
C8 C9 C10 116.7(8) . .
C8 C9 H9A 108.1 . .
C10 C9 H9A 108.1 . .
C8 C9 H9B 108.1 . .
C10 C9 H9B 108.1 . .
H9A C9 H9B 107.3 . .
O1 C10 O2 126.4(6) . .
O1 C10 C9 121.2(7) . .
O2 C10 C9 111.4(7) . .
C13 C11 C14 109.1(8) . .
C13 C11 C5 110.8(5) . .
C14 C11 C5 107.5(6) . .
C13 C11 C12 109.6(7) . .
C14 C11 C12 108.4(6) . .
C5 C11 C12 111.5(5) . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.4 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C11 C13 H13A 109.5 . .
C11 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C11 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C11 C14 H14A 109.5 . .
C11 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C11 C14 H14C 109.4 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C3 S3 C15 105.6(2) . .
C16 C15 C20 120.5(4) . .
C16 C15 S3 124.7(4) . .
C20 C15 S3 114.6(4) . .
C15 C16 C17 118.1(4) . .
C15 C16 S4 121.9(4) . .
C17 C16 S4 120.0(4) . .
C18 C17 C16 120.1(4) . .
C18 C17 S1 115.4(4) . 2_656
C16 C17 S1 124.2(4) . 2_656
C19 C18 C17 122.1(5) . .
C19 C18 H18 119.0 . .
C17 C18 H18 119.0 . .
C18 C19 C20 117.6(4) . .
C18 C19 C25 120.3(5) . .
C20 C19 C25 121.8(5) . .
C19 C20 C15 121.5(5) . .
C19 C20 H20 119.2 . .
C15 C20 H20 119.2 . .
C16 S4 C21 100.9(3) . .
C22 C21 S4 112.7(4) . .
C22 C21 H21A 109.0 . .
S4 C21 H21A 109.0 . .
C22 C21 H21B 109.1 . .
S4 C21 H21B 109.0 . .
H21A C21 H21B 107.8 . .
C23 C22 C21 112.5(7) . .
C23 C22 H22A 109.1 . .
C21 C22 H22A 109.1 . .
C23 C22 H22B 109.1 . .
C21 C22 H22B 109.1 . .
H22A C22 H22B 107.8 . .
C22 C23 C24 120.2(8) . .
C22 C23 H23A 107.2 . .
C24 C23 H23A 107.3 . .
C22 C23 H23B 107.3 . .
C24 C23 H23B 107.3 . .
H23A C23 H23B 106.9 . .
O4 C24 O3 123.7(8) . .
O4 C24 C23 116.5(8) . .
O3 C24 C23 119.7(9) . .
C24 O3 H3 109.5 . .
C27 C25 C28 108.4(8) . .
C27 C25 C26 108.9(8) . .
C28 C25 C26 108.2(8) . .
C27 C25 C19 108.0(5) . .
C28 C25 C19 111.2(5) . .
C26 C25 C19 112.1(5) . .
C25 C26 H26A 109.5 . .
C25 C26 H26B 109.5 . .
H26A C26 H26B 109.5 . .
C25 C26 H26C 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
C25 C27 H27A 109.4 . .
C25 C27 H27B 109.6 . .
H27A C27 H27B 109.5 . .
C25 C27 H27C 109.5 . .
H27A C27 H27C 109.5 . .
H27B C27 H27C 109.5 . .
C25 C28 H28A 109.5 . .
C25 C28 H28B 109.5 . .
H28A C28 H28B 109.5 . .
C25 C28 H28C 109.5 . .
H28A C28 H28C 109.5 . .
H28B C28 H28C 109.5 . .
C29 S5 C45 106.1(2) . 2
C30 C29 C34 120.6(5) . .
C30 C29 S5 123.7(4) . .
C34 C29 S5 115.4(4) . .
C29 C30 C31 117.4(5) . .
C29 C30 S6 121.1(4) . .
C31 C30 S6 121.6(4) . .
C32 C31 C30 120.4(5) . .
C32 C31 S7 115.7(4) . .
C30 C31 S7 123.8(4) . .
C33 C32 C31 122.1(5) . .
C33 C32 H32 118.9 . .
C31 C32 H32 118.9 . .
C34 C33 C32 117.3(5) . .
C34 C33 C39 122.0(5) . .
C32 C33 C39 120.7(5) . .
C33 C34 C29 122.0(5) . .
C33 C34 H34 119.0 . .
C29 C34 H34 119.0 . .
C30 S6 C35 99.2(2) . .
C36 C35 S6 111.7(4) . .
C36 C35 H35A 109.2 . .
S6 C35 H35A 109.3 . .
C36 C35 H35B 109.3 . .
S6 C35 H35B 109.3 . .
H35A C35 H35B 107.9 . .
C35 C36 C37 113.5(5) . .
C35 C36 H36A 108.9 . .
C37 C36 H36A 108.9 . .
C35 C36 H36B 108.8 . .
C37 C36 H36B 108.9 . .
H36A C36 H36B 107.7 . .
C38 C37 C36 116.0(5) . .
C38 C37 H37A 108.3 . .
C36 C37 H37A 108.3 . .
C38 C37 H37B 108.3 . .
C36 C37 H37B 108.3 . .
H37A C37 H37B 107.4 . .
O6 C38 O5 125.0(6) . .
O6 C38 C37 121.3(5) . .
O5 C38 C37 113.4(6) . .
C38 O5 H5 109.5 . .
C42 C39 C41 112.9(8) . .
C42 C39 C33 108.6(5) . .
C41 C39 C33 112.6(5) . .
C42 C39 C40 109.6(9) . .
C41 C39 C40 106.7(7) . .
C33 C39 C40 106.2(5) . .
C39 C40 H40A 109.5 . .
C39 C40 H40B 109.5 . .
H40A C40 H40B 109.5 . .
C39 C40 H40C 109.5 . .
H40A C40 H40C 109.5 . .
H40B C40 H40C 109.5 . .
C39 C41 H41A 109.6 . .
C39 C41 H41B 109.4 . .
H41A C41 H41B 109.5 . .
C39 C41 H41C 109.5 . .
H41A C41 H41C 109.5 . .
H41B C41 H41C 109.5 . .
C39 C42 H42A 109.4 . .
C39 C42 H42B 109.6 . .
H42A C42 H42B 109.5 . .
C39 C42 H42C 109.4 . .
H42A C42 H42C 109.5 . .
H42B C42 H42C 109.5 . .
C31 S7 C43 106.7(2) . .
C48 C43 C44 120.5(5) . .
C48 C43 S7 115.3(4) . .
C44 C43 S7 124.0(4) . .
C45 C44 C43 117.0(5) . .
C45 C44 S8 122.1(4) . .
C43 C44 S8 120.9(4) . .
C44 C45 C46 121.7(5) . .
C44 C45 S5 124.0(4) . 2
C46 C45 S5 114.0(4) . 2
C47 C46 C45 121.2(5) . .
C47 C46 H46 119.4 . .
C45 C46 H46 119.4 . .
C48 C47 C46 117.3(4) . .
C48 C47 C53 120.8(5) . .
C46 C47 C53 121.7(5) . .
C47 C48 C43 122.3(5) . .
C47 C48 H48 118.8 . .
C43 C48 H48 118.8 . .
C44 S8 C49 99.5(3) . .
C50 C49 S8 113.0(4) . .
C50 C49 H49A 109.0 . .
S8 C49 H49A 109.0 . .
C50 C49 H49B 109.0 . .
S8 C49 H49B 109.0 . .
H49A C49 H49B 107.8 . .
C49 C50 C51 110.6(7) . .
C49 C50 H50A 109.5 . .
C51 C50 H50A 109.5 . .
C49 C50 H50B 109.6 . .
C51 C50 H50B 109.5 . .
H50A C50 H50B 108.1 . .
C52 C51 C50 114.8(7) . .
C52 C51 H51A 108.6 . .
C50 C51 H51A 108.6 . .
C52 C51 H51B 108.6 . .
C50 C51 H51B 108.6 . .
H51A C51 H51B 107.6 . .
O7 C52 O8 122.7(7) . .
O7 C52 C51 125.5(7) . .
O8 C52 C51 111.7(6) . .
C52 O8 H8D 109.5 . .
C56 C53 C55 110.3(8) . .
C56 C53 C54 111.8(8) . .
C55 C53 C54 106.0(7) . .
C56 C53 C47 109.3(5) . .
C55 C53 C47 107.2(5) . .
C54 C53 C47 112.1(5) . .
C53 C54 H54A 109.4 . .
C53 C54 H54B 109.5 . .
H54A C54 H54B 109.5 . .
C53 C54 H54C 109.5 . .
H54A C54 H54C 109.5 . .
H54B C54 H54C 109.5 . .
C53 C55 H55A 109.4 . .
C53 C55 H55B 109.6 . .
H55A C55 H55B 109.5 . .
C53 C55 H55C 109.4 . .
H55A C55 H55C 109.5 . .
H55B C55 H55C 109.5 . .
C53 C56 H56A 109.4 . .
C53 C56 H56B 109.4 . .
H56A C56 H56B 109.5 . .
C53 C56 H56C 109.6 . .
H56A C56 H56C 109.5 . .
H56B C56 H56C 109.5 . .
N2 C57 N1 122.4(6) . .
N2 C57 C61 118.6(6) . .
N1 C57 C61 118.9(6) . .
C57 N1 C58 122.2(6) . .
C57 N1 H1 118.9 . .
C58 N1 H1 118.9 . .
N1 C58 C59 108.6(6) . .
N1 C58 H58A 110.0 . .
C59 C58 H58A 110.0 . .
N1 C58 H58B 110.0 . .
C59 C58 H58B 109.9 . .
H58A C58 H58B 108.4 . .
C60 C59 C58 109.8(7) . .
C60 C59 H59A 109.7 . .
C58 C59 H59A 109.7 . .
C60 C59 H59B 109.7 . .
C58 C59 H59B 109.7 . .
H59A C59 H59B 108.2 . .
N2 C60 C59 110.8(6) . .
N2 C60 H60A 109.4 . .
C59 C60 H60A 109.4 . .
N2 C60 H60B 109.6 . .
C59 C60 H60B 109.5 . .
H60A C60 H60B 108.1 . .
C57 N2 C60 121.7(6) . .
C57 N2 H2 119.1 . .
C60 N2 H2 119.2 . .
C57 C61 C62 110.9(5) . .
C57 C61 H61A 109.4 . .
C62 C61 H61A 109.4 . .
C57 C61 H61B 109.5 . .
C62 C61 H61B 109.5 . .
H61A C61 H61B 108.0 . .
C63 C62 C61 113.3(5) . .
C63 C62 H62A 108.9 . .
C61 C62 H62A 109.0 . .
C63 C62 H62B 108.8 . .
C61 C62 H62B 108.9 . .
H62A C62 H62B 107.8 . .
N4 C63 N3 121.8(6) . .
N4 C63 C62 119.8(5) . .
N3 C63 C62 118.4(5) . .
C63 N3 C64 122.7(6) . .
C63 N3 H3A 118.6 . .
C64 N3 H3A 118.7 . .
N3 C64 C65 109.8(6) . .
N3 C64 H64A 109.7 . .
C65 C64 H64A 109.8 . .
N3 C64 H64B 109.7 . .
C65 C64 H64B 109.7 . .
H64A C64 H64B 108.2 . .
C64 C65 C66 109.9(6) . .
C64 C65 H65A 109.7 . .
C66 C65 H65A 109.6 . .
C64 C65 H65B 109.7 . .
C66 C65 H65B 109.7 . .
H65A C65 H65B 108.2 . .
N4 C66 C65 109.5(5) . .
N4 C66 H66A 109.7 . .
C65 C66 H66A 109.7 . .
N4 C66 H66B 109.8 . .
C65 C66 H66B 109.8 . .
H66A C66 H66B 108.3 . .
C63 N4 C66 121.8(5) . .
C63 N4 H4A 119.1 . .
C66 N4 H4A 119.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 C17 1.771(5) 2_656
S1 C1 1.771(5) .
C1 C6 1.393(7) .
C1 C2 1.408(7) .
C2 C3 1.401(7) .
C2 S2 1.771(5) .
C3 C4 1.385(7) .
C3 S3 1.770(5) .
C4 C5 1.389(7) .
C4 H4 0.9500 .
C5 C6 1.380(7) .
C5 C11 1.536(7) .
C6 H6 0.9500 .
S2 C7 1.822(9) .
C7 C8 1.464(11) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 C9 1.450(10) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 C10 1.513(11) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 O1 1.211(9) .
C10 O2 1.266(8) .
C11 C13 1.469(10) .
C11 C14 1.532(11) .
C11 C12 1.538(9) .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 H13A 0.9802 .
C13 H13B 0.9802 .
C13 H13C 0.9802 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
S3 C15 1.777(5) .
C15 C16 1.388(7) .
C15 C20 1.400(7) .
C16 C17 1.409(6) .
C16 S4 1.773(5) .
C17 C18 1.392(7) .
C17 S1 1.771(5) 2_656
C18 C19 1.381(7) .
C18 H18 0.9500 .
C19 C20 1.387(7) .
C19 C25 1.533(7) .
C20 H20 0.9500 .
S4 C21 1.816(6) .
C21 C22 1.576(10) .
C21 H21A 0.9900 .
C21 H21B 0.9900 .
C22 C23 1.441(11) .
C22 H22A 0.9900 .
C22 H22B 0.9900 .
C23 C24 1.493(10) .
C23 H23A 0.9900 .
C23 H23B 0.9900 .
C24 O4 1.210(11) .
C24 O3 1.295(11) .
O3 H3 0.8400 .
C25 C27 1.498(9) .
C25 C28 1.498(9) .
C25 C26 1.520(10) .
C26 H26A 0.9801 .
C26 H26B 0.9801 .
C26 H26C 0.9801 .
C27 H27A 0.9801 .
C27 H27B 0.9802 .
C27 H27C 0.9801 .
C28 H28A 0.9800 .
C28 H28B 0.9800 .
C28 H28C 0.9800 .
S5 C29 1.764(5) .
S5 C45 1.789(5) 2
C29 C30 1.397(7) .
C29 C34 1.403(7) .
C30 C31 1.407(7) .
C30 S6 1.770(5) .
C31 C32 1.393(7) .
C31 S7 1.776(5) .
C32 C33 1.386(7) .
C32 H32 0.9500 .
C33 C34 1.377(8) .
C33 C39 1.543(7) .
C34 H34 0.9500 .
S6 C35 1.818(5) .
C35 C36 1.505(8) .
C35 H35A 0.9900 .
C35 H35B 0.9900 .
C36 C37 1.528(8) .
C36 H36A 0.9900 .
C36 H36B 0.9900 .
C37 C38 1.496(8) .
C37 H37A 0.9900 .
C37 H37B 0.9900 .
C38 O6 1.219(8) .
C38 O5 1.291(8) .
C39 C42 1.484(11) .
C39 C41 1.490(10) .
C39 C40 1.547(10) .
C40 H40A 0.9800 .
C40 H40B 0.9800 .
C40 H40C 0.9800 .
C41 H41A 0.9800 .
C41 H41B 0.9800 .
C41 H41C 0.9800 .
C42 H42A 0.9800 .
C42 H42B 0.9800 .
C42 H42C 0.9800 .
S7 C43 1.780(5) .
C43 C48 1.391(7) .
C43 C44 1.405(6) .
C44 C45 1.390(7) .
C44 S8 1.766(5) .
C45 C46 1.394(7) .
C45 S5 1.789(5) 2
C46 C47 1.386(7) .
C46 H46 0.9500 .
C47 C48 1.381(7) .
C47 C53 1.527(7) .
C48 H48 0.9500 .
S8 C49 1.825(8) .
C49 C50 1.520(11) .
C49 H49A 0.9900 .
C49 H49B 0.9900 .
C50 C51 1.531(10) .
C50 H50A 0.9900 .
C50 H50B 0.9900 .
C51 C52 1.489(10) .
C51 H51A 0.9900 .
C51 H51B 0.9900 .
C52 O7 1.204(9) .
C52 O8 1.316(8) .
O8 H8D 0.8400 .
C53 C56 1.497(10) .
C53 C55 1.511(9) .
C53 C54 1.519(10) .
C54 H54A 0.9800 .
C54 H54B 0.9800 .
C54 H54C 0.9800 .
C55 H55A 0.9800 .
C55 H55B 0.9800 .
C55 H55C 0.9800 .
C56 H56A 0.9800 .
C56 H56B 0.9800 .
C56 H56C 0.9800 .
C57 N2 1.300(9) .
C57 N1 1.320(9) .
C57 C61 1.500(9) .
N1 C58 1.458(9) .
N1 H1 0.8800 .
C58 C59 1.520(12) .
C58 H58A 0.9900 .
C58 H58B 0.9900 .
C59 C60 1.485(10) .
C59 H59A 0.9900 .
C59 H59B 0.9900 .
C60 N2 1.450(9) .
C60 H60A 0.9900 .
C60 H60B 0.9900 .
N2 H2 0.8800 .
C61 C62 1.536(8) .
C61 H61A 0.9900 .
C61 H61B 0.9900 .
C62 C63 1.490(8) .
C62 H62A 0.9900 .
C62 H62B 0.9900 .
C63 N4 1.300(8) .
C63 N3 1.304(8) .
N3 C64 1.442(8) .
N3 H3A 0.8800 .
C64 C65 1.484(11) .
C64 H64A 0.9900 .
C64 H64B 0.9900 .
C65 C66 1.491(9) .
C65 H65A 0.9900 .
C65 H65B 0.9900 .
C66 N4 1.473(8) .
C66 H66A 0.9900 .
C66 H66B 0.9900 .
N4 H4A 0.8800 .
