#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:41:12 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180232 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/18/7111815.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_7111815
loop_
_publ_author_name
'Vaclav Havel'
'Vladimir Sindelar'
'Marek Necas'
'Angel E. Kaifer'
_publ_section_title
;
 Water-mediated inclusion of benzoates and tosylates inside the bambusuril
 macrocycle
;
_journal_name_full               Chem.Commun.
_journal_page_first              1372
_journal_paper_doi               10.1039/c3cc47828a
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C168 H214 N26 O20'
_chemical_formula_weight         2917.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 107.271(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.7270(4)
_cell_length_b                   20.2092(5)
_cell_length_c                   22.9150(6)
_cell_measurement_reflns_used    15510
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.2684
_cell_measurement_theta_min      2.8713
_cell_volume                     7839.1(4)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction Ltd, 2009)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction Ltd, 2009)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction Ltd, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.4353
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_sigmaI/netI    0.0942
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            79854
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.88
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99448
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis RED (Oxford Diffraction Ltd, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3128
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.806
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1005
_refine_ls_number_reflns         13765
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      0.818
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0433
_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)+(0.0537P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.1022
_reflns_number_gt                7065
_reflns_number_total             13765
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc47828a.txt
_cod_data_source_block           vs29
_cod_original_cell_volume        7839.1(3)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7111815
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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 0.25401(8) 0.92277(7) 0.37134(6) 0.0277(4) Uani 1 1 d . . .
O2 O 0.49584(9) 0.81737(8) 0.25312(7) 0.0401(4) Uani 1 1 d . . .
O3 O 0.47658(8) 0.74463(7) 0.51147(6) 0.0289(4) Uani 1 1 d . . .
O4 O 0.21390(8) 0.84786(8) 0.61258(7) 0.0404(4) Uani 1 1 d . . .
O5 O 0.57332(8) 0.89377(7) 0.72218(6) 0.0281(4) Uani 1 1 d . . .
O6 O 0.81741(8) 0.79599(8) 0.59817(7) 0.0375(4) Uani 1 1 d . . .
O81 O 0.62333(12) 0.99977(9) 0.38318(9) 0.0675(6) Uani 1 1 d . . .
O82 O 0.61138(10) 0.95870(9) 0.46949(8) 0.0526(5) Uani 1 1 d . . .
N1 N 0.35861(9) 0.95444(9) 0.33749(8) 0.0266(4) Uani 1 1 d . . .
N2 N 0.37042(10) 0.86396(9) 0.39366(8) 0.0269(5) Uani 1 1 d . . .
N3 N 0.45623(10) 0.91288(9) 0.29029(8) 0.0293(5) Uani 1 1 d . . .
N4 N 0.46179(10) 0.81908(9) 0.34272(8) 0.0263(4) Uani 1 1 d . . .
N5 N 0.37474(9) 0.82047(8) 0.49343(7) 0.0246(4) Uani 1 1 d . . .
N6 N 0.44968(9) 0.80530(8) 0.58857(7) 0.0229(4) Uani 1 1 d . . .
N7 N 0.26876(9) 0.85767(9) 0.53373(8) 0.0266(4) Uani 1 1 d . . .
N8 N 0.34832(10) 0.85036(9) 0.62862(8) 0.0298(5) Uani 1 1 d . . .
N9 N 0.58648(9) 0.83286(9) 0.64044(7) 0.0232(4) Uani 1 1 d . . .
N10 N 0.65517(9) 0.92562(9) 0.66529(7) 0.0228(4) Uani 1 1 d . . .
N11 N 0.68655(10) 0.79277(9) 0.59598(8) 0.0270(4) Uani 1 1 d . . .
N12 N 0.75055(9) 0.88938(9) 0.61347(8) 0.0268(4) Uani 1 1 d . . .
N60 N 0.02248(10) 0.74620(10) 0.58969(8) 0.0349(5) Uani 1 1 d . B .
C1 C 0.32107(12) 0.91452(11) 0.36791(9) 0.0248(5) Uani 1 1 d . . .
C2 C 0.47350(12) 0.84661(12) 0.29163(11) 0.0311(6) Uani 1 1 d . . .
C3 C 0.43993(12) 0.93402(11) 0.34544(9) 0.0263(5) Uani 1 1 d . . .
H3A H 0.4786 0.9681 0.3679 0.032 Uiso 1 1 calc R . .
C4 C 0.44659(12) 0.86872(11) 0.38317(10) 0.0259(5) Uani 1 1 d . . .
H4A H 0.4904 0.8711 0.4224 0.031 Uiso 1 1 calc R . .
C5 C 0.43785(12) 0.78601(11) 0.52932(10) 0.0234(5) Uani 1 1 d . . .
C6 C 0.27148(13) 0.85174(11) 0.59376(11) 0.0308(6) Uani 1 1 d . . .
C7 C 0.34653(11) 0.87042(11) 0.52721(9) 0.0240(5) Uani 1 1 d . . .
H7A H 0.3501 0.9158 0.5108 0.029 Uiso 1 1 calc R . .
C8 C 0.40183(11) 0.86264(11) 0.59314(9) 0.0247(5) Uani 1 1 d . . .
H8A H 0.4348 0.9030 0.6074 0.030 Uiso 1 1 calc R . .
C9 C 0.60173(11) 0.88520(11) 0.68012(10) 0.0234(5) Uani 1 1 d . . .
C10 C 0.75751(13) 0.82315(12) 0.60235(10) 0.0297(6) Uani 1 1 d . . .
C11 C 0.62431(12) 0.84012(10) 0.59315(10) 0.0254(5) Uani 1 1 d . . .
H11A H 0.5848 0.8411 0.5517 0.030 Uiso 1 1 calc R . .
C12 C 0.66928(11) 0.90661(11) 0.60831(9) 0.0240(5) Uani 1 1 d . . .
H12A H 0.6480 0.9403 0.5756 0.029 Uiso 1 1 calc R . .
C13 C 0.48574(13) 0.95691(11) 0.25163(10) 0.0328(6) Uani 1 1 d . . .
H13A H 0.5356 0.9383 0.2476 0.039 Uiso 1 1 calc R . .
H13B H 0.4984 1.0002 0.2725 0.039 Uiso 1 1 calc R . .
C14 C 0.43025(12) 0.96859(11) 0.18843(10) 0.0291(6) Uani 1 1 d . . .
C15 C 0.35361(13) 0.94370(12) 0.16879(11) 0.0370(6) Uani 1 1 d . . .
H15A H 0.3351 0.9159 0.1951 0.044 Uiso 1 1 calc R . .
C16 C 0.30433(14) 0.95909(13) 0.11153(11) 0.0435(7) Uani 1 1 d . . .
H16A H 0.2518 0.9425 0.0990 0.052 Uiso 1 1 calc R . .
C17 C 0.33043(15) 0.99824(12) 0.07226(12) 0.0434(7) Uani 1 1 d . . .
H17A H 0.2961 1.0090 0.0330 0.052 Uiso 1 1 calc R . .
C18 C 0.40710(15) 1.02159(12) 0.09070(11) 0.0424(7) Uani 1 1 d . . .
H18A H 0.4261 1.0479 0.0637 0.051 Uiso 1 1 calc R . .
C19 C 0.45608(14) 1.00677(12) 0.14813(11) 0.0376(6) Uani 1 1 d . . .
H19A H 0.5087 1.0231 0.1603 0.045 Uiso 1 1 calc R . .
C20 C 0.48651(13) 0.75195(11) 0.36134(11) 0.0338(6) Uani 1 1 d . . .
H20A H 0.5168 0.7522 0.4053 0.041 Uiso 1 1 calc R . .
H20B H 0.5226 0.7368 0.3383 0.041 Uiso 1 1 calc R . .
C21 C 0.41932(13) 0.70280(11) 0.35143(10) 0.0305(6) Uani 1 1 d . . .
C22 C 0.35024(14) 0.71079(12) 0.30440(10) 0.0378(6) Uani 1 1 d . . .
H22A H 0.3457 0.7464 0.2765 0.045 Uiso 1 1 calc R . .
C23 C 0.28742(16) 0.66770(14) 0.29723(12) 0.0494(7) Uani 1 1 d . . .
H23A H 0.2400 0.6741 0.2649 0.059 Uiso 1 1 calc R . .
C24 C 0.29361(18) 0.61537(14) 0.33712(13) 0.0561(8) Uani 1 1 d . . .
H24A H 0.2505 0.5859 0.3324 0.067 Uiso 1 1 calc R . .
C25 C 0.36230(18) 0.60616(13) 0.38357(13) 0.0524(8) Uani 1 1 d . . .
H25A H 0.3672 0.5697 0.4106 0.063 Uiso 1 1 calc R . .
C26 C 0.42448(15) 0.64998(12) 0.39108(11) 0.0415(7) Uani 1 1 d . . .
H26A H 0.4714 0.6438 0.4239 0.050 Uiso 1 1 calc R . .
C27 C 0.34646(12) 0.81203(11) 0.42800(9) 0.0256(5) Uani 1 1 d . . .
H27A H 0.2880 0.8100 0.4153 0.031 Uiso 1 1 calc R . .
H27B H 0.3660 0.7691 0.4174 0.031 Uiso 1 1 calc R . .
C28 C 0.19562(12) 0.86924(11) 0.48557(10) 0.0298(6) Uani 1 1 d . . .
H28A H 0.2041 0.9054 0.4590 0.036 Uiso 1 1 calc R . .
H28B H 0.1549 0.8842 0.5043 0.036 Uiso 1 1 calc R . .
C29 C 0.16503(12) 0.80904(12) 0.44651(10) 0.0291(6) Uani 1 1 d . . .
C30 C 0.18079(13) 0.74590(13) 0.46927(11) 0.0376(6) Uani 1 1 d . . .
H30A H 0.2097 0.7395 0.5110 0.045 Uiso 1 1 calc R . .
C31 C 0.15498(15) 0.69164(14) 0.43200(13) 0.0520(7) Uani 1 1 d . . .
H31A H 0.1665 0.6483 0.4484 0.062 Uiso 1 1 calc R . .
C32 C 0.11292(15) 0.69958(16) 0.37163(14) 0.0575(8) Uani 1 1 d . . .
H32A H 0.0956 0.6621 0.3461 0.069 Uiso 1 1 calc R . .
C33 C 0.09624(15) 0.76237(16) 0.34863(13) 0.0534(8) Uani 1 1 d . . .
H33A H 0.0667 0.7684 0.3070 0.064 Uiso 1 1 calc R . .
C34 C 0.12209(13) 0.81683(13) 0.38557(11) 0.0400(6) Uani 1 1 d . . .
H34A H 0.1103 0.8601 0.3691 0.048 Uiso 1 1 calc R . .
C35 C 0.36976(13) 0.86141(12) 0.69423(10) 0.0392(7) Uani 1 1 d . . .
H35A H 0.3292 0.8901 0.7031 0.047 Uiso 1 1 calc R . .
H35B H 0.4206 0.8856 0.7071 0.047 Uiso 1 1 calc R . .
C36 C 0.37771(12) 0.79959(14) 0.73189(11) 0.0364(6) Uani 1 1 d . . .
C37 C 0.39105(15) 0.80600(16) 0.79431(12) 0.0575(8) Uani 1 1 d . . .
H37A H 0.3949 0.8488 0.8121 0.069 Uiso 1 1 calc R . .
C38 C 0.39885(18) 0.7506(2) 0.83084(14) 0.0755(11) Uani 1 1 d . . .
H38A H 0.4082 0.7558 0.8736 0.091 Uiso 1 1 calc R . .
C39 C 0.39343(16) 0.6886(2) 0.80658(15) 0.0670(9) Uani 1 1 d . . .
H39A H 0.3982 0.6508 0.8321 0.080 Uiso 1 1 calc R . .
C40 C 0.38099(15) 0.68127(16) 0.74511(14) 0.0595(8) Uani 1 1 d . . .
H40A H 0.3780 0.6383 0.7278 0.071 Uiso 1 1 calc R . .
C41 C 0.37274(14) 0.73719(15) 0.70788(12) 0.0478(7) Uani 1 1 d . . .
H41A H 0.3635 0.7318 0.6651 0.057 Uiso 1 1 calc R . .
C42 C 0.52132(11) 0.78800(11) 0.63596(9) 0.0254(5) Uani 1 1 d . . .
H42A H 0.5375 0.7428 0.6280 0.030 Uiso 1 1 calc R . .
H42B H 0.5099 0.7871 0.6757 0.030 Uiso 1 1 calc R . .
C43 C 0.67266(13) 0.72398(11) 0.57815(10) 0.0314(6) Uani 1 1 d . . .
H43A H 0.7175 0.7076 0.5648 0.038 Uiso 1 1 calc R . .
H43B H 0.6244 0.7210 0.5428 0.038 Uiso 1 1 calc R . .
C44 C 0.66298(12) 0.67959(11) 0.62857(10) 0.0282(6) Uani 1 1 d . . .
C45 C 0.61466(13) 0.62461(12) 0.61573(11) 0.0378(6) Uani 1 1 d . . .
H45A H 0.5867 0.6143 0.5745 0.045 Uiso 1 1 calc R . .
C46 C 0.60668(14) 0.58434(13) 0.66241(13) 0.0447(7) Uani 1 1 d . . .
H46A H 0.5737 0.5464 0.6529 0.054 Uiso 1 1 calc R . .
C47 C 0.64584(14) 0.59866(13) 0.72234(13) 0.0443(7) Uani 1 1 d . . .
H47A H 0.6397 0.5712 0.7543 0.053 Uiso 1 1 calc R . .
C48 C 0.69410(14) 0.65340(13) 0.73549(12) 0.0460(7) Uani 1 1 d . . .
H48A H 0.7214 0.6640 0.7768 0.055 Uiso 1 1 calc R . .
C49 C 0.70293(13) 0.69302(12) 0.68877(11) 0.0378(6) Uani 1 1 d . . .
H49A H 0.7372 0.7302 0.6984 0.045 Uiso 1 1 calc R . .
C50 C 0.80470(12) 0.93562(11) 0.59801(10) 0.0308(6) Uani 1 1 d . . .
H50A H 0.7755 0.9768 0.5822 0.037 Uiso 1 1 calc R . .
H50B H 0.8223 0.9162 0.5645 0.037 Uiso 1 1 calc R . .
C51 C 0.87676(12) 0.95345(11) 0.64979(11) 0.0294(6) Uani 1 1 d . . .
C52 C 0.93213(14) 0.99609(12) 0.63879(12) 0.0431(7) Uani 1 1 d . . .
H52A H 0.9252 1.0122 0.5986 0.052 Uiso 1 1 calc R . .
C53 C 0.99718(15) 1.01542(14) 0.68563(14) 0.0558(8) Uani 1 1 d . . .
H53A H 1.0345 1.0450 0.6775 0.067 Uiso 1 1 calc R . .
C54 C 1.00844(14) 0.99221(13) 0.74416(13) 0.0472(7) Uani 1 1 d . . .
H54A H 1.0531 1.0059 0.7764 0.057 Uiso 1 1 calc R . .
C55 C 0.95501(14) 0.94940(12) 0.75539(12) 0.0420(7) Uani 1 1 d . . .
H55A H 0.9626 0.9328 0.7955 0.050 Uiso 1 1 calc R . .
C56 C 0.88956(13) 0.93004(11) 0.70826(11) 0.0350(6) Uani 1 1 d . . .
H56A H 0.8528 0.9000 0.7165 0.042 Uiso 1 1 calc R . .
C57 C 0.67926(12) 0.98777(11) 0.69595(10) 0.0264(5) Uani 1 1 d . . .
H57A H 0.7371 0.9924 0.7044 0.032 Uiso 1 1 calc R . .
H57B H 0.6681 0.9866 0.7358 0.032 Uiso 1 1 calc R . .
C61 C 0.01372(14) 0.77797(13) 0.64779(11) 0.0420(7) Uani 1 1 d . . .
H61A H -0.0391 0.7988 0.6380 0.050 Uiso 1 1 calc R A 1
H61B H 0.0156 0.7426 0.6781 0.050 Uiso 1 1 calc R A 1
C62A C 0.07543(16) 0.82964(15) 0.67721(12) 0.0595(9) Uani 0.464(8) 1 d PD B 1
H62A H 0.0971 0.8463 0.6448 0.071 Uiso 0.464(8) 1 calc PR B 1
H62B H 0.0470 0.8671 0.6890 0.071 Uiso 0.464(8) 1 calc PR B 1
C63A C 0.1386(4) 0.8155(3) 0.7268(3) 0.047(2) Uani 0.464(8) 1 d PDU B 1
H63A H 0.1756 0.7869 0.7134 0.056 Uiso 0.464(8) 1 calc PR B 1
H63B H 0.1195 0.7898 0.7564 0.056 Uiso 0.464(8) 1 calc PR B 1
C64A C 0.1841(9) 0.8760(9) 0.7598(7) 0.065(4) Uani 0.464(8) 1 d PDU B 1
H64A H 0.2061 0.9005 0.7317 0.098 Uiso 0.464(8) 1 calc PR B 1
H64B H 0.2271 0.8613 0.7952 0.098 Uiso 0.464(8) 1 calc PR B 1
H64C H 0.1482 0.9048 0.7735 0.098 Uiso 0.464(8) 1 calc PR B 1
C62B C 0.07543(16) 0.82964(15) 0.67721(12) 0.0595(9) Uani 0.536(8) 1 d PD B 2
H62C H 0.0550 0.8739 0.6618 0.071 Uiso 0.536(8) 1 calc PR B 2
H62D H 0.1235 0.8214 0.6648 0.071 Uiso 0.536(8) 1 calc PR B 2
C63B C 0.0976(4) 0.8297(3) 0.7465(2) 0.0452(18) Uani 0.536(8) 1 d PDU B 2
H63C H 0.0512 0.8438 0.7591 0.054 Uiso 0.536(8) 1 calc PR B 2
H63D H 0.1114 0.7841 0.7617 0.054 Uiso 0.536(8) 1 calc PR B 2
C64B C 0.1665(7) 0.8752(7) 0.7760(6) 0.061(3) Uani 0.536(8) 1 d PDU B 2
H64D H 0.2158 0.8543 0.7747 0.092 Uiso 0.536(8) 1 calc PR B 2
H64E H 0.1686 0.8834 0.8186 0.092 Uiso 0.536(8) 1 calc PR B 2
H64F H 0.1595 0.9173 0.7537 0.092 Uiso 0.536(8) 1 calc PR B 2
C65 C -0.04865(13) 0.70178(12) 0.56556(11) 0.0378(6) Uani 1 1 d . . .
H65A H -0.0966 0.7298 0.5526 0.045 Uiso 1 1 calc R B .
H65B H -0.0535 0.6732 0.5993 0.045 Uiso 1 1 calc R . .
C66 C -0.04635(13) 0.65791(13) 0.51209(11) 0.0455(7) Uani 1 1 d D B .
H66A H -0.0279 0.6841 0.4825 0.055 Uiso 1 1 calc R . .
H66B H -0.0084 0.6213 0.5271 0.055 Uiso 1 1 calc R . .
C67 C -0.12712(14) 0.62962(13) 0.48044(12) 0.0489(7) Uani 1 1 d D . .
H67A H -0.1623 0.6659 0.4594 0.059 Uiso 1 1 calc R B .
H67B H -0.1495 0.6108 0.5116 0.059 Uiso 1 1 calc R . .
C68 C -0.12581(17) 0.57637(15) 0.43427(12) 0.0667(9) Uani 1 1 d D B .
H68A H -0.1800 0.5621 0.4134 0.100 Uiso 1 1 calc R . .
H68B H -0.0950 0.5385 0.4553 0.100 Uiso 1 1 calc R . .
H68C H -0.1016 0.5940 0.4042 0.100 Uiso 1 1 calc R . .
C69 C 0.09846(13) 0.70787(13) 0.60225(11) 0.0406(7) Uani 1 1 d . . .
H69A H 0.1429 0.7392 0.6176 0.049 Uiso 1 1 calc R B .
H69B H 0.1021 0.6898 0.5630 0.049 Uiso 1 1 calc R . .
C70 C 0.10942(14) 0.65105(13) 0.64768(11) 0.0436(7) Uani 1 1 d D B .
H70A H 0.0620 0.6224 0.6367 0.052 Uiso 1 1 calc R . .
H70B H 0.1169 0.6687 0.6893 0.052 Uiso 1 1 calc R . .
C71 C 0.18211(14) 0.61081(14) 0.64611(12) 0.0540(8) Uani 1 1 d D . .
H71A H 0.1727 0.5920 0.6047 0.065 Uiso 1 1 calc R B .
H71B H 0.2281 0.6409 0.6538 0.065 Uiso 1 1 calc R . .
C72 C 0.20242(18) 0.55433(15) 0.69294(13) 0.0723(9) Uani 1 1 d D B .
H72A H 0.2481 0.5298 0.6886 0.108 Uiso 1 1 calc R . .
H72B H 0.1571 0.5244 0.6859 0.108 Uiso 1 1 calc R . .
H72C H 0.2150 0.5727 0.7343 0.108 Uiso 1 1 calc R . .
C73 C 0.02559(13) 0.79850(12) 0.54294(10) 0.0352(6) Uani 1 1 d . . .
H73A H 0.0320 0.7757 0.5065 0.042 Uiso 1 1 calc R B .
H73B H 0.0735 0.8257 0.5603 0.042 Uiso 1 1 calc R . .
C74 C -0.04501(13) 0.84503(12) 0.52195(11) 0.0418(7) Uani 1 1 d D B .
H74A H -0.0932 0.8191 0.5020 0.050 Uiso 1 1 calc R . .
H74B H -0.0532 0.8678 0.5578 0.050 Uiso 1 1 calc R . .
C75 C -0.03162(14) 0.89578(12) 0.47750(11) 0.0433(7) Uani 1 1 d D . .
H75A H -0.0182 0.8726 0.4439 0.052 Uiso 1 1 calc R B .
H75B H 0.0140 0.9238 0.4988 0.052 Uiso 1 1 calc R . .
C76 C -0.10280(14) 0.93972(13) 0.45062(12) 0.0536(8) Uani 1 1 d D B .
H76A H -0.0911 0.9709 0.4218 0.080 Uiso 1 1 calc R . .
H76B H -0.1152 0.9643 0.4835 0.080 Uiso 1 1 calc R . .
H76C H -0.1482 0.9123 0.4292 0.080 Uiso 1 1 calc R . .
C80 C 0.66597(12) 0.89075(12) 0.40692(10) 0.0317(6) Uani 1 1 d . . .
C81 C 0.68304(15) 0.83915(14) 0.44871(12) 0.0502(7) Uani 1 1 d . . .
H81A H 0.6724 0.8445 0.4867 0.060 Uiso 1 1 calc R . .
C82 C 0.71499(17) 0.78047(15) 0.43669(13) 0.0592(8) Uani 1 1 d . . .
H82A H 0.7278 0.7463 0.4664 0.071 Uiso 1 1 calc R . .
C83 C 0.72803(16) 0.77217(14) 0.38083(14) 0.0558(8) Uani 1 1 d . . .
H83A H 0.7490 0.7316 0.3714 0.067 Uiso 1 1 calc R . .
C84 C 0.71076(15) 0.82244(15) 0.33890(12) 0.0548(8) Uani 1 1 d . . .
H84A H 0.7200 0.8166 0.3005 0.066 Uiso 1 1 calc R . .
C85 C 0.68016(13) 0.88125(13) 0.35185(11) 0.0391(6) Uani 1 1 d . . .
H85A H 0.6687 0.9157 0.3223 0.047 Uiso 1 1 calc R . .
C86 C 0.63177(13) 0.95459(14) 0.42150(12) 0.0391(6) Uani 1 1 d . . .
C91 C 0.6575(3) 0.36489(17) 0.4488(2) 0.1317(18) Uani 1 1 d . . .
H91A H 0.6247 0.3254 0.4362 0.198 Uiso 1 1 calc R . .
H91B H 0.6868 0.3616 0.4923 0.198 Uiso 1 1 calc R . .
H91C H 0.6948 0.3683 0.4248 0.198 Uiso 1 1 calc R . .
C92 C 0.60957(18) 0.42081(18) 0.43895(16) 0.0820(11) Uani 1 1 d . . .
H92A H 0.5720 0.4176 0.3973 0.098 Uiso 1 1 calc R . .
H92B H 0.5781 0.4194 0.4681 0.098 Uiso 1 1 calc R . .
O93 O 0.64573(12) 0.48146(11) 0.44431(10) 0.0796(7) Uani 1 1 d . . .
C94 C 0.6040(2) 0.53798(18) 0.43917(18) 0.0966(12) Uani 1 1 d . . .
H94A H 0.5774 0.5382 0.4715 0.116 Uiso 1 1 calc R . .
H94B H 0.5622 0.5373 0.3994 0.116 Uiso 1 1 calc R . .
C95 C 0.64675(19) 0.59835(16) 0.44318(16) 0.0885(11) Uani 1 1 d . . .
H95A H 0.6096 0.6354 0.4327 0.133 Uiso 1 1 calc R . .
H95B H 0.6783 0.5971 0.4146 0.133 Uiso 1 1 calc R . .
H95C H 0.6817 0.6040 0.4849 0.133 Uiso 1 1 calc R . .
O100 O 0.49927(18) 0.94374(16) 0.52955(14) 0.0361(8) Uani 0.50 1 d PDU . .
H101 H 0.475(2) 0.9827(12) 0.5297(19) 0.054 Uiso 0.50 1 d PD . .
H102 H 0.509(2) 0.953(2) 0.4949(11) 0.054 Uiso 0.50 1 d PD . .
O101 O 0.2275(4) 0.9829(3) 0.6679(3) 0.176(3) Uani 0.50 1 d 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'
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 C57 121.90(17) . 3_676
C1 N1 C3 112.56(18) . .
C57 N1 C3 125.47(17) 3_676 .
C1 N2 C4 112.99(17) . .
C1 N2 C27 121.68(17) . .
C4 N2 C27 125.32(16) . .
C2 N3 C3 111.77(18) . .
C2 N3 C13 119.44(19) . .
C3 N3 C13 123.57(18) . .
C2 N4 C4 111.82(18) . .
C2 N4 C20 121.56(19) . .
C4 N4 C20 123.95(18) . .
C5 N5 C27 122.35(17) . .
C5 N5 C7 112.61(17) . .
C27 N5 C7 124.69(17) . .
C5 N6 C42 121.19(17) . .
C5 N6 C8 112.14(17) . .
C42 N6 C8 122.52(17) . .
C6 N7 C28 122.42(17) . .
C6 N7 C7 111.58(17) . .
C28 N7 C7 123.66(17) . .
C6 N8 C8 112.16(17) . .
C6 N8 C35 120.86(18) . .
C8 N8 C35 122.86(17) . .
C9 N9 C11 112.13(17) . .
C9 N9 C42 121.82(17) . .
C11 N9 C42 123.36(17) . .
C9 N10 C57 121.75(18) . .
C9 N10 C12 112.48(17) . .
C57 N10 C12 124.33(17) . .
C10 N11 C11 111.88(18) . .
C10 N11 C43 122.31(18) . .
C11 N11 C43 123.92(17) . .
C10 N12 C12 111.08(17) . .
C10 N12 C50 118.52(17) . .
C12 N12 C50 122.40(18) . .
C69 N60 C65 111.46(18) . .
C69 N60 C73 105.98(16) . .
C65 N60 C73 110.88(17) . .
C69 N60 C61 111.49(17) . .
C65 N60 C61 106.19(16) . .
C73 N60 C61 110.93(18) . .
O1 C1 N2 125.8(2) . .
O1 C1 N1 125.6(2) . .
N2 C1 N1 108.54(18) . .
O2 C2 N4 125.9(2) . .
O2 C2 N3 125.0(2) . .
N4 C2 N3 109.1(2) . .
N3 C3 N1 114.98(17) . .
N3 C3 C4 103.45(17) . .
N1 C3 C4 102.57(16) . .
N4 C4 N2 115.00(17) . .
N4 C4 C3 103.26(16) . .
N2 C4 C3 103.15(16) . .
O3 C5 N5 125.9(2) . .
O3 C5 N6 126.10(19) . .
N5 C5 N6 108.01(18) . .
O4 C6 N8 125.9(2) . .
O4 C6 N7 125.2(2) . .
N8 C6 N7 108.84(18) . .
N5 C7 N7 114.82(17) . .
N5 C7 C8 103.42(16) . .
N7 C7 C8 103.13(16) . .
N8 C8 N6 113.44(17) . .
N8 C8 C7 103.66(15) . .
N6 C8 C7 102.96(16) . .
O5 C9 N10 126.0(2) . .
O5 C9 N9 125.9(2) . .
N10 C9 N9 108.13(18) . .
O6 C10 N11 125.6(2) . .
O6 C10 N12 125.4(2) . .
N11 C10 N12 109.05(19) . .
N9 C11 N11 114.70(17) . .
N9 C11 C12 104.06(16) . .
N11 C11 C12 103.23(16) . .
N10 C12 N12 114.94(16) . .
N10 C12 C11 102.52(16) . .
N12 C12 C11 104.02(16) . .
N3 C13 C14 115.44(18) . .
C19 C14 C15 118.1(2) . .
C19 C14 C13 118.6(2) . .
C15 C14 C13 123.3(2) . .
C16 C15 C14 120.5(2) . .
C17 C16 C15 120.7(2) . .
C16 C17 C18 119.2(2) . .
C19 C18 C17 120.1(2) . .
C18 C19 C14 121.3(2) . .
N4 C20 C21 114.43(18) . .
C22 C21 C26 118.2(2) . .
C22 C21 C20 121.1(2) . .
C26 C21 C20 120.7(2) . .
C21 C22 C23 121.0(2) . .
C24 C23 C22 120.0(3) . .
C25 C24 C23 119.7(3) . .
C24 C25 C26 120.0(3) . .
C25 C26 C21 121.0(2) . .
N5 C27 N2 114.29(17) . .
N7 C28 C29 113.76(18) . .
C30 C29 C34 118.4(2) . .
C30 C29 C28 121.7(2) . .
C34 C29 C28 119.9(2) . .
C29 C30 C31 120.6(2) . .
C32 C31 C30 120.8(3) . .
C33 C32 C31 119.1(3) . .
C32 C33 C34 120.5(3) . .
C33 C34 C29 120.6(2) . .
N8 C35 C36 114.7(2) . .
C41 C36 C37 118.2(3) . .
C41 C36 C35 123.5(2) . .
C37 C36 C35 118.3(3) . .
C38 C37 C36 120.4(3) . .
C39 C38 C37 121.1(3) . .
C38 C39 C40 119.3(3) . .
C39 C40 C41 119.8(3) . .
C36 C41 C40 121.1(3) . .
N6 C42 N9 113.93(17) . .
N11 C43 C44 113.71(18) . .
C49 C44 C45 118.3(2) . .
C49 C44 C43 120.5(2) . .
C45 C44 C43 121.2(2) . .
C44 C45 C46 120.5(2) . .
C47 C46 C45 120.8(2) . .
C46 C47 C48 119.0(2) . .
C47 C48 C49 120.1(2) . .
C44 C49 C48 121.2(2) . .
N12 C50 C51 115.33(18) . .
C56 C51 C52 118.1(2) . .
C56 C51 C50 122.8(2) . .
C52 C51 C50 119.1(2) . .
C53 C52 C51 120.6(2) . .
C54 C53 C52 120.5(2) . .
C55 C54 C53 119.5(2) . .
C54 C55 C56 120.0(2) . .
C51 C56 C55 121.3(2) . .
N10 C57 N1 114.93(16) . 3_676
C62A C61 N60 115.47(19) . .
C63A C62A C61 122.0(3) . .
C62A C63A C64A 115.1(9) . .
N60 C65 C66 114.91(18) . .
C67 C66 C65 111.0(2) . .
C66 C67 C68 113.3(2) . .
N60 C69 C70 116.35(18) . .
C69 C70 C71 108.75(19) . .
C72 C71 C70 113.7(2) . .
N60 C73 C74 116.99(17) . .
C75 C74 C73 110.63(19) . .
C74 C75 C76 113.1(2) . .
C85 C80 C81 117.9(2) . .
C85 C80 C86 121.4(2) . .
C81 C80 C86 120.7(2) . .
C82 C81 C80 121.9(2) . .
C83 C82 C81 118.9(3) . .
C84 C83 C82 119.9(3) . .
C83 C84 C85 120.7(3) . .
C80 C85 C84 120.8(2) . .
O81 C86 O82 124.2(2) . .
O81 C86 C80 116.4(2) . .
O82 C86 C80 119.3(2) . .
O93 C92 C91 117.7(3) . .
C94 O93 C92 121.4(3) . .
O93 C94 C95 117.0(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(2) .
O2 C2 1.222(2) .
O3 C5 1.227(2) .
O4 C6 1.223(2) .
O5 C9 1.225(2) .
O6 C10 1.224(2) .
O81 C86 1.245(3) .
O82 C86 1.258(3) .
N1 C1 1.362(3) .
N1 C57 1.448(3) 3_676
N1 C3 1.458(2) .
N2 C1 1.360(3) .
N2 C4 1.443(2) .
N2 C27 1.449(2) .
N3 C2 1.372(3) .
N3 C3 1.442(2) .
N3 C13 1.458(3) .
N4 C2 1.366(3) .
N4 C4 1.444(2) .
N4 C20 1.450(3) .
N5 C5 1.366(2) .
N5 C27 1.443(2) .
N5 C7 1.449(2) .
N6 C5 1.368(2) .
N6 C42 1.448(2) .
N6 C8 1.458(2) .
N7 C6 1.367(3) .
N7 C28 1.450(2) .
N7 C7 1.453(2) .
N8 C6 1.359(3) .
N8 C8 1.442(2) .
N8 C35 1.454(3) .
N9 C9 1.368(3) .
N9 C11 1.441(2) .
N9 C42 1.448(2) .
N10 C9 1.368(2) .
N10 C57 1.441(2) .
N10 C12 1.452(2) .
N11 C10 1.368(3) .
N11 C11 1.447(2) .
N11 C43 1.449(3) .
N12 C10 1.375(3) .
N12 C12 1.452(2) .
N12 C50 1.457(2) .
N60 C69 1.506(3) .
N60 C65 1.513(3) .
N60 C73 1.517(3) .
N60 C61 1.527(3) .
C3 C4 1.563(3) .
C7 C8 1.546(3) .
C11 C12 1.548(3) .
C13 C14 1.508(3) .
C14 C19 1.382(3) .
C14 C15 1.392(3) .
C15 C16 1.379(3) .
C16 C17 1.377(3) .
C17 C18 1.381(3) .
C18 C19 1.377(3) .
C20 C21 1.515(3) .
C21 C22 1.380(3) .
C21 C26 1.387(3) .
C22 C23 1.384(3) .
C23 C24 1.381(3) .
C24 C25 1.371(4) .
C25 C26 1.384(3) .
C28 C29 1.512(3) .
C29 C30 1.375(3) .
C29 C34 1.387(3) .
C30 C31 1.382(3) .
C31 C32 1.372(3) .
C32 C33 1.372(4) .
C33 C34 1.381(3) .
C35 C36 1.501(3) .
C36 C41 1.368(3) .
C36 C37 1.385(3) .
C37 C38 1.380(4) .
C38 C39 1.363(4) .
C39 C40 1.368(4) .
C40 C41 1.397(3) .
C43 C44 1.512(3) .
C44 C49 1.378(3) .
C44 C45 1.380(3) .
C45 C46 1.384(3) .
C46 C47 1.373(3) .
C47 C48 1.376(3) .
C48 C49 1.383(3) .
C50 C51 1.507(3) .
C51 C56 1.375(3) .
C51 C52 1.384(3) .
C52 C53 1.378(3) .
C53 C54 1.378(3) .
C54 C55 1.363(3) .
C55 C56 1.386(3) .
C57 N1 1.448(3) 3_676
C61 C62A 1.518(3) .
C62A C63A 1.368(6) .
C63A C64A 1.534(11) .
C63B C64B 1.517(9) .
C65 C66 1.523(3) .
C66 C67 1.512(3) .
C67 C68 1.514(3) .
C69 C70 1.523(3) .
C70 C71 1.533(3) .
C71 C72 1.534(3) .
C73 C74 1.525(3) .
C74 C75 1.513(3) .
C75 C76 1.516(3) .
C80 C85 1.372(3) .
C80 C81 1.387(3) .
C80 C86 1.504(3) .
C81 C82 1.377(3) .
C82 C83 1.377(4) .
C83 C84 1.369(3) .
C84 C85 1.375(3) .
C91 C92 1.392(4) .
C92 O93 1.372(3) .
O93 C94 1.346(3) .
C94 C95 1.424(4) .
