#------------------------------------------------------------------------------
#$Date: 2019-11-12 04:18:55 +0200 (Tue, 12 Nov 2019) $
#$Revision: 227527 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/03/34/4033488.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_4033488
loop_
_publ_author_name
'Fiala, Tomas'
'Sleziakova, Kristina'
'Marsalek, Kamil'
'Salvadori, Karolina'
'Sindelar, Vladimir'
_publ_section_title
;
 Thermodynamics of Halide Binding to a Neutral Bambusuril in Water and
 Organic Solvents.
;
_journal_issue                   4
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              1903
_journal_page_last               1912
_journal_paper_doi               10.1021/acs.joc.7b02846
_journal_volume                  83
_journal_year                    2018
_chemical_formula_moiety         'C114 H108 N24 O12, C2 H2 Cl6, 8 (C H Cl3)'
_chemical_formula_sum            'C124 H118 Cl30 N24 O12'
_chemical_formula_weight         3199.92
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_update_record
;
2010-09-08 # Formatted by publCIF
;
_cell_angle_alpha                98.852(6)
_cell_angle_beta                 110.605(8)
_cell_angle_gamma                104.194(6)
_cell_formula_units_Z            1
_cell_length_a                   14.0083(12)
_cell_length_b                   15.8585(10)
_cell_length_c                   18.1756(15)
_cell_measurement_reflns_used    3878
_cell_measurement_temperature    119.9
_cell_measurement_theta_max      68.8452
_cell_measurement_theta_min      2.9781
_cell_volume                     3533.4(6)
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction Ltd.,2010)'
_computing_data_collection       'CrysAlisPro (Oxford Diffraction Ltd.,2010)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction Ltd.,2010)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      119.9
_diffrn_detector_area_resol_mean 10.3784
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method
;
  Rotation method data acquisition using ω scans 
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.1689
_diffrn_reflns_av_sigmaI/netI    0.2501
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24449
_diffrn_reflns_theta_full        54.24
_diffrn_reflns_theta_max         54.24
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    5.836
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53907
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Oxford Diffraction Ltd.,Version 1.171.34.36'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1636
_exptl_crystal_size_max          0.2486
_exptl_crystal_size_mid          0.1445
_exptl_crystal_size_min          0.0935
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         8589
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.2880
_refine_ls_R_factor_gt           0.1364
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3320
_refine_ls_wR_factor_ref         0.4382
_reflns_number_gt                2942
_reflns_number_total             8589
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo7b02846_si_002.cif
_cod_data_source_block           sind_bnbu6_1_6
_cod_depositor_comments          'Adding full bibliography for 4033488.cif.'
_cod_original_cell_volume        3533.4(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4033488
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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3168(13) 0.4449(10) 0.1725(9) 0.057(5) Uani 1 1 d . . .
H1A H 0.3293 0.3876 0.1746 0.068 Uiso 1 1 calc R . .
H1B H 0.3809 0.4920 0.2128 0.068 Uiso 1 1 calc R . .
C2 C 0.2583(11) 0.3870(9) 0.0174(8) 0.039(4) Uani 1 1 d . . .
H2 H 0.1839 0.3506 0.0040 0.046 Uiso 1 1 calc R . .
C3 C 0.2652(11) 0.4431(8) -0.0470(9) 0.038(4) Uani 1 1 d . . .
H3 H 0.1937 0.4360 -0.0876 0.046 Uiso 1 1 calc R . .
C4 C 0.3409(12) 0.5427(9) 0.0838(11) 0.046(4) Uani 1 1 d . . .
C5 C 0.3556(12) 0.3393(10) -0.0514(9) 0.042(4) Uani 1 1 d . . .
C6 C 0.3292(12) 0.2537(8) 0.0480(8) 0.046(4) Uani 1 1 d . . .
H6A H 0.2805 0.2465 0.0752 0.056 Uiso 1 1 calc R . .
H6B H 0.3045 0.1993 0.0046 0.056 Uiso 1 1 calc R . .
C7 C 0.4377(6) 0.2642(7) 0.1066(6) 0.058(2) Uani 1 1 d G . .
C8 C 0.5101(8) 0.3479(5) 0.1584(6) 0.058(2) Uani 1 1 d G . .
H8 H 0.4926 0.4006 0.1562 0.069 Uiso 1 1 calc R . .
C9 C 0.6124(7) 0.3489(5) 0.2148(5) 0.058(2) Uani 1 1 d G . .
H9 H 0.6610 0.4032 0.2515 0.069 Uiso 1 1 calc R . .
C10 C 0.6419(6) 0.2693(6) 0.2163(5) 0.058(2) Uani 1 1 d G . .
H10 H 0.7087 0.2718 0.2537 0.069 Uiso 1 1 calc R . .
C11 C 0.5695(8) 0.1868(5) 0.1607(6) 0.058(2) Uani 1 1 d G . .
H11 H 0.5901 0.1354 0.1594 0.069 Uiso 1 1 calc R . .
C12 C 0.4609(7) 0.1815(5) 0.1047(6) 0.058(2) Uani 1 1 d G . .
H12 H 0.4103 0.1270 0.0699 0.069 Uiso 1 1 calc R . .
C13 C 0.3289(12) 0.4103(10) -0.1631(9) 0.054(4) Uani 1 1 d . . .
H13A H 0.3955 0.4029 -0.1633 0.064 Uiso 1 1 calc R . .
H13B H 0.3294 0.4700 -0.1696 0.064 Uiso 1 1 calc R . .
C14 C 0.2369(7) 0.3421(6) -0.2343(6) 0.069(2) Uani 1 1 d G . .
C15 C 0.1491(9) 0.3657(5) -0.2790(6) 0.069(2) Uani 1 1 d G . .
H15 H 0.1476 0.4240 -0.2641 0.083 Uiso 1 1 calc R . .
C16 C 0.0635(7) 0.3023(7) -0.3458(6) 0.069(2) Uani 1 1 d G . .
H16 H 0.0047 0.3182 -0.3756 0.083 Uiso 1 1 calc R . .
C17 C 0.0657(7) 0.2152(6) -0.3679(5) 0.069(2) Uani 1 1 d G . .
H17 H 0.0084 0.1727 -0.4126 0.083 Uiso 1 1 calc R . .
C18 C 0.1536(9) 0.1915(5) -0.3233(6) 0.069(2) Uani 1 1 d G . .
H18 H 0.1551 0.1332 -0.3382 0.083 Uiso 1 1 calc R . .
C19 C 0.2392(7) 0.2549(7) -0.2565(6) 0.069(2) Uani 1 1 d G . .
H19 H 0.2980 0.2391 -0.2267 0.083 Uiso 1 1 calc R . .
C20 C 0.3486(12) 0.6157(9) -0.0246(9) 0.048(4) Uani 1 1 d . . .
H20A H 0.4141 0.6590 0.0181 0.058 Uiso 1 1 calc R . .
H20B H 0.3639 0.5993 -0.0719 0.058 Uiso 1 1 calc R . .
C21 C -0.2690(11) 0.2585(9) 0.0004(9) 0.046(4) Uani 1 1 d . . .
H21 H -0.2792 0.2591 -0.0557 0.055 Uiso 1 1 calc R . .
C22 C -0.1573(11) 0.2532(9) 0.0500(9) 0.046(4) Uani 1 1 d . . .
H22 H -0.1095 0.2649 0.0216 0.056 Uiso 1 1 calc R . .
C23 C -0.1818(13) 0.3758(10) 0.1214(10) 0.048(4) Uani 1 1 d . . .
C24 C -0.2903(14) 0.1177(11) 0.0280(9) 0.049(5) Uani 1 1 d . . .
C25 C -0.4586(10) 0.1394(9) -0.0568(8) 0.042(4) Uani 1 1 d . . .
H25A H -0.4944 0.1836 -0.0508 0.050 Uiso 1 1 calc R . .
H25B H -0.4942 0.0858 -0.0449 0.050 Uiso 1 1 calc R . .
C26 C -0.4678(8) 0.1156(7) -0.1443(5) 0.060(2) Uani 1 1 d G . .
C27 C -0.4470(8) 0.0383(6) -0.1722(6) 0.060(2) Uani 1 1 d G . .
H27 H -0.4285 0.0016 -0.1380 0.072 Uiso 1 1 calc R . .
C28 C -0.4537(7) 0.0159(5) -0.2513(6) 0.060(2) Uani 1 1 d G . .
H28 H -0.4398 -0.0358 -0.2700 0.072 Uiso 1 1 calc R . .
C29 C -0.4813(8) 0.0708(6) -0.3024(5) 0.060(2) Uani 1 1 d G . .
H29 H -0.4859 0.0558 -0.3554 0.072 Uiso 1 1 calc R . .
C30 C -0.5021(8) 0.1481(6) -0.2745(6) 0.060(2) Uani 1 1 d G . .
H30 H -0.5206 0.1848 -0.3087 0.072 Uiso 1 1 calc R . .
C31 C -0.4954(7) 0.1705(5) -0.1954(6) 0.060(2) Uani 1 1 d G . .
H31 H -0.5093 0.2222 -0.1767 0.072 Uiso 1 1 calc R . .
C32 C -0.1065(11) 0.1087(9) 0.0613(9) 0.053(5) Uani 1 1 d . . .
H32A H -0.1366 0.0510 0.0700 0.064 Uiso 1 1 calc R . .
H32B H -0.0386 0.1404 0.1079 0.064 Uiso 1 1 calc R . .
C33 C -0.0842(9) 0.0917(7) -0.0139(5) 0.079(3) Uani 1 1 d G . .
C34 C 0.0204(8) 0.1196(7) -0.0092(5) 0.079(3) Uani 1 1 d G . .
H34 H 0.0777 0.1501 0.0408 0.095 Uiso 1 1 calc R . .
C35 C 0.0392(7) 0.1020(7) -0.0793(7) 0.079(3) Uani 1 1 d G . .
H35 H 0.1092 0.1207 -0.0762 0.095 Uiso 1 1 calc R . .
C36 C -0.0465(9) 0.0564(7) -0.1540(5) 0.079(3) Uani 1 1 d G . .
H36 H -0.0339 0.0447 -0.2008 0.095 Uiso 1 1 calc R . .
C37 C -0.1511(7) 0.0285(7) -0.1586(5) 0.079(3) Uani 1 1 d G . .
H37 H -0.2084 -0.0020 -0.2086 0.095 Uiso 1 1 calc R . .
C38 C -0.1699(7) 0.0461(7) -0.0886(7) 0.079(3) Uani 1 1 d G . .
H38 H -0.2399 0.0275 -0.0917 0.095 Uiso 1 1 calc R . .
C39 C -0.0211(12) 0.3333(9) 0.1998(9) 0.052(5) Uani 1 1 d . . .
H39A H -0.0352 0.3513 0.2474 0.062 Uiso 1 1 calc R . .
H39B H -0.0068 0.2765 0.2002 0.062 Uiso 1 1 calc R . .
C40 C 0.1097(12) 0.4952(8) 0.2412(9) 0.045(4) Uani 1 1 d . . .
H40 H 0.0586 0.5252 0.2152 0.054 Uiso 1 1 calc R . .
C41 C 0.2197(12) 0.5294(9) 0.2328(9) 0.047(4) Uani 1 1 d . . .
H41 H 0.2176 0.5717 0.1987 0.057 Uiso 1 1 calc R . .
C42 C 0.1389(14) 0.3737(11) 0.1747(10) 0.054(5) Uani 1 1 d . . .
C43 C 0.2536(12) 0.5697(9) 0.3727(13) 0.048(5) Uani 1 1 d . . .
C44 C 0.0680(13) 0.5239(10) 0.3673(9) 0.058(5) Uani 1 1 d . . .
H44A H 0.0077 0.5354 0.3285 0.070 Uiso 1 1 calc R . .
H44B H 0.1031 0.5755 0.4147 0.070 Uiso 1 1 calc R . .
C45 C 0.0248(9) 0.4429(6) 0.3932(6) 0.066(2) Uani 1 1 d G . .
C46 C -0.0765(8) 0.4278(6) 0.3946(6) 0.066(2) Uani 1 1 d G . .
H46 H -0.1150 0.4669 0.3792 0.079 Uiso 1 1 calc R . .
C47 C -0.1203(6) 0.3543(7) 0.4191(6) 0.066(2) Uani 1 1 d G . .
H47 H -0.1880 0.3443 0.4200 0.079 Uiso 1 1 calc R . .
C48 C -0.0627(8) 0.2959(6) 0.4422(6) 0.066(2) Uani 1 1 d G . .
H48 H -0.0920 0.2468 0.4586 0.079 Uiso 1 1 calc R . .
C49 C 0.0386(8) 0.3110(7) 0.4409(6) 0.066(2) Uani 1 1 d G . .
H49 H 0.0771 0.2719 0.4563 0.079 Uiso 1 1 calc R . .
C50 C 0.0823(6) 0.3844(7) 0.4164(6) 0.066(2) Uani 1 1 d G . .
H50 H 0.1501 0.3945 0.4154 0.079 Uiso 1 1 calc R . .
C51 C 0.4026(11) 0.6303(9) 0.3350(9) 0.050(4) Uani 1 1 d . . .
H51A H 0.4184 0.6837 0.3771 0.060 Uiso 1 1 calc R . .
H51B H 0.4025 0.6496 0.2869 0.060 Uiso 1 1 calc R . .
C52 C 0.4922(7) 0.5915(7) 0.3631(6) 0.064(2) Uani 1 1 d G . .
C53 C 0.4804(7) 0.5157(7) 0.3929(6) 0.064(2) Uani 1 1 d G . .
H53 H 0.4160 0.4882 0.3964 0.077 Uiso 1 1 calc R . .
C54 C 0.5650(9) 0.4808(6) 0.4174(6) 0.064(2) Uani 1 1 d G . .
H54 H 0.5571 0.4301 0.4374 0.077 Uiso 1 1 calc R . .
C55 C 0.6613(7) 0.5218(7) 0.4121(6) 0.064(2) Uani 1 1 d G . .
H55 H 0.7179 0.4985 0.4286 0.077 Uiso 1 1 calc R . .
C56 C 0.6731(7) 0.5976(7) 0.3823(6) 0.064(2) Uani 1 1 d G . .
H56 H 0.7375 0.6251 0.3788 0.077 Uiso 1 1 calc R . .
C57 C 0.5885(9) 0.6325(6) 0.3578(6) 0.064(2) Uani 1 1 d G . .
H57 H 0.5963 0.6832 0.3379 0.077 Uiso 1 1 calc R . .
N1 N 0.3011(9) 0.4581(8) 0.0912(7) 0.046(3) Uani 1 1 d . . .
N2 N 0.3192(9) 0.5338(7) 0.0035(7) 0.042(3) Uani 1 1 d . . .
N3 N 0.3248(9) 0.3315(8) 0.0120(8) 0.047(3) Uani 1 1 d . . .
N4 N 0.3271(10) 0.4056(8) -0.0829(7) 0.045(3) Uani 1 1 d . . .
N5 N 0.2672(10) 0.6578(8) -0.0453(8) 0.051(4) Uani 1 1 d . . .
N6 N -0.1178(10) 0.3205(7) 0.1250(7) 0.050(4) Uani 1 1 d . . .
N7 N -0.3404(9) 0.1775(8) 0.0034(7) 0.045(3) Uani 1 1 d . . .
N8 N -0.1798(10) 0.1606(8) 0.0587(7) 0.047(3) Uani 1 1 d . . .
N9 N 0.0718(10) 0.4004(8) 0.2041(8) 0.049(4) Uani 1 1 d . . .
N10 N 0.2272(10) 0.4457(8) 0.1940(7) 0.049(3) Uani 1 1 d . . .
N11 N 0.1451(11) 0.5172(8) 0.3302(8) 0.049(3) Uani 1 1 d . . .
N12 N 0.2976(10) 0.5728(7) 0.3163(8) 0.044(3) Uani 1 1 d . . .
O1 O 0.3807(8) 0.6116(6) 0.1388(6) 0.049(3) Uani 1 1 d . . .
O2 O 0.4016(8) 0.2899(6) -0.0727(6) 0.050(3) Uani 1 1 d . . .
O3 O -0.1632(7) 0.4434(6) 0.1741(6) 0.047(3) Uani 1 1 d . . .
O4 O -0.3334(8) 0.0412(7) 0.0256(6) 0.055(3) Uani 1 1 d . . .
O5 O 0.1284(8) 0.2962(7) 0.1377(6) 0.059(3) Uani 1 1 d . . .
O6 O 0.2994(8) 0.6050(7) 0.4445(6) 0.056(3) Uani 1 1 d . . .
C58 C 0.0802(13) 0.7190(11) 0.1323(11) 0.071(5) Uani 1 1 d . . .
H58 H 0.0607 0.7628 0.1022 0.086 Uiso 1 1 calc R . .
Cl1 Cl 0.0410(4) 0.6162(3) 0.0628(3) 0.0759(15) Uani 1 1 d . . .
Cl2 Cl 0.0148(4) 0.7114(3) 0.1985(3) 0.0955(18) Uani 1 1 d . . .
Cl3 Cl 0.2224(4) 0.7588(3) 0.1902(3) 0.0809(15) Uani 1 1 d . . .
C61 C 0.7859(18) 0.0410(16) 0.2132(17) 0.059(7) Uani 0.60 1 d PD A 1
H61 H 0.7522 0.0670 0.1693 0.071 Uiso 0.60 1 calc PR A 1
Cl10 Cl 0.752(2) -0.0752(15) 0.171(2) 0.099(7) Uani 0.60 1 d PD A 1
Cl11 Cl 0.7268(15) 0.0524(13) 0.2833(10) 0.113(6) Uani 0.60 1 d PD A 1
Cl12 Cl 0.9210(8) 0.0996(7) 0.2578(6) 0.112(3) Uani 0.60 1 d PD A 1
C361 C 0.763(4) 0.0333(18) 0.222(2) 0.059(7) Uani 0.40 1 d PD B 2
H361 H 0.6929 0.0309 0.1829 0.071 Uiso 0.40 1 calc PR B 2
Cl32 Cl 0.8471(13) 0.1422(10) 0.2499(9) 0.112(3) Uani 0.40 1 d PD B 2
Cl31 Cl 0.748(3) 0.020(2) 0.3113(17) 0.113(6) Uani 0.40 1 d PD B 2
Cl30 Cl 0.794(4) -0.057(2) 0.182(4) 0.099(7) Uani 0.40 1 d PD B 2
C59 C 0.288(2) 0.2530(18) 0.3189(17) 0.163(11) Uani 1 1 d U . .
H59 H 0.2769 0.3063 0.3009 0.196 Uiso 1 1 calc R . .
Cl4 Cl 0.3517(5) 0.3003(4) 0.4292(3) 0.128(2) Uani 1 1 d . . .
Cl5 Cl 0.1670(7) 0.1899(5) 0.2872(4) 0.174(3) Uani 1 1 d . . .
Cl6 Cl 0.3824(7) 0.2369(4) 0.2843(5) 0.170(3) Uani 1 1 d . . .
C60 C 0.650(2) 0.193(3) 0.5104(14) 0.064(8) Uani 0.50 1 d PDU C 1
H60 H 0.6519 0.2541 0.5073 0.076 Uiso 0.50 1 calc PR C 1
Cl7 Cl 0.520(3) 0.135(3) 0.496(3) 0.110(6) Uani 0.50 1 d PD C 1
Cl8 Cl 0.747(3) 0.203(3) 0.6060(16) 0.150(5) Uani 0.50 1 d PD C 1
Cl9 Cl 0.6844(14) 0.1499(11) 0.4350(11) 0.122(6) Uani 0.50 1 d PDU C 1
C260 C 0.615(2) 0.196(2) 0.4877(14) 0.064(8) Uani 0.50 1 d PDU D 2
H260 H 0.5978 0.2524 0.4921 0.076 Uiso 0.50 1 calc PR D 2
Cl29 Cl 0.6408(14) 0.1770(11) 0.4019(11) 0.122(6) Uani 0.50 1 d PDU D 2
Cl28 Cl 0.727(3) 0.210(3) 0.5768(16) 0.150(5) Uani 0.50 1 d PD D 2
Cl27 Cl 0.502(3) 0.111(3) 0.477(3) 0.110(6) Uani 0.50 1 d PD D 2
C62 C 0.802(2) 0.926(2) 0.5524(13) 0.145(15) Uani 0.60 1 d PDU E 1
H62 H 0.7670 0.8662 0.5560 0.174 Uiso 0.60 1 calc PR E 1
Cl13 Cl 0.803(4) 1.009(2) 0.6298(10) 0.175(6) Uani 0.60 1 d PD E 1
Cl14 Cl 0.7282(12) 0.9407(12) 0.4572(7) 0.197(6) Uani 0.60 1 d PD E 1
Cl15 Cl 0.936(2) 0.939(3) 0.570(4) 0.243(17) Uani 0.60 1 d PD E 1
C362 C 0.813(4) 0.963(2) 0.517(3) 0.145(15) Uani 0.40 1 d PDU F 2
H362 H 0.7978 0.9965 0.4757 0.174 Uiso 0.40 1 calc PR F 2
Cl34 Cl 0.7420(17) 0.8452(17) 0.4767(11) 0.197(6) Uani 0.40 1 d PD F 2
Cl33 Cl 0.784(6) 1.003(4) 0.5985(19) 0.175(6) Uani 0.40 1 d PD F 2
Cl35 Cl 0.948(3) 0.965(5) 0.556(6) 0.243(17) Uani 0.40 1 d PD F 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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
N10 C1 N1 114.0(12) . .
N10 C1 H1A 108.8 . .
N1 C1 H1A 108.8 . .
N10 C1 H1B 108.8 . .
N1 C1 H1B 108.8 . .
H1A C1 H1B 107.6 . .
N1 C2 N3 116.1(11) . .
N1 C2 C3 101.2(11) . .
N3 C2 C3 103.0(11) . .
N1 C2 H2 111.9 . .
N3 C2 H2 111.9 . .
C3 C2 H2 111.9 . .
N2 C3 N4 115.1(11) . .
N2 C3 C2 102.5(11) . .
N4 C3 C2 102.8(10) . .
N2 C3 H3 111.9 . .
N4 C3 H3 111.9 . .
C2 C3 H3 111.9 . .
O1 C4 N2 128.1(14) . .
O1 C4 N1 125.2(16) . .
N2 C4 N1 106.5(13) . .
O2 C5 N4 128.5(15) . .
O2 C5 N3 121.4(15) . .
N4 C5 N3 110.2(14) . .
C7 C6 N3 113.1(11) . .
C7 C6 H6A 109.0 . .
N3 C6 H6A 109.0 . .
C7 C6 H6B 109.0 . .
N3 C6 H6B 109.0 . .
H6A C6 H6B 107.8 . .
C8 C7 C12 124.3 . .
C8 C7 C6 122.5(8) . .
C12 C7 C6 113.3(8) . .
C7 C8 C9 117.1 . .
C7 C8 H8 121.4 . .
C9 C8 H8 121.4 . .
C10 C9 C8 121.9 . .
C10 C9 H9 119.0 . .
C8 C9 H9 119.0 . .
C11 C10 C9 119.6 . .
C11 C10 H10 120.2 . .
C9 C10 H10 120.2 . .
C10 C11 C12 120.4 . .
C10 C11 H11 119.8 . .
C12 C11 H11 119.8 . .
C7 C12 C11 116.5 . .
C7 C12 H12 121.8 . .
C11 C12 H12 121.8 . .
N4 C13 C14 114.9(12) . .
N4 C13 H13A 108.6 . .
C14 C13 H13A 108.6 . .
N4 C13 H13B 108.6 . .
C14 C13 H13B 108.6 . .
H13A C13 H13B 107.5 . .
C15 C14 C19 120.0 . .
C15 C14 C13 119.9(9) . .
C19 C14 C13 120.1(9) . .
C16 C15 C14 120.0 . .
C16 C15 H15 120.0 . .
C14 C15 H15 120.0 . .
C17 C16 C15 120.0 . .
C17 C16 H16 120.0 . .
C15 C16 H16 120.0 . .
C16 C17 C18 120.0 . .
C16 C17 H17 120.0 . .
C18 C17 H17 120.0 . .
C19 C18 C17 120.0 . .
C19 C18 H18 120.0 . .
C17 C18 H18 120.0 . .
C18 C19 C14 120.0 . .
C18 C19 H19 120.0 . .
C14 C19 H19 120.0 . .
N5 C20 N2 114.0(12) . .
N5 C20 H20A 108.7 . .
N2 C20 H20A 108.7 . .
N5 C20 H20B 108.7 . .
N2 C20 H20B 108.7 . .
H20A C20 H20B 107.6 . .
N5 C21 N7 116.1(12) 2_565 .
N5 C21 C22 102.4(11) 2_565 .
N7 C21 C22 102.2(12) . .
N5 C21 H21 111.8 2_565 .
N7 C21 H21 111.8 . .
C22 C21 H21 111.8 . .
N6 C22 N8 113.7(13) . .
N6 C22 C21 104.6(11) . .
N8 C22 C21 104.1(11) . .
N6 C22 H22 111.4 . .
N8 C22 H22 111.4 . .
C21 C22 H22 111.4 . .
O3 C23 N5 127.0(14) . 2_565
O3 C23 N6 126.3(14) . .
N5 C23 N6 106.6(12) 2_565 .
O4 C24 N7 126.2(16) . .
O4 C24 N8 125.5(16) . .
N7 C24 N8 108.3(14) . .
N7 C25 C26 110.5(10) . .
N7 C25 H25A 109.5 . .
C26 C25 H25A 109.5 . .
N7 C25 H25B 109.5 . .
C26 C25 H25B 109.5 . .
H25A C25 H25B 108.1 . .
C27 C26 C31 120.0 . .
C27 C26 C25 119.0(9) . .
C31 C26 C25 121.0(9) . .
C28 C27 C26 120.0 . .
C28 C27 H27 120.0 . .
C26 C27 H27 120.0 . .
C27 C28 C29 120.0 . .
C27 C28 H28 120.0 . .
C29 C28 H28 120.0 . .
C30 C29 C28 120.0 . .
C30 C29 H29 120.0 . .
C28 C29 H29 120.0 . .
C29 C30 C31 120.0 . .
C29 C30 H30 120.0 . .
C31 C30 H30 120.0 . .
C30 C31 C26 120.0 . .
C30 C31 H31 120.0 . .
C26 C31 H31 120.0 . .
N8 C32 C33 114.9(12) . .
N8 C32 H32A 108.5 . .
C33 C32 H32A 108.5 . .
N8 C32 H32B 108.5 . .
C33 C32 H32B 108.5 . .
H32A C32 H32B 107.5 . .
C34 C33 C38 120.0 . .
C34 C33 C32 121.0(9) . .
C38 C33 C32 119.0(9) . .
C33 C34 C35 120.0 . .
C33 C34 H34 120.0 . .
C35 C34 H34 120.0 . .
C34 C35 C36 120.0 . .
C34 C35 H35 120.0 . .
C36 C35 H35 120.0 . .
C37 C36 C35 120.0 . .
C37 C36 H36 120.0 . .
C35 C36 H36 120.0 . .
C36 C37 C38 120.0 . .
C36 C37 H37 120.0 . .
C38 C37 H37 120.0 . .
C37 C38 C33 120.0 . .
C37 C38 H38 120.0 . .
C33 C38 H38 120.0 . .
N9 C39 N6 111.5(13) . .
N9 C39 H39A 109.3 . .
N6 C39 H39A 109.3 . .
N9 C39 H39B 109.3 . .
N6 C39 H39B 109.3 . .
H39A C39 H39B 108.0 . .
N9 C40 N11 112.9(13) . .
N9 C40 C41 103.8(11) . .
N11 C40 C41 101.7(11) . .
N9 C40 H40 112.5 . .
N11 C40 H40 112.5 . .
C41 C40 H40 112.5 . .
N10 C41 N12 116.3(12) . .
N10 C41 C40 101.5(11) . .
N12 C41 C40 103.8(12) . .
N10 C41 H41 111.5 . .
N12 C41 H41 111.5 . .
C40 C41 H41 111.5 . .
O5 C42 N9 128.6(15) . .
O5 C42 N10 122.5(17) . .
N9 C42 N10 108.9(14) . .
O6 C43 N12 126.7(14) . .
O6 C43 N11 126.7(16) . .
N12 C43 N11 106.6(16) . .
N11 C44 C45 115.8(11) . .
N11 C44 H44A 108.3 . .
C45 C44 H44A 108.3 . .
N11 C44 H44B 108.3 . .
C45 C44 H44B 108.3 . .
H44A C44 H44B 107.4 . .
C46 C45 C50 120.0 . .
C46 C45 C44 117.4(10) . .
C50 C45 C44 122.6(10) . .
C45 C46 C47 120.0 . .
C45 C46 H46 120.0 . .
C47 C46 H46 120.0 . .
C48 C47 C46 120.0 . .
C48 C47 H47 120.0 . .
C46 C47 H47 120.0 . .
C49 C48 C47 120.0 . .
C49 C48 H48 120.0 . .
C47 C48 H48 120.0 . .
C48 C49 C50 120.0 . .
C48 C49 H49 120.0 . .
C50 C49 H49 120.0 . .
C49 C50 C45 120.0 . .
C49 C50 H50 120.0 . .
C45 C50 H50 120.0 . .
N12 C51 C52 116.6(12) . .
N12 C51 H51A 108.2 . .
C52 C51 H51A 108.2 . .
N12 C51 H51B 108.2 . .
C52 C51 H51B 108.2 . .
H51A C51 H51B 107.3 . .
C53 C52 C57 120.0 . .
C53 C52 C51 121.6(10) . .
C57 C52 C51 118.3(9) . .
C52 C53 C54 120.0 . .
C52 C53 H53 120.0 . .
C54 C53 H53 120.0 . .
C53 C54 C55 120.0 . .
C53 C54 H54 120.0 . .
C55 C54 H54 120.0 . .
C56 C55 C54 120.0 . .
C56 C55 H55 120.0 . .
C54 C55 H55 120.0 . .
C55 C56 C57 120.0 . .
C55 C56 H56 120.0 . .
C57 C56 H56 120.0 . .
C56 C57 C52 120.0 . .
C56 C57 H57 120.0 . .
C52 C57 H57 120.0 . .
C4 N1 C2 114.9(13) . .
C4 N1 C1 119.5(13) . .
C2 N1 C1 125.1(13) . .
C4 N2 C3 114.6(12) . .
C4 N2 C20 119.3(11) . .
C3 N2 C20 126.2(12) . .
C5 N3 C2 110.9(13) . .
C5 N3 C6 121.1(12) . .
C2 N3 C6 124.9(13) . .
C5 N4 C3 112.5(13) . .
C5 N4 C13 118.3(12) . .
C3 N4 C13 125.7(13) . .
C23 N5 C20 119.4(12) 2_565 .
C23 N5 C21 112.7(12) 2_565 2_565
C20 N5 C21 127.2(12) . 2_565
C23 N6 C22 111.7(12) . .
C23 N6 C39 121.9(11) . .
C22 N6 C39 126.4(12) . .
C24 N7 C21 113.2(13) . .
C24 N7 C25 117.3(12) . .
C21 N7 C25 121.1(12) . .
C24 N8 C32 120.8(12) . .
C24 N8 C22 110.1(12) . .
C32 N8 C22 123.3(12) . .
C42 N9 C40 112.6(12) . .
C42 N9 C39 118.8(12) . .
C40 N9 C39 128.4(13) . .
C42 N10 C1 125.6(13) . .
C42 N10 C41 113.1(13) . .
C1 N10 C41 121.1(13) . .
C43 N11 C40 113.2(14) . .
C43 N11 C44 119.6(13) . .
C40 N11 C44 120.7(12) . .
C43 N12 C51 122.5(13) . .
C43 N12 C41 113.9(13) . .
C51 N12 C41 122.1(13) . .
Cl1 C58 Cl2 111.3(9) . .
Cl1 C58 Cl3 110.8(9) . .
Cl2 C58 Cl3 109.4(10) . .
Cl1 C58 H58 108.4 . .
Cl2 C58 H58 108.4 . .
Cl3 C58 H58 108.4 . .
Cl12 C61 Cl11 111.0(15) . .
Cl12 C61 Cl10 115.2(16) . .
Cl11 C61 Cl10 107.0(15) . .
Cl12 C61 H61 107.8 . .
Cl11 C61 H61 107.8 . .
Cl10 C61 H61 107.8 . .
Cl32 C361 Cl30 122(3) . .
Cl32 C361 Cl31 103.3(19) . .
Cl30 C361 Cl31 110(3) . .
Cl32 C361 H361 107.1 . .
Cl30 C361 H361 107.1 . .
Cl31 C361 H361 107.1 . .
Cl5 C59 Cl6 127.1(18) . .
Cl5 C59 Cl4 113.2(13) . .
Cl6 C59 Cl4 109.5(15) . .
Cl5 C59 H59 100.6 . .
Cl6 C59 H59 100.6 . .
Cl4 C59 H59 100.6 . .
Cl9 C60 Cl8 111(2) . .
Cl9 C60 Cl7 113(2) . .
Cl8 C60 Cl7 113(2) . .
Cl9 C60 H60 106.2 . .
Cl8 C60 H60 106.2 . .
Cl7 C60 H60 106.2 . .
Cl29 C260 Cl27 110(2) . .
Cl29 C260 Cl28 112.2(19) . .
Cl27 C260 Cl28 112(2) . .
Cl29 C260 H260 107.2 . .
Cl27 C260 H260 107.2 . .
Cl28 C260 H260 107.2 . .
Cl15 C62 Cl13 107(2) . .
Cl15 C62 Cl14 112(3) . .
Cl13 C62 Cl14 109.2(16) . .
Cl15 C62 H62 109.4 . .
Cl13 C62 H62 109.4 . .
Cl14 C62 H62 109.4 . .
Cl33 C362 Cl35 109(3) . .
Cl33 C362 Cl34 109(2) . .
Cl35 C362 Cl34 102(3) . .
Cl33 C362 H362 112.4 . .
Cl35 C362 H362 112.4 . .
Cl34 C362 H362 112.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N10 1.442(18) .
C1 N1 1.472(18) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 N1 1.438(16) .
C2 N3 1.447(15) .
C2 C3 1.589(18) .
C2 H2 0.9800 .
C3 N2 1.433(15) .
C3 N4 1.436(16) .
C3 H3 0.9800 .
C4 O1 1.215(15) .
C4 N2 1.359(19) .
C4 N1 1.366(17) .
C5 O2 1.229(16) .
C5 N4 1.350(17) .
C5 N3 1.376(18) .
C6 C7 1.468(15) .
C6 N3 1.488(16) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C7 C8 1.3994 .
C7 C12 1.4252 .
C8 C9 1.4341 .
C8 H8 0.9300 .
C9 C10 1.4219 .
C9 H9 0.9300 .
C10 C11 1.4077 .
C10 H10 0.9300 .
C11 C12 1.4755 .
C11 H11 0.9300 .
C12 H12 0.9300 .
C13 N4 1.479(17) .
C13 C14 1.490(15) .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
C14 C15 1.3900 .
C14 C19 1.3900 .
C15 C16 1.3900 .
C15 H15 0.9300 .
C16 C17 1.3900 .
C16 H16 0.9300 .
C17 C18 1.3900 .
C17 H17 0.9300 .
C18 C19 1.3900 .
C18 H18 0.9300 .
C19 H19 0.9300 .
C20 N5 1.427(16) .
C20 N2 1.486(16) .
C20 H20A 0.9700 .
C20 H20B 0.9700 .
C21 N5 1.437(15) 2_565
C21 N7 1.444(16) .
C21 C22 1.537(17) .
C21 H21 0.9800 .
C22 N6 1.426(16) .
C22 N8 1.470(16) .
C22 H22 0.9800 .
C23 O3 1.226(15) .
C23 N5 1.387(18) 2_565
C23 N6 1.394(17) .
C24 O4 1.202(16) .
C24 N7 1.352(17) .
C24 N8 1.389(18) .
C25 N7 1.528(16) .
C25 C26 1.528(15) .
C25 H25A 0.9700 .
C25 H25B 0.9700 .
C26 C27 1.3900 .
C26 C31 1.3900 .
C27 C28 1.3900 .
C27 H27 0.9300 .
C28 C29 1.3900 .
C28 H28 0.9300 .
C29 C30 1.3900 .
C29 H29 0.9300 .
C30 C31 1.3900 .
C30 H30 0.9300 .
C31 H31 0.9300 .
C32 N8 1.459(16) .
C32 C33 1.506(17) .
C32 H32A 0.9700 .
C32 H32B 0.9700 .
C33 C34 1.3900 .
C33 C38 1.3900 .
C34 C35 1.3900 .
C34 H34 0.9300 .
C35 C36 1.3900 .
C35 H35 0.9300 .
C36 C37 1.3900 .
C36 H36 0.9300 .
C37 C38 1.3900 .
C37 H37 0.9300 .
C38 H38 0.9300 .
C39 N9 1.435(17) .
C39 N6 1.486(16) .
C39 H39A 0.9700 .
C39 H39B 0.9700 .
C40 N9 1.429(16) .
C40 N11 1.471(18) .
C40 C41 1.572(19) .
C40 H40 0.9800 .
C41 N10 1.450(16) .
C41 N12 1.453(17) .
C41 H41 0.9800 .
C42 O5 1.253(17) .
C42 N9 1.351(19) .
C42 N10 1.355(17) .
C43 O6 1.200(19) .
C43 N12 1.369(19) .
C43 N11 1.398(17) .
C44 N11 1.477(17) .
C44 C45 1.498(16) .
C44 H44A 0.9700 .
C44 H44B 0.9700 .
C45 C46 1.3900 .
C45 C50 1.3900 .
C46 C47 1.3900 .
C46 H46 0.9300 .
C47 C48 1.3900 .
C47 H47 0.9300 .
C48 C49 1.3900 .
C48 H48 0.9300 .
C49 C50 1.3900 .
C49 H49 0.9300 .
C50 H50 0.9300 .
C51 N12 1.416(16) .
C51 C52 1.496(15) .
C51 H51A 0.9700 .
C51 H51B 0.9700 .
C52 C53 1.3900 .
C52 C57 1.3900 .
C53 C54 1.3900 .
C53 H53 0.9300 .
C54 C55 1.3900 .
C54 H54 0.9300 .
C55 C56 1.3900 .
C55 H55 0.9300 .
C56 C57 1.3900 .
C56 H56 0.9300 .
C57 H57 0.9300 .
N5 C23 1.387(18) 2_565
N5 C21 1.437(15) 2_565
C58 Cl1 1.731(15) .
C58 Cl2 1.752(17) .
C58 Cl3 1.782(17) .
C58 H58 0.9800 .
C61 Cl12 1.712(18) .
C61 Cl11 1.756(17) .
C61 Cl10 1.758(17) .
C61 H61 0.9800 .
C361 Cl32 1.714(19) .
C361 Cl30 1.730(19) .
C361 Cl31 1.74(2) .
C361 H361 0.9800 .
C59 Cl5 1.58(2) .
C59 Cl6 1.71(2) .
C59 Cl4 1.82(3) .
C59 H59 0.9800 .
C60 Cl9 1.702(18) .
C60 Cl8 1.735(18) .
C60 Cl7 1.741(18) .
C60 H60 0.9800 .
C260 Cl29 1.721(18) .
C260 Cl27 1.742(19) .
C260 Cl28 1.751(18) .
C260 H260 0.9800 .
C62 Cl15 1.750(19) .
C62 Cl13 1.752(19) .
C62 Cl14 1.758(19) .
C62 H62 0.9800 .
C362 Cl33 1.74(2) .
C362 Cl35 1.76(2) .
C362 Cl34 1.78(2) .
C362 H362 0.9800 .
