#------------------------------------------------------------------------------
#$Date: 2016-03-21 03:38:45 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178435 $
#$URL: svn://www.crystallography.net/cod/cif/4/02/56/4025675.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_4025675
loop_
_publ_author_name
'Grazia Cafeo'
'Howard M. Colquhoun'
'Angela Cuzzola'
'Mario Gattuso'
'Franz H. Kohnke'
'Luca Valenti'
'Andrew J. P. White'
_publ_section_title
;
 Synthesis, X-ray Structure, and Anion-Binding Properties of a
 Cryptand-Like Hybrid Calixpyrrole
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              6263
_journal_page_last               6266
_journal_paper_doi               10.1021/jo1010262
_journal_volume                  75
_journal_year                    2010
_chemical_formula_moiety         'C62 H68 N6, 3(C3 H6 O)'
_chemical_formula_sum            'C71 H86 N6 O3'
_chemical_formula_weight         1071.46
_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                 102.5717(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3422(2)
_cell_length_b                   22.6427(4)
_cell_length_c                   21.7077(3)
_cell_measurement_reflns_used    14699
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.8406
_cell_measurement_theta_min      2.8363
_cell_volume                     6400.74(18)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 15.9863
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.839
_diffrn_measurement_device_type  'OD Xcalibur 3'
_diffrn_measurement_method       'omega scans'
_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  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            41615
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.90
_diffrn_reflns_theta_min         2.84
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.981
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) 
(compiled Feb 27 2009,15:38:38) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     789
_refine_ls_number_reflns         20074
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0511
_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)+(0.0704P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1244
_refine_ls_wR_factor_ref         0.1328
_reflns_number_gt                11778
_reflns_number_total             20074
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo1010262_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4025675
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
C1 C 0.24519(9) 0.62753(5) 0.81837(5) 0.0286(2) Uani 1 1 d . . .
H1A H 0.2945 0.6127 0.8567 0.034 Uiso 1 1 calc R . .
C2 C 0.26633(9) 0.59607(5) 0.76113(6) 0.0311(3) Uani 1 1 d . . .
N3 N 0.36228(8) 0.59803(5) 0.74839(5) 0.0350(2) Uani 1 1 d D . .
H3 H 0.4165(7) 0.6169(6) 0.7721(6) 0.057(5) Uiso 1 1 d D . .
C4 C 0.36220(11) 0.57225(5) 0.69124(6) 0.0382(3) Uani 1 1 d . . .
C5 C 0.26425(11) 0.55239(6) 0.66807(6) 0.0411(3) Uani 1 1 d . . .
H5A H 0.2409 0.5321 0.6293 0.049 Uiso 1 1 calc R . .
C6 C 0.20363(11) 0.56735(5) 0.71208(6) 0.0373(3) Uani 1 1 d . . .
H6A H 0.1327 0.5590 0.7082 0.045 Uiso 1 1 calc R . .
C7 C 0.45747(11) 0.57480(7) 0.66406(6) 0.0470(4) Uani 1 1 d . . .
C8 C 0.43862(15) 0.53872(7) 0.60224(7) 0.0621(5) Uani 1 1 d . . .
H8A H 0.3809 0.5559 0.5717 0.093 Uiso 1 1 calc R . .
H8B H 0.4226 0.4977 0.6110 0.093 Uiso 1 1 calc R . .
H8C H 0.5004 0.5397 0.5848 0.093 Uiso 1 1 calc R . .
C9 C 0.54835(13) 0.54681(9) 0.71103(8) 0.0683(5) Uani 1 1 d . . .
H9A H 0.5619 0.5694 0.7505 0.102 Uiso 1 1 calc R . .
H9B H 0.6095 0.5473 0.6929 0.102 Uiso 1 1 calc R . .
H9C H 0.5314 0.5059 0.7196 0.102 Uiso 1 1 calc R . .
C10 C 0.47682(10) 0.63922(6) 0.64939(6) 0.0408(3) Uani 1 1 d . . .
C11 C 0.39483(9) 0.67285(6) 0.61558(5) 0.0344(3) Uani 1 1 d . . .
H11A H 0.3294 0.6546 0.6031 0.041 Uiso 1 1 calc R . .
C12 C 0.40472(9) 0.73124(6) 0.59962(5) 0.0341(3) Uani 1 1 d . . .
C13 C 0.50134(10) 0.75776(7) 0.61840(7) 0.0476(4) Uani 1 1 d . . .
H13A H 0.5104 0.7980 0.6083 0.057 Uiso 1 1 calc R . .
C14 C 0.58342(12) 0.72567(9) 0.65149(8) 0.0610(5) Uani 1 1 d . . .
H14A H 0.6488 0.7440 0.6637 0.073 Uiso 1 1 calc R . .
C15 C 0.57212(11) 0.66740(8) 0.66710(7) 0.0548(4) Uani 1 1 d . . .
H15A H 0.6296 0.6462 0.6901 0.066 Uiso 1 1 calc R . .
C16 C 0.31400(9) 0.76653(6) 0.56051(6) 0.0339(3) Uani 1 1 d . . .
C17 C 0.33016(12) 0.77342(8) 0.49279(7) 0.0563(4) Uani 1 1 d . . .
H17A H 0.2730 0.7960 0.4675 0.084 Uiso 1 1 calc R . .
H17B H 0.3330 0.7343 0.4739 0.084 Uiso 1 1 calc R . .
H17C H 0.3947 0.7944 0.4938 0.084 Uiso 1 1 calc R . .
C18 C 0.30821(12) 0.82842(6) 0.58909(8) 0.0488(4) Uani 1 1 d . . .
H18A H 0.2503 0.8502 0.5636 0.073 Uiso 1 1 calc R . .
H18B H 0.3722 0.8498 0.5895 0.073 Uiso 1 1 calc R . .
H18C H 0.2985 0.8246 0.6324 0.073 Uiso 1 1 calc R . .
C19 C 0.21480(9) 0.73394(5) 0.55841(5) 0.0266(2) Uani 1 1 d . . .
N20 N 0.16400(7) 0.73814(4) 0.60704(4) 0.0267(2) Uani 1 1 d D . .
H20 H 0.1826(10) 0.7625(4) 0.6403(4) 0.036(4) Uiso 1 1 d D . .
C21 C 0.08183(8) 0.70043(5) 0.59786(5) 0.0243(2) Uani 1 1 d . . .
C22 C 0.07997(9) 0.67108(5) 0.54258(5) 0.0281(2) Uani 1 1 d . . .
H22A H 0.0317 0.6418 0.5241 0.034 Uiso 1 1 calc R . .
C23 C 0.16327(9) 0.69221(5) 0.51782(5) 0.0294(2) Uani 1 1 d . . .
H23A H 0.1804 0.6796 0.4797 0.035 Uiso 1 1 calc R . .
C24 C 0.01868(8) 0.69469(5) 0.64721(5) 0.0243(2) Uani 1 1 d . . .
H24A H 0.0651 0.6785 0.6860 0.029 Uiso 1 1 calc R . .
C25 C -0.02075(9) 0.75285(5) 0.66511(5) 0.0256(2) Uani 1 1 d . . .
N26 N -0.04965(7) 0.75825(4) 0.72174(4) 0.0261(2) Uani 1 1 d D . .
H26 H -0.0397(11) 0.7282(4) 0.7495(5) 0.045(4) Uiso 1 1 d D . .
C27 C -0.09008(9) 0.81309(5) 0.72788(5) 0.0272(2) Uani 1 1 d . . .
C28 C -0.08730(11) 0.84290(5) 0.67381(6) 0.0382(3) Uani 1 1 d . . .
H28A H -0.1105 0.8822 0.6642 0.046 Uiso 1 1 calc R . .
C29 C -0.04369(11) 0.80524(6) 0.63424(6) 0.0377(3) Uani 1 1 d . . .
H29A H -0.0326 0.8148 0.5936 0.045 Uiso 1 1 calc R . .
C30 C -0.12700(9) 0.83046(5) 0.78637(6) 0.0304(2) Uani 1 1 d . . .
C31 C -0.20184(11) 0.78295(7) 0.80018(7) 0.0471(3) Uani 1 1 d . . .
H31A H -0.1656 0.7452 0.8089 0.071 Uiso 1 1 calc R . .
H31B H -0.2589 0.7786 0.7635 0.071 Uiso 1 1 calc R . .
H31C H -0.2286 0.7948 0.8369 0.071 Uiso 1 1 calc R . .
C32 C -0.18562(11) 0.88924(6) 0.77311(7) 0.0473(3) Uani 1 1 d . . .
H32A H -0.1390 0.9200 0.7643 0.071 Uiso 1 1 calc R . .
H32B H -0.2124 0.9005 0.8100 0.071 Uiso 1 1 calc R . .
H32C H -0.2428 0.8846 0.7365 0.071 Uiso 1 1 calc R . .
C33 C -0.03833(9) 0.83764(5) 0.84431(6) 0.0319(3) Uani 1 1 d . . .
C34 C 0.06425(9) 0.83451(5) 0.84111(6) 0.0305(2) Uani 1 1 d . . .
H34A H 0.0809 0.8283 0.8012 0.037 Uiso 1 1 calc R . .
C35 C 0.14424(10) 0.84018(5) 0.89474(6) 0.0348(3) Uani 1 1 d . . .
C36 C 0.11948(12) 0.84931(7) 0.95262(7) 0.0542(4) Uani 1 1 d . . .
H36A H 0.1725 0.8528 0.9896 0.065 Uiso 1 1 calc R . .
C37 C 0.01783(13) 0.85332(9) 0.95691(7) 0.0670(5) Uani 1 1 d . . .
H37A H 0.0013 0.8598 0.9968 0.080 Uiso 1 1 calc R . .
C38 C -0.05995(12) 0.84791(7) 0.90358(7) 0.0515(4) Uani 1 1 d . . .
H38A H -0.1294 0.8512 0.9073 0.062 Uiso 1 1 calc R . .
C39 C 0.25614(10) 0.83772(5) 0.88733(6) 0.0381(3) Uani 1 1 d . . .
C40 C 0.33231(12) 0.82764(7) 0.95042(7) 0.0609(5) Uani 1 1 d . . .
H40A H 0.4024 0.8267 0.9434 0.091 Uiso 1 1 calc R . .
H40B H 0.3171 0.7899 0.9686 0.091 Uiso 1 1 calc R . .
H40C H 0.3261 0.8598 0.9796 0.091 Uiso 1 1 calc R . .
C41 C 0.28069(13) 0.89671(6) 0.85985(9) 0.0608(5) Uani 1 1 d . . .
H41A H 0.2324 0.9036 0.8195 0.091 Uiso 1 1 calc R . .
H41B H 0.3509 0.8958 0.8531 0.091 Uiso 1 1 calc R . .
H41C H 0.2744 0.9286 0.8893 0.091 Uiso 1 1 calc R . .
C42 C 0.26745(8) 0.78818(5) 0.84262(6) 0.0293(2) Uani 1 1 d . . .
N43 N 0.25694(8) 0.73104(4) 0.86043(4) 0.0287(2) Uani 1 1 d D . .
H43 H 0.2494(12) 0.7191(6) 0.8987(3) 0.050(4) Uiso 1 1 d D . .
C44 C 0.26260(8) 0.69283(5) 0.81207(5) 0.0259(2) Uani 1 1 d . . .
C45 C 0.27959(9) 0.72618(5) 0.76303(5) 0.0307(2) Uani 1 1 d . . .
H45A H 0.2881 0.7119 0.7233 0.037 Uiso 1 1 calc R . .
C46 C 0.28228(9) 0.78654(5) 0.78249(6) 0.0334(3) Uani 1 1 d . . .
H46A H 0.2926 0.8197 0.7578 0.040 Uiso 1 1 calc R . .
C47 C 0.13705(9) 0.61607(5) 0.82619(5) 0.0296(2) Uani 1 1 d . . .
N48 N 0.10068(8) 0.55976(4) 0.82902(5) 0.0336(2) Uani 1 1 d D . .
H48 H 0.1424(10) 0.5283(4) 0.8308(7) 0.063(5) Uiso 1 1 d D . .
C49 C 0.00034(9) 0.56058(5) 0.83515(5) 0.0321(3) Uani 1 1 d . . .
C50 C -0.02686(10) 0.61844(6) 0.83710(6) 0.0367(3) Uani 1 1 d . . .
H50A H -0.0919 0.6328 0.8413 0.044 Uiso 1 1 calc R . .
C51 C 0.05903(10) 0.65344(5) 0.83175(6) 0.0337(3) Uani 1 1 d . . .
H51A H 0.0618 0.6954 0.8320 0.040 Uiso 1 1 calc R . .
C52 C -0.05780(10) 0.50353(6) 0.83715(6) 0.0376(3) Uani 1 1 d . . .
C53 C -0.16895(11) 0.51729(7) 0.84075(7) 0.0463(3) Uani 1 1 d . . .
H53A H -0.2029 0.5389 0.8028 0.069 Uiso 1 1 calc R . .
H53B H -0.1692 0.5415 0.8782 0.069 Uiso 1 1 calc R . .
H53C H -0.2058 0.4803 0.8436 0.069 Uiso 1 1 calc R . .
C54 C -0.00663(14) 0.46939(7) 0.89739(7) 0.0588(4) Uani 1 1 d . . .
H54A H -0.0082 0.4936 0.9346 0.088 Uiso 1 1 calc R . .
H54B H 0.0648 0.4605 0.8962 0.088 Uiso 1 1 calc R . .
H54C H -0.0440 0.4325 0.8996 0.088 Uiso 1 1 calc R . .
C55 C -0.05852(9) 0.46803(5) 0.77682(6) 0.0340(3) Uani 1 1 d . . .
C56 C -0.09542(9) 0.49501(5) 0.71863(5) 0.0314(3) Uani 1 1 d . . .
H56A H -0.1173 0.5350 0.7179 0.038 Uiso 1 1 calc R . .
C57 C -0.10155(9) 0.46579(5) 0.66142(6) 0.0339(3) Uani 1 1 d . . .
C58 C -0.06918(11) 0.40715(6) 0.66391(8) 0.0472(4) Uani 1 1 d . . .
H58A H -0.0731 0.3857 0.6258 0.057 Uiso 1 1 calc R . .
C59 C -0.03160(12) 0.38003(6) 0.72091(9) 0.0553(4) Uani 1 1 d . . .
H59A H -0.0091 0.3402 0.7217 0.066 Uiso 1 1 calc R . .
C60 C -0.02602(11) 0.40978(6) 0.77699(8) 0.0470(4) Uani 1 1 d . . .
H60A H 0.0002 0.3903 0.8159 0.056 Uiso 1 1 calc R . .
C61 C -0.14603(11) 0.49649(6) 0.59844(6) 0.0392(3) Uani 1 1 d . . .
C62 C -0.25787(13) 0.47646(7) 0.57506(7) 0.0561(4) Uani 1 1 d . . .
H62A H -0.2976 0.4868 0.6065 0.084 Uiso 1 1 calc R . .
H62B H -0.2598 0.4336 0.5686 0.084 Uiso 1 1 calc R . .
H62C H -0.2875 0.4962 0.5351 0.084 Uiso 1 1 calc R . .
C63 C -0.08460(17) 0.47984(7) 0.54838(8) 0.0736(6) Uani 1 1 d . . .
H63A H -0.0131 0.4926 0.5627 0.110 Uiso 1 1 calc R . .
H63B H -0.1149 0.4994 0.5084 0.110 Uiso 1 1 calc R . .
H63C H -0.0868 0.4369 0.5422 0.110 Uiso 1 1 calc R . .
C64 C -0.14357(9) 0.56254(5) 0.60628(5) 0.0306(3) Uani 1 1 d . . .
N65 N -0.05185(8) 0.59283(4) 0.62025(4) 0.0281(2) Uani 1 1 d D . .
H65 H 0.0109(4) 0.5769(5) 0.6237(6) 0.042(4) Uiso 1 1 d D . .
C66 C -0.06892(9) 0.65178(5) 0.62863(5) 0.0250(2) Uani 1 1 d . . .
C67 C -0.17240(9) 0.65922(6) 0.61996(5) 0.0322(3) Uani 1 1 d . . .
H67A H -0.2070 0.6955 0.6228 0.039 Uiso 1 1 calc R . .
C68 C -0.21927(9) 0.60311(6) 0.60587(5) 0.0341(3) Uani 1 1 d . . .
H68A H -0.2909 0.5952 0.5976 0.041 Uiso 1 1 calc R . .
O70 O 0.52421(10) 0.62286(5) 0.86012(5) 0.0689(3) Uani 1 1 d . . .
C70 C 0.52961(11) 0.66886(7) 0.88952(7) 0.0486(4) Uani 1 1 d . . .
C71 C 0.53890(14) 0.72668(8) 0.85898(8) 0.0628(4) Uani 1 1 d . . .
H71A H 0.5491 0.7202 0.8161 0.094 Uiso 1 1 calc R . .
H71B H 0.5977 0.7484 0.8836 0.094 Uiso 1 1 calc R . .
H71C H 0.4761 0.7497 0.8571 0.094 Uiso 1 1 calc R . .
C72 C 0.52402(15) 0.66929(9) 0.95704(8) 0.0721(5) Uani 1 1 d . . .
H72A H 0.4552 0.6816 0.9608 0.108 Uiso 1 1 calc R . .
H72B H 0.5750 0.6970 0.9802 0.108 Uiso 1 1 calc R . .
H72C H 0.5382 0.6296 0.9747 0.108 Uiso 1 1 calc R . .
O80 O 0.2863(4) 0.6620(2) 0.9751(2) 0.0803(17) Uani 0.745(10) 1 d PD A 1
C80 C 0.2234(3) 0.6341(2) 0.99551(19) 0.055(2) Uani 0.745(10) 1 d PD A 1
C81 C 0.1247(4) 0.6612(2) 1.0022(3) 0.119(2) Uani 0.745(10) 1 d PD A 1
H81A H 0.1221 0.7023 0.9878 0.179 Uiso 0.745(10) 1 calc PR A 1
H81B H 0.1199 0.6600 1.0466 0.179 Uiso 0.745(10) 1 calc PR A 1
H81C H 0.0673 0.6392 0.9765 0.179 Uiso 0.745(10) 1 calc PR A 1
C82 C 0.2415(5) 0.57014(15) 1.0117(2) 0.0908(13) Uani 0.745(10) 1 d PD A 1
H82A H 0.1908 0.5461 0.9829 0.136 Uiso 0.745(10) 1 calc PR A 1
H82B H 0.2348 0.5634 1.0553 0.136 Uiso 0.745(10) 1 calc PR A 1
H82C H 0.3108 0.5591 1.0077 0.136 Uiso 0.745(10) 1 calc PR A 1
O80' O 0.2804(12) 0.6580(5) 0.9708(7) 0.059(4) Uiso 0.255(10) 1 d PD A 2
C80' C 0.2204(13) 0.6364(6) 0.9983(7) 0.075(9) Uiso 0.255(10) 1 d PD A 2
C81' C 0.1667(9) 0.6715(4) 1.0385(6) 0.075(3) Uiso 0.255(10) 1 d PD A 2
H81D H 0.2033 0.6682 1.0827 0.113 Uiso 0.255(10) 1 calc PR A 2
H81E H 0.0964 0.6567 1.0340 0.113 Uiso 0.255(10) 1 calc PR A 2
H81F H 0.1646 0.7130 1.0255 0.113 Uiso 0.255(10) 1 calc PR A 2
C82' C 0.1960(11) 0.5729(4) 0.9944(5) 0.074(3) Uiso 0.255(10) 1 d PD A 2
H82D H 0.1235 0.5674 0.9738 0.111 Uiso 0.255(10) 1 calc PR A 2
H82E H 0.2087 0.5561 1.0370 0.111 Uiso 0.255(10) 1 calc PR A 2
H82F H 0.2393 0.5528 0.9697 0.111 Uiso 0.255(10) 1 calc PR A 2
O90 O 0.27169(15) 0.47973(9) 0.88647(11) 0.0672(6) Uani 0.771(5) 1 d PD B 1
C90 C 0.3471(3) 0.46699(13) 0.86600(14) 0.0458(12) Uani 0.771(5) 1 d PD B 1
C91 C 0.4518(2) 0.47892(16) 0.90297(18) 0.0944(11) Uani 0.771(5) 1 d PD B 1
H91A H 0.4479 0.4948 0.9444 0.142 Uiso 0.771(5) 1 calc PR B 1
H91B H 0.4855 0.5077 0.8805 0.142 Uiso 0.771(5) 1 calc PR B 1
H91C H 0.4914 0.4421 0.9086 0.142 Uiso 0.771(5) 1 calc PR B 1
C92 C 0.3339(3) 0.44004(11) 0.80275(10) 0.0721(10) Uani 0.771(5) 1 d PD B 1
H92A H 0.2611 0.4313 0.7862 0.108 Uiso 0.771(5) 1 calc PR B 1
H92B H 0.3737 0.4034 0.8058 0.108 Uiso 0.771(5) 1 calc PR B 1
H92C H 0.3581 0.4676 0.7743 0.108 Uiso 0.771(5) 1 calc PR B 1
O90' O 0.2651(6) 0.4675(4) 0.8603(4) 0.074(2) Uiso 0.229(5) 1 d PD B 2
C90' C 0.3570(11) 0.4656(7) 0.8650(6) 0.084(8) Uiso 0.229(5) 1 d PD B 2
C91' C 0.4274(9) 0.4536(6) 0.9269(5) 0.097(4) Uiso 0.229(5) 1 d PD B 2
H91D H 0.4784 0.4853 0.9366 0.146 Uiso 0.229(5) 1 calc PR B 2
H91E H 0.4624 0.4158 0.9249 0.146 Uiso 0.229(5) 1 calc PR B 2
H91F H 0.3878 0.4518 0.9599 0.146 Uiso 0.229(5) 1 calc PR B 2
C92' C 0.4048(6) 0.4689(4) 0.8098(3) 0.056(2) Uiso 0.229(5) 1 d PD B 2
H92D H 0.4382 0.4312 0.8048 0.085 Uiso 0.229(5) 1 calc PR B 2
H92E H 0.4561 0.5006 0.8163 0.085 Uiso 0.229(5) 1 calc PR B 2
H92F H 0.3519 0.4772 0.7718 0.085 Uiso 0.229(5) 1 calc PR B 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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
_geom_angle_publ_flag
C44 C1 C2 109.13(9) . . ?
C44 C1 C47 110.38(9) . . ?
C2 C1 C47 111.41(10) . . ?
C6 C2 N3 107.40(11) . . ?
C6 C2 C1 132.26(12) . . ?
N3 C2 C1 120.09(10) . . ?
C2 N3 C4 110.65(11) . . ?
C5 C4 N3 106.55(11) . . ?
C5 C4 C7 133.14(12) . . ?
N3 C4 C7 120.07(12) . . ?
C4 C5 C6 108.18(11) . . ?
C2 C6 C5 107.20(12) . . ?
C4 C7 C10 108.19(10) . . ?
C4 C7 C9 109.44(12) . . ?
C10 C7 C9 112.74(14) . . ?
C4 C7 C8 109.07(13) . . ?
C10 C7 C8 109.09(12) . . ?
C9 C7 C8 108.25(12) . . ?
C15 C10 C11 117.06(14) . . ?
C15 C10 C7 124.26(13) . . ?
C11 C10 C7 118.68(12) . . ?
C12 C11 C10 123.04(12) . . ?
C11 C12 C13 118.04(13) . . ?
C11 C12 C16 121.87(11) . . ?
C13 C12 C16 120.06(13) . . ?
C14 C13 C12 120.16(15) . . ?
C13 C14 C15 121.02(14) . . ?
C14 C15 C10 120.68(14) . . ?
C19 C16 C17 108.98(10) . . ?
C19 C16 C18 109.68(10) . . ?
C17 C16 C18 108.78(11) . . ?
C19 C16 C12 110.00(10) . . ?
C17 C16 C12 108.78(11) . . ?
C18 C16 C12 110.59(11) . . ?
C23 C19 N20 106.20(10) . . ?
C23 C19 C16 132.17(10) . . ?
N20 C19 C16 121.24(10) . . ?
C21 N20 C19 110.95(9) . . ?
C22 C21 N20 106.96(9) . . ?
C22 C21 C24 132.57(10) . . ?
N20 C21 C24 120.30(9) . . ?
C21 C22 C23 107.61(10) . . ?
C19 C23 C22 108.28(10) . . ?
C25 C24 C21 112.99(9) . . ?
C25 C24 C66 109.89(9) . . ?
C21 C24 C66 112.77(9) . . ?
C29 C25 N26 106.62(10) . . ?
C29 C25 C24 133.62(10) . . ?
N26 C25 C24 119.55(9) . . ?
C25 N26 C27 111.16(9) . . ?
C28 C27 N26 106.25(10) . . ?
C28 C27 C30 132.12(11) . . ?
N26 C27 C30 121.63(10) . . ?
C27 C28 C29 108.37(11) . . ?
C25 C29 C28 107.60(10) . . ?
C27 C30 C33 112.44(9) . . ?
C27 C30 C32 108.26(10) . . ?
C33 C30 C32 109.33(10) . . ?
C27 C30 C31 108.99(9) . . ?
C33 C30 C31 109.32(11) . . ?
C32 C30 C31 108.40(11) . . ?
C34 C33 C38 117.26(12) . . ?
C34 C33 C30 123.09(10) . . ?
C38 C33 C30 119.65(11) . . ?
C33 C34 C35 122.29(11) . . ?
C36 C35 C34 118.59(12) . . ?
C36 C35 C39 122.02(12) . . ?
C34 C35 C39 119.37(11) . . ?
C37 C36 C35 120.20(13) . . ?
C38 C37 C36 120.44(13) . . ?
C37 C38 C33 121.20(13) . . ?
C42 C39 C41 109.77(12) . . ?
C42 C39 C40 108.87(10) . . ?
C41 C39 C40 108.78(12) . . ?
C42 C39 C35 109.20(10) . . ?
C41 C39 C35 107.76(11) . . ?
C40 C39 C35 112.44(12) . . ?
C46 C42 N43 106.90(10) . . ?
C46 C42 C39 133.68(12) . . ?
N43 C42 C39 119.34(11) . . ?
C42 N43 C44 110.71(9) . . ?
C45 C44 N43 107.07(10) . . ?
C45 C44 C1 131.99(10) . . ?
N43 C44 C1 120.85(10) . . ?
C44 C45 C46 107.26(10) . . ?
C42 C46 C45 108.04(10) . . ?
C51 C47 N48 106.74(11) . . ?
C51 C47 C1 131.87(11) . . ?
N48 C47 C1 121.39(10) . . ?
C47 N48 C49 110.72(10) . . ?
C50 C49 N48 106.72(11) . . ?
C50 C49 C52 132.74(12) . . ?
N48 C49 C52 120.52(11) . . ?
C49 C50 C51 108.02(11) . . ?
C47 C51 C50 107.79(11) . . ?
C49 C52 C53 109.61(11) . . ?
C49 C52 C55 109.32(10) . . ?
C53 C52 C55 108.87(11) . . ?
C49 C52 C54 108.46(11) . . ?
C53 C52 C54 108.21(11) . . ?
C55 C52 C54 112.33(12) . . ?
C60 C55 C56 117.89(12) . . ?
C60 C55 C52 123.46(12) . . ?
C56 C55 C52 118.64(11) . . ?
C55 C56 C57 122.71(11) . . ?
C58 C57 C56 117.40(13) . . ?
C58 C57 C61 121.54(11) . . ?
C56 C57 C61 121.03(11) . . ?
C59 C58 C57 120.65(13) . . ?
C58 C59 C60 121.02(13) . . ?
C59 C60 C55 120.32(14) . . ?
C64 C61 C57 110.80(9) . . ?
C64 C61 C62 109.06(12) . . ?
C57 C61 C62 108.68(10) . . ?
C64 C61 C63 108.69(10) . . ?
C57 C61 C63 110.80(13) . . ?
C62 C61 C63 108.76(12) . . ?
C68 C64 N65 106.68(10) . . ?
C68 C64 C61 132.13(11) . . ?
N65 C64 C61 121.08(11) . . ?
C66 N65 C64 110.38(10) . . ?
C67 C66 N65 107.11(10) . . ?
C67 C66 C24 131.40(10) . . ?
N65 C66 C24 121.42(10) . . ?
C66 C67 C68 107.74(11) . . ?
C64 C68 C67 108.09(11) . . ?
O70 C70 C72 120.95(16) . . ?
O70 C70 C71 121.49(15) . . ?
C72 C70 C71 117.54(15) . . ?
O80 C80 C81 121.3(4) . . ?
O80 C80 C82 120.1(4) . . ?
C81 C80 C82 118.5(3) . . ?
O80' C80' C82' 122.2(11) . . ?
O80' C80' C81' 122.3(11) . . ?
C82' C80' C81' 115.5(10) . . ?
O90 C90 C91 121.1(3) . . ?
O90 C90 C92 119.7(3) . . ?
C91 C90 C92 119.2(3) . . ?
O90' C90' C92' 122.6(11) . . ?
O90' C90' C91' 120.9(11) . . ?
C92' C90' C91' 116.2(10) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C44 1.5075(16) . ?
C1 C2 1.5111(16) . ?
C1 C47 1.5114(16) . ?
C2 C6 1.3670(16) . ?
C2 N3 1.3679(16) . ?
N3 C4 1.3707(15) . ?
C4 C5 1.370(2) . ?
C4 C7 1.514(2) . ?
C5 C6 1.4206(19) . ?
C7 C10 1.527(2) . ?
C7 C9 1.541(2) . ?
C7 C8 1.5443(19) . ?
C10 C15 1.400(2) . ?
C10 C11 1.4020(18) . ?
C11 C12 1.3803(18) . ?
C12 C13 1.3998(18) . ?
C12 C16 1.5419(18) . ?
C13 C14 1.379(2) . ?
C14 C15 1.379(2) . ?
C16 C19 1.5073(16) . ?
C16 C17 1.5395(17) . ?
C16 C18 1.5414(19) . ?
C19 C23 1.3704(16) . ?
C19 N20 1.3764(14) . ?
N20 C21 1.3696(14) . ?
C21 C22 1.3674(15) . ?
C21 C24 1.5057(14) . ?
C22 C23 1.4188(16) . ?
C24 C25 1.5004(15) . ?
C24 C66 1.5058(15) . ?
C25 C29 1.3640(16) . ?
C25 N26 1.3715(14) . ?
N26 C27 1.3718(14) . ?
C27 C28 1.3615(17) . ?
C27 C30 1.5105(15) . ?
C28 C29 1.4217(17) . ?
C30 C33 1.5363(17) . ?
C30 C32 1.5388(18) . ?
C30 C31 1.5410(18) . ?
C33 C34 1.3872(16) . ?
C33 C38 1.3981(17) . ?
C34 C35 1.4035(17) . ?
C35 C36 1.3826(19) . ?
C35 C39 1.5370(17) . ?
C36 C37 1.383(2) . ?
C37 C38 1.382(2) . ?
C39 C42 1.5122(16) . ?
C39 C41 1.527(2) . ?
C39 C40 1.535(2) . ?
C42 C46 1.3625(16) . ?
C42 N43 1.3663(15) . ?
N43 C44 1.3751(14) . ?
C44 C45 1.3639(16) . ?
C45 C46 1.4286(17) . ?
C47 C51 1.3671(17) . ?
C47 N48 1.3704(15) . ?
N48 C49 1.3740(16) . ?
C49 C50 1.3625(17) . ?
C49 C52 1.5122(17) . ?
C50 C51 1.4188(17) . ?
C52 C53 1.5339(19) . ?
C52 C55 1.5348(18) . ?
C52 C54 1.5445(18) . ?
C55 C60 1.3882(18) . ?
C55 C56 1.3929(17) . ?
C56 C57 1.3938(16) . ?
C57 C58 1.3936(19) . ?
C57 C61 1.5334(19) . ?
C58 C59 1.375(2) . ?
C59 C60 1.379(2) . ?
C61 C64 1.5046(17) . ?
C61 C62 1.536(2) . ?
C61 C63 1.5436(18) . ?
C64 C68 1.3639(18) . ?
C64 N65 1.3779(15) . ?
N65 C66 1.3728(14) . ?
C66 C67 1.3626(16) . ?
C67 C68 1.4197(17) . ?
O70 C70 1.2154(18) . ?
C70 C72 1.484(2) . ?
C70 C71 1.485(2) . ?
O80 C80 1.208(4) . ?
C80 C81 1.488(5) . ?
C80 C82 1.497(5) . ?
O80' C80' 1.202(12) . ?
C80' C82' 1.473(12) . ?
C80' C81' 1.477(12) . ?
O90 C90 1.220(4) . ?
C90 C91 1.476(4) . ?
C90 C92 1.478(4) . ?
O90' C90' 1.208(13) . ?
C90' C92' 1.477(12) . ?
C90' C91' 1.486(12) . ?
