#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:37:24 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179589 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/54/4505426.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_4505426
loop_
_publ_author_name
'Ma, Bao-Qing'
'Coppens, Philip'
_publ_section_title
;
 Variable Conformation of Benzophenone in a Series of Resorcinarene-Based
 Supramolecular Frameworks
;
_journal_issue                   6
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1377
_journal_paper_doi               10.1021/cg0499562
_journal_volume                  4
_journal_year                    2004
_chemical_formula_sum            'C90 H88 N8 O10'
_chemical_formula_weight         1441.68
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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
_cell_angle_alpha                99.649(3)
_cell_angle_beta                 107.176(3)
_cell_angle_gamma                90.599(3)
_cell_formula_units_Z            2
_cell_length_a                   15.8791(10)
_cell_length_b                   15.9052(12)
_cell_length_c                   15.9729(9)
_cell_measurement_temperature    90(1)
_cell_volume                     3792.0(4)
_computing_cell_refinement       SMART
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(1)
_diffrn_measured_fraction_theta_full 0.846
_diffrn_measured_fraction_theta_max 0.846
_diffrn_measurement_device_type  'SMART CCD 1000'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_sigmaI/netI    0.1598
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41090
_diffrn_reflns_theta_full        31.09
_diffrn_reflns_theta_max         31.09
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    0.083
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.627
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.0116(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.872
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1393
_refine_ls_number_reflns         20623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.872
_refine_ls_R_factor_all          0.1576
_refine_ls_R_factor_gt           0.0622
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0661P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1614
_reflns_number_gt                8814
_reflns_number_total             20623
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg0499562si20040122_042301.cif
_cod_data_source_block           p-1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4505426
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
O1 O 1.36912(11) -0.86335(11) 0.84786(11) 0.0252(4) Uani 1 1 d . . .
O2 O 1.38945(11) -1.07201(11) 1.02634(11) 0.0262(4) Uani 1 1 d . . .
O3 O 1.33102(11) -1.13976(10) 1.15537(11) 0.0250(4) Uani 1 1 d . . .
O4 O 1.28806(11) -0.93723(11) 1.39674(10) 0.0254(4) Uani 1 1 d . . .
O5 O 1.34323(12) -0.77190(12) 1.39306(11) 0.0319(4) Uani 1 1 d . . .
O6 O 1.34725(12) -0.55806(11) 1.22421(12) 0.0333(4) Uani 1 1 d . . .
O7 O 1.28864(12) -0.50222(10) 1.05802(11) 0.0288(4) Uani 1 1 d . . .
O8 O 1.29802(11) -0.70955(10) 0.80446(11) 0.0278(4) Uani 1 1 d . . .
O9 O 0.17685(17) 0.71538(16) 0.54719(17) 0.0740(8) Uani 1 1 d . . .
C1 C 1.23816(14) -0.89787(13) 0.88796(14) 0.0185(5) Uani 1 1 d . . .
C2 C 1.32599(15) -0.90835(14) 0.89126(14) 0.0195(5) Uani 1 1 d . . .
C3 C 1.37476(15) -0.96679(14) 0.93756(15) 0.0207(5) Uani 1 1 d . . .
C4 C 1.33585(14) -1.01675(14) 0.98101(14) 0.0191(5) Uani 1 1 d . . .
C5 C 1.24768(14) -1.01024(13) 0.97821(14) 0.0182(5) Uani 1 1 d . . .
C6 C 1.20152(15) -0.94998(14) 0.93121(14) 0.0188(5) Uani 1 1 d . . .
C7 C 1.20566(14) -1.06622(14) 1.02537(14) 0.0180(5) Uani 1 1 d . . .
C8 C 1.10573(15) -1.08257(16) 0.98371(16) 0.0240(5) Uani 1 1 d . . .
C9 C 1.06738(19) -1.1499(2) 1.0220(2) 0.0362(7) Uani 1 1 d . . .
C10 C 1.23010(14) -1.03186(14) 1.12467(14) 0.0190(5) Uani 1 1 d . . .
C11 C 1.28988(15) -1.07159(14) 1.18668(15) 0.0208(5) Uani 1 1 d . . .
C12 C 1.30931(15) -1.04128(15) 1.27766(15) 0.0216(5) Uani 1 1 d . . .
C13 C 1.26929(15) -0.96959(14) 1.30752(14) 0.0212(5) Uani 1 1 d . . .
C14 C 1.21076(14) -0.92720(14) 1.24781(14) 0.0192(5) Uani 1 1 d . . .
C15 C 1.19376(14) -0.95964(14) 1.15791(15) 0.0191(5) Uani 1 1 d . . .
C16 C 1.16943(15) -0.84683(14) 1.28022(15) 0.0202(5) Uani 1 1 d . . .
C17 C 1.06925(15) -0.85336(16) 1.24007(17) 0.0236(5) Uani 1 1 d . . .
C18 C 1.02505(19) -0.92001(19) 1.2736(2) 0.0346(7) Uani 1 1 d . . .
C19 C 1.21459(14) -0.76871(14) 1.26470(14) 0.0195(5) Uani 1 1 d . . .
C20 C 1.29822(15) -0.73644(15) 1.32040(15) 0.0242(5) Uani 1 1 d . . .
C21 C 1.34020(17) -0.66630(15) 1.30586(16) 0.0270(6) Uani 1 1 d . . .
C22 C 1.29941(16) -0.62607(14) 1.23511(15) 0.0254(5) Uani 1 1 d . . .
C23 C 1.21471(15) -0.65453(14) 1.17829(15) 0.0215(5) Uani 1 1 d . . .
C24 C 1.17581(15) -0.72552(14) 1.19543(15) 0.0195(5) Uani 1 1 d . . .
C25 C 1.17042(15) -0.61005(15) 1.10149(15) 0.0229(5) Uani 1 1 d . . .
C26 C 1.06847(16) -0.62415(17) 1.06991(19) 0.0355(7) Uani 1 1 d . . .
C27 C 1.0195(4) -0.5923(3) 1.1280(3) 0.0330(12) Uani 0.50 1 d P . .
C27' C 1.0284(4) -0.5623(4) 1.0131(4) 0.0406(14) Uani 0.50 1 d P . .
C28 C 1.20659(15) -0.63554(14) 1.02353(15) 0.0209(5) Uani 1 1 d . . .
C29 C 1.26131(15) -0.57918(14) 1.00168(15) 0.0229(5) Uani 1 1 d . . .
C30 C 1.29084(16) -0.60180(14) 0.92754(15) 0.0227(5) Uani 1 1 d . . .
C31 C 1.26678(15) -0.68292(14) 0.87516(15) 0.0225(5) Uani 1 1 d . . .
C32 C 1.21402(14) -0.74154(14) 0.89669(14) 0.0202(5) Uani 1 1 d . . .
C33 C 1.18596(15) -0.71573(15) 0.97058(15) 0.0217(5) Uani 1 1 d . . .
C34 C 1.18734(15) -0.83058(14) 0.83968(16) 0.0217(5) Uani 1 1 d . . .
C35 C 1.08681(16) -0.84751(16) 0.80821(17) 0.0261(6) Uani 1 1 d . . .
C36 C 1.0411(2) -0.7839(2) 0.7503(2) 0.0391(7) Uani 1 1 d . . .
C37 C 1.45521(17) -0.40339(16) 0.97195(17) 0.0289(6) Uani 1 1 d . . .
C38 C 1.41351(18) -0.31860(16) 1.06794(17) 0.0306(6) Uani 1 1 d . . .
C39 C 1.46817(17) -0.27118(17) 1.04103(17) 0.0320(6) Uani 1 1 d . . .
C40 C 1.55619(18) -0.30579(17) 0.93178(19) 0.0297(6) Uani 1 1 d . . .
C41 C 1.52933(15) -0.23528(15) 0.87910(15) 0.0239(5) Uani 1 1 d . . .
C42 C 1.44314(17) -0.21297(17) 0.84940(18) 0.0316(6) Uani 1 1 d . . .
C43 C 1.42301(17) -0.14475(16) 0.80506(16) 0.0283(6) Uani 1 1 d . . .
C44 C 1.48850(15) -0.09843(14) 0.78812(14) 0.0218(5) Uani 1 1 d . . .
C45 C 1.57455(16) -0.12249(16) 0.81593(15) 0.0243(5) Uani 1 1 d . . .
C46 C 1.59508(17) -0.18980(15) 0.86114(15) 0.0242(5) Uani 1 1 d . . .
C47 C 1.46803(19) -0.02096(16) 0.74526(16) 0.0265(6) Uani 1 1 d . . .
C48 C 1.37594(16) -0.01073(15) 0.58959(16) 0.0243(5) Uani 1 1 d . . .
C49 C 1.44668(18) -0.08422(18) 0.51177(18) 0.0342(6) Uani 1 1 d . . .
C50 C 1.48913(17) -0.08782(17) 0.59785(16) 0.0317(6) Uani 1 1 d . . .
C51 C 1.2910(7) 0.4572(6) -0.3077(5) 0.037(2) Uani 0.50 1 d P . .
C51' C 1.3144(7) 0.4810(6) -0.2681(6) 0.042(2) Uani 0.50 1 d P . .
C52 C 1.4412(3) 0.46365(19) -0.22820(19) 0.0527(9) Uani 1 1 d . . .
C53 C 1.4297(3) 0.5349(2) -0.2657(2) 0.0586(10) Uani 1 1 d . . .
C54 C 1.3105(6) 0.6139(7) -0.3331(7) 0.044(2) Uani 0.50 1 d P . .
C54' C 1.2811(7) 0.5882(7) -0.3800(8) 0.054(2) Uani 0.50 1 d P . .
C55 C 1.3436(2) 0.6125(2) -0.4225(3) 0.0509(9) Uani 1 1 d . . .
C56 C 1.3420(9) 0.5450(10) -0.5068(8) 0.035(3) Uani 0.50 1 d P . .
C56' C 1.3279(13) 0.5537(12) -0.4779(9) 0.045(3) Uani 0.50 1 d P . .
C57 C 1.4050(6) 0.5560(8) -0.5509(10) 0.036(3) Uani 0.50 1 d P . .
C57' C 1.3650(9) 0.5503(8) -0.5472(10) 0.047(4) Uani 0.50 1 d P . .
C58 C 1.4467(2) 0.6229(2) -0.5331(2) 0.0512(9) Uani 1 1 d . . .
C59 C 1.44972(18) 0.68709(19) -0.46461(19) 0.0362(7) Uani 1 1 d . . .
C60 C 1.3984(2) 0.68127(19) -0.4103(2) 0.0452(8) Uani 1 1 d . . .
C61 C 1.5291(4) 0.6409(4) -0.5716(4) 0.0240(12) Uani 0.50 1 d P . .
C61' C 1.4822(6) 0.6027(5) -0.6078(5) 0.0540(19) Uani 0.50 1 d P . .
C62 C 1.4260(2) 0.7260(2) -0.6802(2) 0.0471(8) Uani 1 1 d . . .
C63 C 1.5302(2) 0.7993(2) -0.6973(2) 0.0449(8) Uani 1 1 d . . .
C64 C 1.5691(3) 0.7450(3) -0.6442(2) 0.0644(11) Uani 1 1 d . . .
C65 C 0.1435(2) 0.6524(2) 0.3647(3) 0.0567(10) Uani 1 1 d . . .
C66 C 0.1430(2) 0.6209(2) 0.2780(3) 0.0664(11) Uani 1 1 d . . .
C67 C 0.1729(2) 0.6721(2) 0.2314(2) 0.0572(9) Uani 1 1 d . . .
C68 C 0.20495(19) 0.75435(19) 0.2696(2) 0.0428(7) Uani 1 1 d . . .
C69 C 0.20581(17) 0.78671(18) 0.35609(18) 0.0338(6) Uani 1 1 d . . .
C70 C 0.17427(17) 0.73674(18) 0.40523(19) 0.0364(7) Uani 1 1 d . . .
C71 C 0.17353(18) 0.7671(2) 0.4977(2) 0.0454(8) Uani 1 1 d . . .
C72 C 0.16642(17) 0.85893(19) 0.53295(18) 0.0377(7) Uani 1 1 d . . .
C73 C 0.12765(19) 0.91702(19) 0.4795(2) 0.0414(7) Uani 1 1 d . . .
C74 C 0.1188(2) 1.0003(2) 0.5173(2) 0.0524(9) Uani 1 1 d . . .
C75 C 0.1474(2) 1.0265(3) 0.6079(2) 0.0566(9) Uani 1 1 d . . .
C76 C 0.1853(2) 0.9690(3) 0.6624(2) 0.0584(10) Uani 1 1 d . . .
C77 C 0.19485(19) 0.8866(3) 0.6256(2) 0.0511(9) Uani 1 1 d . . .
C81 C 1.1744(4) -0.6800(3) 1.4813(3) 0.0945(15) Uani 1 1 d . . .
C82 C 1.1257(7) -0.6457(3) 1.4147(4) 0.154(3) Uani 1 1 d . A .
C78 C 1.0083(4) -0.6816(4) 1.4442(4) 0.0451(15) Uani 0.529(3) 1 d P A 1
C79 C 1.0524(4) -0.7166(4) 1.5183(4) 0.0600(19) Uani 0.529(3) 1 d P A 1
C80 C 1.1468(4) -0.7219(5) 1.5370(5) 0.060(2) Uani 0.529(3) 1 d P A 1
C83 C 1.0584(3) -0.6459(4) 1.3977(4) 0.0274(14) Uani 0.529(3) 1 d P A 1
C84 C 1.0066(4) -0.6036(3) 1.3175(4) 0.0427(14) Uani 0.529(3) 1 d P A 1
C85 C 0.8952(4) -0.6202(5) 1.2865(5) 0.0514(18) Uani 0.529(3) 1 d P A 1
C86 C 0.8468(5) -0.5767(5) 1.2161(5) 0.059(2) Uani 0.529(3) 1 d P A 1
O10 O 1.0427(3) -0.5398(3) 1.3072(3) 0.0606(13) Uani 0.529(3) 1 d P A 1
C78' C 1.0231(4) -0.5824(5) 1.5256(4) 0.0514(19) Uani 0.471(3) 1 d P . 2
C79' C 1.0878(5) -0.6143(5) 1.5882(5) 0.060(2) Uani 0.471(3) 1 d P . 2
C80' C 1.1541(5) -0.6641(7) 1.5644(5) 0.068(3) Uani 0.471(3) 1 d P A 2
C83' C 1.0206(4) -0.5997(5) 1.4347(4) 0.0496(18) Uani 0.471(3) 1 d P A 2
C84' C 0.9477(4) -0.5640(4) 1.3702(5) 0.0514(18) Uani 0.471(3) 1 d P A 2
C85' C 0.9215(4) -0.6404(4) 1.2521(4) 0.0286(14) Uani 0.471(3) 1 d P A 2
C86' C 0.8782(5) -0.5892(4) 1.1884(5) 0.0373(17) Uani 0.471(3) 1 d P A 2
O10' O 0.9255(3) -0.4906(3) 1.3891(3) 0.0775(18) Uani 0.471(3) 1 d P . 2
C87 C 0.7968(2) -0.6238(2) 1.1303(3) 0.0705(11) Uani 1 1 d . . .
C88 C 0.7750(2) -0.7105(2) 1.1209(2) 0.0617(9) Uani 1 1 d . A .
C89 C 0.8202(2) -0.7564(2) 1.1869(2) 0.0591(9) Uani 1 1 d . . .
C90 C 0.8880(2) -0.7153(2) 1.2614(3) 0.0651(11) Uani 1 1 d . A .
N1 N 1.40578(14) -0.40182(12) 1.02516(13) 0.0291(5) Uani 1 1 d . . .
N2 N 1.49455(13) -0.32590(12) 0.97898(13) 0.0256(5) Uani 1 1 d . . .
N3 N 1.37526(13) -0.03480(13) 0.50671(13) 0.0276(5) Uani 1 1 d . . .
N4 N 1.44325(12) -0.04127(12) 0.64734(12) 0.0232(4) Uani 1 1 d . . .
N5 N 1.3600(2) 0.42244(16) -0.24323(18) 0.0575(8) Uani 1 1 d . . .
N6 N 1.3413(2) 0.53773(19) -0.3031(3) 0.0843(12) Uani 1 1 d . . .
N7 N 1.44054(14) 0.78780(13) -0.71979(13) 0.0312(5) Uani 1 1 d . . .
N8 N 1.5025(2) 0.6985(2) -0.63243(17) 0.0663(10) Uani 1 1 d . . .
H34A H 1.2026(14) -0.8292(14) 0.7855(15) 0.023(6) Uiso 1 1 d . . .
H16A H 1.1811(12) -0.8447(12) 1.3444(14) 0.007(5) Uiso 1 1 d . . .
H17B H 1.0505(14) -0.8706(14) 1.1715(15) 0.022(6) Uiso 1 1 d . . .
H17A H 1.0455(14) -0.8001(15) 1.2538(14) 0.019(6) Uiso 1 1 d . . .
H9A H 1.101(2) -1.210(2) 1.0142(19) 0.063(9) Uiso 1 1 d . . .
H6A H 1.1403(15) -0.9470(13) 0.9290(14) 0.019(6) Uiso 1 1 d . . .
H24A H 1.1196(14) -0.7493(13) 1.1585(14) 0.015(6) Uiso 1 1 d . . .
H30A H 1.3291(14) -0.5615(14) 0.9121(14) 0.018(6) Uiso 1 1 d . . .
H12A H 1.3508(14) -1.0703(14) 1.3216(14) 0.020(6) Uiso 1 1 d . . .
H25A H 1.1825(14) -0.5484(14) 1.1221(14) 0.020(6) Uiso 1 1 d . . .
H35A H 1.0650(14) -0.8476(13) 0.8637(15) 0.018(6) Uiso 1 1 d . . .
H47B H 1.4204(15) 0.0065(14) 0.7597(15) 0.021(6) Uiso 1 1 d . . .
H33A H 1.1523(14) -0.7586(14) 0.9879(14) 0.023(6) Uiso 1 1 d . . .
H43A H 1.3635(16) -0.1302(14) 0.7867(14) 0.022(6) Uiso 1 1 d . . .
H8B H 1.0741(15) -1.0273(15) 0.9938(15) 0.028(7) Uiso 1 1 d . . .
H35B H 1.0734(17) -0.9090(18) 0.7722(17) 0.045(8) Uiso 1 1 d . . .
H36A H 0.978(2) -0.7971(17) 0.7335(18) 0.046(8) Uiso 1 1 d . . .
H37A H 1.4668(15) -0.4545(15) 0.9308(15) 0.027(6) Uiso 1 1 d . . .
H8A H 1.0931(15) -1.1031(15) 0.9187(16) 0.026(6) Uiso 1 1 d . . .
H48A H 1.337(2) 0.0322(19) 0.6095(19) 0.061(9) Uiso 1 1 d . . .
H15A H 1.1518(15) -0.9288(14) 1.1161(15) 0.023(6) Uiso 1 1 d . . .
H9C H 1.0010(18) -1.1560(16) 0.9934(16) 0.037(7) Uiso 1 1 d . . .
H18C H 0.961(2) -0.9295(17) 1.2433(17) 0.047(8) Uiso 1 1 d . . .
H18B H 1.0337(17) -0.9003(17) 1.338(2) 0.043(8) Uiso 1 1 d . . .
H38A H 1.3801(17) -0.2989(16) 1.1073(17) 0.034(7) Uiso 1 1 d . . .
H7A H 1.2266(13) -1.1216(14) 1.0191(13) 0.013(5) Uiso 1 1 d . . .
H40A H 1.5575(15) -0.3617(15) 0.8895(15) 0.026(6) Uiso 1 1 d . . .
H3A H 1.4368(15) -0.9694(13) 0.9409(14) 0.019(6) Uiso 1 1 d . . .
H18A H 1.0502(18) -0.9754(19) 1.2640(18) 0.052(9) Uiso 1 1 d . . .
H46A H 1.6517(16) -0.2055(15) 0.8831(15) 0.028(7) Uiso 1 1 d . . .
H21A H 1.4031(17) -0.6486(15) 1.3415(16) 0.032(7) Uiso 1 1 d . . .
H45A H 1.6211(16) -0.0911(15) 0.8072(15) 0.032(7) Uiso 1 1 d . . .
H9B H 1.0761(16) -1.1302(16) 1.0860(18) 0.038(8) Uiso 1 1 d . . .
H50A H 1.5362(16) -0.1185(15) 0.6213(15) 0.029(7) Uiso 1 1 d . . .
H3 H 1.365(2) -1.162(2) 1.203(2) 0.077(11) Uiso 1 1 d . . .
H47A H 1.5171(16) 0.0224(15) 0.7641(15) 0.028(7) Uiso 1 1 d . . .
H1 H 1.3418(19) -0.8176(19) 0.8280(19) 0.056(9) Uiso 1 1 d . . .
H5 H 1.3162(19) -0.8210(19) 1.3977(19) 0.056(9) Uiso 1 1 d . . .
H69A H 0.2333(16) 0.8470(17) 0.3839(16) 0.039(7) Uiso 1 1 d . . .
H2 H 1.3659(17) -1.0998(17) 1.0586(18) 0.042(8) Uiso 1 1 d . . .
H4 H 1.318(2) -0.974(2) 1.431(2) 0.065(10) Uiso 1 1 d . . .
H73A H 0.1089(19) 0.9025(18) 0.414(2) 0.058(9) Uiso 1 1 d . . .
H65A H 0.1209(17) 0.6263(17) 0.4003(17) 0.036(8) Uiso 1 1 d . . .
H6 H 1.3268(18) -0.5372(17) 1.1773(18) 0.040(9) Uiso 1 1 d . . .
H36C H 1.0582(18) -0.7849(18) 0.694(2) 0.052(9) Uiso 1 1 d . . .
H8 H 1.322(3) -0.659(3) 0.787(3) 0.108(14) Uiso 1 1 d . . .
H36B H 1.0564(18) -0.7176(19) 0.7847(18) 0.053(8) Uiso 1 1 d . . .
H66A H 0.121(2) 0.562(2) 0.254(2) 0.076(11) Uiso 1 1 d . . .
H59A H 1.4920(19) 0.7377(18) -0.4517(18) 0.053(9) Uiso 1 1 d . . .
H40B H 1.6153(18) -0.2886(17) 0.9751(17) 0.042(8) Uiso 1 1 d . . .
H77A H 0.221(2) 0.840(2) 0.663(2) 0.067(10) Uiso 1 1 d . . .
H74A H 0.084(2) 1.039(2) 0.476(2) 0.073(10) Uiso 1 1 d . . .
H39A H 1.4898(18) -0.2113(19) 1.0572(18) 0.053(9) Uiso 1 1 d . . .
H67A H 0.166(2) 0.645(2) 0.160(2) 0.079(11) Uiso 1 1 d . . .
H62A H 1.364(2) 0.7000(19) -0.685(2) 0.066(10) Uiso 1 1 d . . .
H52A H 1.506(2) 0.437(2) -0.193(2) 0.076(11) Uiso 1 1 d . . .
H68A H 0.230(2) 0.791(2) 0.233(2) 0.076(11) Uiso 1 1 d . . .
H60A H 1.406(2) 0.731(2) -0.362(2) 0.070(10) Uiso 1 1 d . . .
H53A H 1.476(2) 0.578(2) -0.270(2) 0.062(10) Uiso 1 1 d . . .
H75A H 0.143(2) 1.090(2) 0.639(2) 0.073(10) Uiso 1 1 d . . .
H49A H 1.4640(17) -0.1065(17) 0.4604(18) 0.041(8) Uiso 1 1 d . . .
H57A H 1.386(4) 0.522(3) -0.587(4) 0.14(3) Uiso 1 1 d . . .
H64A H 1.636(2) 0.734(2) -0.616(2) 0.079(11) Uiso 1 1 d . . .
H42A H 1.3961(19) -0.2457(18) 0.8571(18) 0.053(9) Uiso 1 1 d . . .
H76A H 0.203(2) 0.986(2) 0.725(2) 0.077(11) Uiso 1 1 d . . .
H7 H 1.335(3) -0.468(3) 1.045(3) 0.113(15) Uiso 1 1 d . . .
H61B H 1.537(2) 0.580(2) -0.609(2) 0.067(10) Uiso 1 1 d . . .
H56A H 1.290(3) 0.497(3) -0.513(3) 0.094(13) Uiso 1 1 d . . .
H61A H 1.579(2) 0.662(2) -0.531(2) 0.086(12) Uiso 1 1 d . . .
H51A H 1.240(3) 0.454(3) -0.311(3) 0.111(19) Uiso 1 1 d . . .
H63A H 1.557(2) 0.843(2) -0.718(2) 0.094(14) Uiso 1 1 d . . .
H54A H 1.297(4) 0.648(3) -0.314(4) 0.13(3) Uiso 1 1 d . . .
H54B H 1.230(4) 0.565(4) -0.414(4) 0.19(3) Uiso 1 1 d . . .
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
C6 C1 C2 116.9(2) . .
C6 C1 C34 123.0(2) . .
C2 C1 C34 120.1(2) . .
O1 C2 C3 115.9(2) . .
O1 C2 C1 122.78(19) . .
C3 C2 C1 121.3(2) . .
C2 C3 C4 119.9(2) . .
O2 C4 C3 115.9(2) . .
O2 C4 C5 122.8(2) . .
C3 C4 C5 121.2(2) . .
C4 C5 C6 116.7(2) . .
C4 C5 C7 120.60(19) . .
C6 C5 C7 122.7(2) . .
C1 C6 C5 124.0(2) . .
C10 C7 C5 111.60(18) . .
C10 C7 C8 111.56(19) . .
C5 C7 C8 113.51(18) . .
C9 C8 C7 112.5(2) . .
C15 C10 C11 116.9(2) . .
C15 C10 C7 121.48(19) . .
C11 C10 C7 121.6(2) . .
O3 C11 C12 120.8(2) . .
O3 C11 C10 118.1(2) . .
C12 C11 C10 121.0(2) . .
C11 C12 C13 119.6(2) . .
O4 C13 C14 117.8(2) . .
O4 C13 C12 121.1(2) . .
C14 C13 C12 121.1(2) . .
C15 C14 C13 117.1(2) . .
C15 C14 C16 121.7(2) . .
C13 C14 C16 121.2(2) . .
C14 C15 C10 124.1(2) . .
C19 C16 C17 113.96(18) . .
C19 C16 C14 109.54(18) . .
C17 C16 C14 111.83(19) . .
C18 C17 C16 112.3(2) . .
C24 C19 C20 116.5(2) . .
C24 C19 C16 122.5(2) . .
C20 C19 C16 120.98(19) . .
C21 C20 O5 116.3(2) . .
C21 C20 C19 121.3(2) . .
O5 C20 C19 122.5(2) . .
C20 C21 C22 120.1(2) . .
O6 C22 C21 116.1(2) . .
O6 C22 C23 122.9(2) . .
C21 C22 C23 121.0(2) . .
C24 C23 C22 116.5(2) . .
C24 C23 C25 122.8(2) . .
C22 C23 C25 120.7(2) . .
C23 C24 C19 124.6(2) . .
C23 C25 C28 111.54(19) . .
C23 C25 C26 113.4(2) . .
C28 C25 C26 110.1(2) . .
C27 C26 C27' 88.6(3) . .
C27 C26 C25 119.9(3) . .
C27' C26 C25 110.6(3) . .
C26 C27 C27' 46.9(2) . .
C26 C27' C27 44.5(2) . .
C33 C28 C29 117.2(2) . .
C33 C28 C25 121.2(2) . .
C29 C28 C25 121.6(2) . .
O7 C29 C30 120.9(2) . .
O7 C29 C28 117.8(2) . .
C30 C29 C28 121.2(2) . .
C29 C30 C31 119.5(2) . .
O8 C31 C30 121.5(2) . .
O8 C31 C32 117.7(2) . .
C30 C31 C32 120.7(2) . .
C33 C32 C31 117.6(2) . .
C33 C32 C34 121.4(2) . .
C31 C32 C34 121.1(2) . .
C32 C33 C28 123.9(2) . .
C1 C34 C32 110.39(18) . .
C1 C34 C35 114.72(19) . .
C32 C34 C35 110.96(19) . .
C36 C35 C34 111.7(2) . .
N1 C37 N2 111.9(2) . .
C39 C38 N1 110.5(2) . .
C38 C39 N2 105.9(2) . .
N2 C40 C41 114.2(2) . .
C42 C41 C46 118.8(2) . .
C42 C41 C40 123.2(2) . .
C46 C41 C40 117.9(2) . .
C41 C42 C43 120.6(2) . .
C42 C43 C44 120.7(2) . .
C43 C44 C45 118.4(2) . .
C43 C44 C47 121.0(2) . .
C45 C44 C47 120.5(2) . .
C46 C45 C44 121.0(2) . .
C45 C46 C41 120.3(2) . .
N4 C47 C44 112.9(2) . .
N3 C48 N4 112.3(2) . .
C50 C49 N3 109.9(2) . .
C49 C50 N4 106.5(2) . .
C51' C51 N5 57.9(14) . .
C51' C51 N6 58.7(14) . .
N5 C51 N6 96.6(6) . .
C51 C51' N5 94.4(16) . .
C51 C51' N6 94.2(16) . .
N5 C51' N6 122.2(8) . .
C51 C51' C52 116.0(17) . .
N5 C51' C52 44.1(4) . .
N6 C51' C52 81.5(5) . .
C51 C51' C53 115.3(17) . .
N5 C51' C53 83.5(6) . .
N6 C51' C53 42.0(3) . .
C52 C51' C53 40.1(2) . .
C53 C52 N5 109.1(4) . .
C53 C52 C51' 71.5(4) . .
N5 C52 C51' 38.5(3) . .
N6 C53 C52 106.4(3) . .
N6 C53 C51' 38.8(3) . .
C52 C53 C51' 68.4(4) . .
C54' C54 N6 92.2(13) . .
C54' C54 C55 60.3(11) . .
N6 C54 C55 103.6(7) . .
C54 C54' C55 91.0(13) . .
C54 C54' N6 59.0(10) . .
C55 C54' N6 102.9(6) . .
C54 C54' C56' 122.4(15) . .
C55 C54' C56' 36.2(7) . .
N6 C54' C56' 102.4(7) . .
C56' C55 C60 129.1(8) . .
C56' C55 C54' 95.7(10) . .
C60 C55 C54' 135.1(6) . .
C56' C55 C56 16.1(10) . .
C60 C55 C56 113.0(5) . .
C54' C55 C56 111.8(7) . .
C56' C55 C54 120.5(9) . .
C60 C55 C54 109.6(5) . .
C54' C55 C54 28.7(4) . .
C56 C55 C54 136.1(6) . .
C56' C56 C57' 160(4) . .
C56' C56 C57 152(4) . .
C57' C56 C57 18.4(13) . .
C56' C56 C55 34(3) . .
C57' C56 C55 128.0(15) . .
C57 C56 C55 118.4(10) . .
C56 C56' C55 130(4) . .
C56 C56' C57' 12(2) . .
C55 C56' C57' 119.3(16) . .
C56 C56' C54' 178(4) . .
C55 C56' C54' 48.1(6) . .
C57' C56' C54' 165.9(15) . .
C56 C56' C57 20(3) . .
C55 C56' C57 110.2(13) . .
C57' C56' C57 13.7(9) . .
C54' C56' C57 158.1(13) . .
C57' C57 C58 125(2) . .
C57' C57 C56 24(2) . .
C58 C57 C56 118.7(12) . .
C57' C57 C56' 30(2) . .
C58 C57 C56' 111.3(11) . .
C56 C57 C56' 8.0(10) . .
C57' C57 C61' 150(3) . .
C58 C57 C61' 48.6(5) . .
C56 C57 C61' 164.4(11) . .
C56' C57 C61' 158.8(10) . .
C57 C57' C56 138(3) . .
C57 C57' C56' 136(3) . .
C56 C57' C56' 7.9(17) . .
C57 C57' C58 35.7(18) . .
C56 C57' C58 122.9(14) . .
C56' C57' C58 116.8(13) . .
C57 C58 C59 126.4(7) . .
C57 C58 C61' 93.5(8) . .
C59 C58 C61' 140.1(5) . .
C57 C58 C61 123.7(7) . .
C59 C58 C61 108.1(4) . .
C61' C58 C61 34.5(3) . .
C57 C58 C57' 18.9(7) . .
C59 C58 C57' 110.8(5) . .
C61' C58 C57' 108.2(7) . .
C61 C58 C57' 141.0(6) . .
C58 C59 C60 120.6(3) . .
C55 C60 C59 121.7(3) . .
C61' C61 N8 88.8(6) . .
C61' C61 C58 61.6(6) . .
N8 C61 C58 108.3(4) . .
C61 C61' C58 83.9(7) . .
C61 C61' N8 57.6(6) . .
C58 C61' N8 104.6(5) . .
C61 C61' C57 117.5(8) . .
C58 C61' C57 38.0(5) . .
N8 C61' C57 136.6(6) . .
N7 C62 N8 111.3(3) . .
C64 C63 N7 110.6(3) . .
C63 C64 N8 106.0(3) . .
C66 C65 C70 121.0(3) . .
C67 C66 C65 119.9(3) . .
C66 C67 C68 120.6(4) . .
C67 C68 C69 120.1(3) . .
C68 C69 C70 120.9(3) . .
C69 C70 C65 117.5(3) . .
C69 C70 C71 123.6(3) . .
C65 C70 C71 118.9(3) . .
O9 C71 C70 119.5(3) . .
O9 C71 C72 118.1(3) . .
C70 C71 C72 122.4(3) . .
C73 C72 C77 118.2(3) . .
C73 C72 C71 123.5(3) . .
C77 C72 C71 118.2(3) . .
C74 C73 C72 120.4(3) . .
C75 C74 C73 120.8(3) . .
C74 C75 C76 119.6(4) . .
C77 C76 C75 120.1(3) . .
C76 C77 C72 120.9(3) . .
C82 C81 C80 128.1(7) . .
C82 C81 C80' 118.1(6) . .
C80 C81 C80' 39.1(4) . .
C83 C82 C81 123.5(9) . .
C83 C82 C83' 29.7(5) . .
C81 C82 C83' 113.6(5) . .
C79 C78 C83 118.7(5) . .
C78 C79 C80 117.1(6) . .
C81 C80 C79 108.8(6) . .
C82 C83 C78 123.3(8) . .
C82 C83 C84 119.7(8) . .
C78 C83 C84 117.0(5) . .
O10 C84 C83 116.1(5) . .
O10 C84 C85 122.3(5) . .
C83 C84 C85 115.3(5) . .
C86 C85 C90 114.3(6) . .
C86 C85 C84 115.4(6) . .
C90 C85 C84 99.1(5) . .
C87 C86 C85 121.1(7) . .
C79' C78' C83' 120.0(7) . .
C79' C78' O10' 67.1(4) . 2_748
C83' C78' O10' 134.3(6) . 2_748
C78' C79' C80' 121.4(7) . .
C78' C79' O10' 63.8(5) . 2_748
C80' C79' O10' 134.8(7) . 2_748
C79' C80' C81 129.6(8) . .
C78' C83' C84' 117.0(6) . .
C78' C83' C82 114.4(5) . .
C84' C83' C82 127.2(6) . .
O10' C84' C83' 120.7(6) . .
O10' C84' C85' 129.6(6) . .
C83' C84' C85' 108.1(5) . .
C90 C85' C86' 125.2(6) . .
C90 C85' C84' 106.2(5) . .
C86' C85' C84' 105.3(5) . .
C87 C86' C85' 115.2(6) . .
C84' O10' C78' 127.1(6) . 2_748
C84' O10' C79' 169.9(6) . 2_748
C78' O10' C79' 49.1(4) 2_748 2_748
C88 C87 C86' 119.2(4) . .
C88 C87 C86 119.6(5) . .
C86' C87 C86 31.4(3) . .
C87 C88 C89 119.8(3) . .
C90 C89 C88 120.3(3) . .
C85' C90 C89 114.8(4) . .
C85' C90 C85 32.7(3) . .
C89 C90 C85 120.3(4) . .
C37 N1 C38 105.0(2) . .
C37 N2 C39 106.7(2) . .
C37 N2 C40 126.1(2) . .
C39 N2 C40 127.1(2) . .
C48 N3 C49 104.8(2) . .
C48 N4 C50 106.6(2) . .
C48 N4 C47 126.6(2) . .
C50 N4 C47 126.6(2) . .
C51' N5 C52 97.4(5) . .
C51' N5 C51 27.8(4) . .
C52 N5 C51 111.7(5) . .
C51' N6 C53 99.2(5) . .
C51' N6 C54 137.1(6) . .
C53 N6 C54 117.4(5) . .
C51' N6 C51 27.1(4) . .
C53 N6 C51 113.1(5) . .
C54 N6 C51 129.4(6) . .
C51' N6 C54' 127.2(7) . .
C53 N6 C54' 133.3(4) . .
C54 N6 C54' 28.8(4) . .
C51 N6 C54' 107.7(6) . .
C62 N7 C63 105.2(3) . .
C62 N8 C64 106.9(3) . .
C62 N8 C61 137.4(4) . .
C64 N8 C61 115.6(4) . .
C62 N8 C61' 109.2(4) . .
C64 N8 C61' 140.1(3) . .
C61 N8 C61' 33.7(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 C2 1.378(3) .
O2 C4 1.373(2) .
O3 C11 1.371(3) .
O4 C13 1.373(3) .
O5 C20 1.383(3) .
O6 C22 1.379(3) .
O7 C29 1.373(3) .
O8 C31 1.370(3) .
O9 C71 1.224(3) .
C1 C6 1.386(3) .
C1 C2 1.393(3) .
C1 C34 1.523(3) .
C2 C3 1.385(3) .
C3 C4 1.386(3) .
C4 C5 1.393(3) .
C5 C6 1.396(3) .
C5 C7 1.521(3) .
C7 C10 1.519(3) .
C7 C8 1.529(3) .
C8 C9 1.523(3) .
C10 C15 1.387(3) .
C10 C11 1.396(3) .
C11 C12 1.392(3) .
C12 C13 1.394(3) .
C13 C14 1.390(3) .
C14 C15 1.386(3) .
C14 C16 1.526(3) .
C16 C19 1.520(3) .
C16 C17 1.524(3) .
C17 C18 1.517(3) .
C19 C24 1.392(3) .
C19 C20 1.398(3) .
C20 C21 1.380(3) .
C21 C22 1.387(3) .
C22 C23 1.402(3) .
C23 C24 1.386(3) .
C23 C25 1.514(3) .
C25 C28 1.517(3) .
C25 C26 1.549(3) .
C26 C27 1.413(6) .
C26 C27' 1.472(5) .
C27 C27' 2.015(7) .
C28 C33 1.384(3) .
C28 C29 1.396(3) .
C29 C30 1.393(3) .
C30 C31 1.396(3) .
C31 C32 1.397(3) .
C32 C33 1.383(3) .
C32 C34 1.530(3) .
C34 C35 1.531(3) .
C35 C36 1.530(4) .
C37 N1 1.314(3) .
C37 N2 1.348(3) .
C38 C39 1.350(4) .
C38 N1 1.370(3) .
C39 N2 1.371(3) .
C40 N2 1.463(3) .
C40 C41 1.504(3) .
C41 C42 1.381(3) .
C41 C46 1.388(3) .
C42 C43 1.383(3) .
C43 C44 1.384(3) .
C44 C45 1.386(3) .
C44 C47 1.501(3) .
C45 C46 1.379(3) .
C47 N4 1.473(3) .
C48 N3 1.312(3) .
C48 N4 1.345(3) .
C49 C50 1.352(3) .
C49 N3 1.377(3) .
C50 N4 1.363(3) .
C51 C51' 0.678(8) .
C51 N5 1.450(10) .
C51 N6 1.483(10) .
C51' N5 1.231(10) .
C51' N6 1.271(10) .
C51' C52 1.961(11) .
C51' C53 2.001(11) .
C52 C53 1.358(4) .
C52 N5 1.377(4) .
C53 N6 1.357(5) .
C54 C54' 0.796(10) .
C54 N6 1.416(9) .
C54 C55 1.658(10) .
C54' C55 1.440(10) .
C54' N6 1.650(9) .
C54' C56' 1.925(16) .
C55 C56' 1.143(17) .
C55 C60 1.342(4) .
C55 C56 1.568(14) .
C56 C56' 0.567(16) .
C56 C57' 0.846(15) .
C56 C57 1.408(15) .
C56' C57' 1.393(15) .
C56' C57 1.927(19) .
C57 C57' 0.662(14) .
C57 C58 1.193(12) .
C57 C61' 1.936(15) .
C57' C58 1.666(15) .
C58 C59 1.355(4) .
C58 C61' 1.454(8) .
C58 C61 1.644(7) .
C59 C60 1.367(4) .
C61 C61' 0.936(9) .
C61 N8 1.424(6) .
C61' N8 1.687(8) .
C62 N7 1.307(3) .
C62 N8 1.350(4) .
C63 C64 1.339(4) .
C63 N7 1.363(4) .
C64 N8 1.359(5) .
C65 C66 1.388(5) .
C65 C70 1.402(4) .
C66 C67 1.358(5) .
C67 C68 1.371(4) .
C68 C69 1.387(4) .
C69 C70 1.390(4) .
C70 C71 1.478(4) .
C71 C72 1.493(4) .
C72 C73 1.388(4) .
C72 C77 1.403(4) .
C73 C74 1.387(4) .
C74 C75 1.371(4) .
C75 C76 1.387(5) .
C76 C77 1.374(5) .
C81 C82 1.322(7) .
C81 C80 1.361(9) .
C81 C80' 1.440(9) .
C82 C83 1.021(10) .
C82 C83' 1.919(11) .
C78 C79 1.394(8) .
C78 C83 1.410(8) .
C79 C80 1.445(9) .
C83 C84 1.565(8) .
C84 O10 1.220(6) .
C84 C85 1.695(9) .
C85 C86 1.448(10) .
C85 C90 1.492(8) .
C86 C87 1.437(8) .
C78' C79' 1.374(9) .
C78' C83' 1.419(9) .
C78' O10' 1.632(8) 2_748
C79' C80' 1.427(10) .
C79' O10' 1.676(9) 2_748
C83' C84' 1.494(9) .
C84' O10' 1.237(7) .
C84' C85' 1.991(9) .
C85' C90 1.349(7) .
C85' C86' 1.430(9) .
C86' C87 1.392(8) .
O10' C78' 1.632(8) 2_748
O10' C79' 1.676(9) 2_748
C87 C88 1.391(5) .
C88 C89 1.408(5) .
C89 C90 1.404(5) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O8 0.91(3) 1.91(3) 2.811(2) 170(3) .
O2 H2 O3 0.89(3) 1.98(3) 2.850(2) 166(3) .
O3 H3 N7 0.92(3) 1.75(3) 2.663(3) 169(3) 1_537
O4 H4 N3 0.92(3) 1.72(3) 2.633(2) 173(3) 1_546
O5 H5 O4 0.91(3) 1.89(3) 2.778(2) 163(3) .
O6 H6 O7 0.85(3) 2.00(3) 2.837(2) 171(3) .
O7 H7 N1 1.01(4) 1.66(4) 2.661(3) 173(4) .
O8 H8 N5 1.00(4) 1.63(4) 2.625(3) 179(4) 1_546
