# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
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data_q6_glyphe2
_database_code_depnum_ccdc_archive 'CCDC 1548093'
_audit_update_record             
;
2017-05-05 deposited with the CCDC.
2017-06-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            'cucurbit[6]uril/Gly-Phe exclusion complex'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C47 H50 N26 O30'
_chemical_formula_weight         1459.13

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'
O O 0.0106 0.0060 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   12.8276(3)
_cell_length_b                   15.6361(4)
_cell_length_c                   16.4483(4)
_cell_angle_alpha                90
_cell_angle_beta                 105.3839(10)
_cell_angle_gamma                90
_cell_volume                     3180.91(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6823
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      27.1

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_F_000             1508
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.129
_shelx_estimated_absorpt_T_min   0.950
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  KappaApexII
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            47337
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_av_R_equivalents  0.063
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_theta_min         2.569
_diffrn_reflns_theta_max         28.277
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             15276
_reflns_number_gt                13884
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.885
_reflns_Friedel_fraction_max     0.944
_reflns_Friedel_fraction_full    0.980

_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
'Collect data collection software (Nonius B.V., 1998)'
_computing_cell_refinement       'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_data_reduction        'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0965P)²+9.3731P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 5940 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.0(5)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         15276
_refine_ls_number_parameters     929
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0827
_refine_ls_wR_factor_ref         0.2127
_refine_ls_wR_factor_gt          0.2047
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O4 O 0.4046(4) 0.5589(3) 0.8202(3) 0.0201(9) Uani 1 1 d . . . . .
O8 O 1.0764(3) 0.6858(3) 1.0945(3) 0.0177(8) Uani 1 1 d . . . . .
O2 O 0.8151(3) 0.3783(3) 0.9375(3) 0.0190(8) Uani 1 1 d . . . . .
O3 O 0.5724(4) 0.4457(3) 0.9775(3) 0.0187(8) Uani 1 1 d . . . . .
O10 O 0.6431(4) 0.8912(3) 0.9636(3) 0.0191(8) Uani 1 1 d . . . . .
O7 O 1.1760(3) 0.7118(3) 0.9276(3) 0.0195(8) Uani 1 1 d . . . . .
O9 O 0.8099(4) 0.7782(3) 1.1245(3) 0.0181(8) Uani 1 1 d . . . . .
O6 O 0.7530(4) 0.5159(3) 0.6164(3) 0.0240(9) Uani 1 1 d . . . . .
N17 N 0.8028(4) 0.6306(3) 1.1368(3) 0.0140(9) Uani 1 1 d . . . . .
N14 N 1.1688(4) 0.5639(3) 0.9352(3) 0.0163(9) Uani 1 1 d . . . . .
N15 N 1.0984(4) 0.5457(3) 1.0588(3) 0.0161(9) Uani 1 1 d . . . . .
O11 O 0.7226(4) 0.9302(3) 0.7958(3) 0.0226(9) Uani 1 1 d . . . . .
N9 N 0.4810(4) 0.7304(3) 0.6831(3) 0.0183(10) Uani 1 1 d . . . . .
O1 O 0.9064(4) 0.4044(3) 0.7629(3) 0.0211(9) Uani 1 1 d . . . . .
N3 N 0.9911(4) 0.4232(3) 0.9939(3) 0.0165(9) Uani 1 1 d . . . . .
N8 N 0.4106(4) 0.7056(3) 0.8036(3) 0.0175(10) Uani 1 1 d . . . . .
N6 N 0.5571(4) 0.5764(3) 1.0407(3) 0.0150(9) Uani 1 1 d . . . . .
N5 N 0.7034(4) 0.4959(3) 1.0932(3) 0.0150(9) Uani 1 1 d . . . . .
C16 C 0.9718(5) 0.4813(3) 1.1199(3) 0.0139(10) Uani 1 1 d . . . . .
H16 H 0.9902 0.4527 1.1763 0.017 Uiso 1 1 calc R U . . .
N21 N 0.5541(4) 0.8720(3) 0.7347(3) 0.0196(10) Uani 1 1 d . . . . .
N7 N 0.4244(4) 0.6533(3) 0.9320(3) 0.0156(9) Uani 1 1 d . . . . .
N1 N 1.0358(4) 0.4981(3) 0.7423(3) 0.0191(10) Uani 1 1 d . . . . .
N20 N 0.4946(4) 0.8413(3) 0.8611(3) 0.0185(10) Uani 1 1 d . . . . .
C2X C 0.5489(5) 0.4138(4) 0.7380(4) 0.0210(12) Uani 1 1 d . . . . .
N18 N 0.6492(4) 0.7057(3) 1.1090(3) 0.0143(9) Uani 1 1 d . . . . .
O3X O 0.2173(4) 0.3784(4) 0.5393(3) 0.0347(12) Uani 1 1 d . . . . .
O2X O 0.2490(4) 0.4857(3) 0.6343(3) 0.0305(11) Uani 1 1 d . . . . .
N12 N 0.9164(4) 0.5845(3) 0.6321(3) 0.0170(9) Uani 1 1 d . . . . .
N23 N 0.8592(4) 0.7842(3) 0.6631(3) 0.0195(10) Uani 1 1 d . . . . .
N2 N 1.0556(4) 0.4433(3) 0.8696(3) 0.0159(9) Uani 1 1 d . . . . .
N24 N 1.0133(4) 0.7105(3) 0.7014(3) 0.0183(10) Uani 1 1 d . . . . .
C30 C 0.5769(4) 0.7772(3) 1.0778(3) 0.0143(10) Uani 1 1 d . . . . .
H30A H 0.5146 0.7741 1.1027 0.017 Uiso 1 1 calc R U . . .
H30B H 0.6157 0.8314 1.0967 0.017 Uiso 1 1 calc R U . . .
N16 N 0.9752(4) 0.5744(3) 1.1273(3) 0.0141(9) Uani 1 1 d . . . . .
C9 C 0.5289(5) 0.6729(4) 0.6427(4) 0.0180(11) Uani 1 1 d . . . . .
N10 N 0.5962(4) 0.7163(3) 0.6050(3) 0.0188(10) Uani 1 1 d . . . . .
O12 O 0.9835(4) 0.8165(3) 0.7903(3) 0.0236(9) Uani 1 1 d . . . . .
N13 N 1.1359(4) 0.6240(3) 0.8091(3) 0.0190(10) Uani 1 1 d . . . . .
C6 C 0.4446(5) 0.5903(4) 0.9993(4) 0.0174(11) Uani 1 1 d . . . . .
H6A H 0.4074 0.6089 1.0419 0.021 Uiso 1 1 calc R U . . .
H6B H 0.4120 0.5353 0.9756 0.021 Uiso 1 1 calc R U . . .
O1X O 0.5979(4) 0.3484(3) 0.7267(3) 0.0336(11) Uani 1 1 d . . . . .
C22 C 0.5937(5) 0.8071(4) 0.6183(4) 0.0165(11) Uani 1 1 d . . . . .
H22 H 0.5777 0.8394 0.5639 0.020 Uiso 1 1 calc R U . . .
C24 C 0.9564(5) 0.6706(4) 0.6231(4) 0.0174(11) Uani 1 1 d . . . . .
H24 H 0.9995 0.6724 0.5806 0.021 Uiso 1 1 calc R U . . .
C34 C 0.7909(5) 0.8583(4) 0.6580(4) 0.0179(11) Uani 1 1 d . . . . .
H34A H 0.7741 0.8815 0.6000 0.021 Uiso 1 1 calc R U . . .
H34B H 0.8311 0.9028 0.6967 0.021 Uiso 1 1 calc R U . . .
C29 C 0.7590(4) 0.7122(3) 1.1233(3) 0.0120(10) Uani 1 1 d . . . . .
C21 C 0.5027(5) 0.8186(4) 0.6636(4) 0.0163(11) Uani 1 1 d . . . . .
H21 H 0.4373 0.8467 0.6262 0.020 Uiso 1 1 calc R U . . .
C19 C 0.4302(5) 0.7445(3) 0.9456(4) 0.0143(10) Uani 1 1 d . . . . .
H19 H 0.3751 0.7644 0.9745 0.017 Uiso 1 1 calc R U . . .
N22 N 0.6897(4) 0.8408(3) 0.6795(3) 0.0199(10) Uani 1 1 d . . . . .
C28 C 0.9176(5) 0.6207(4) 1.1771(3) 0.0154(10) Uani 1 1 d . . . . .
H28A H 0.9505 0.6781 1.1897 0.018 Uiso 1 1 calc R U . . .
H28B H 0.9265 0.5905 1.2314 0.018 Uiso 1 1 calc R U . . .
O5 O 0.5136(4) 0.5951(3) 0.6398(3) 0.0271(10) Uani 1 1 d . . . . .
N4 N 0.8711(4) 0.4491(3) 1.0651(3) 0.0150(9) Uani 1 1 d . . . . .
C35 C 0.9534(5) 0.7745(4) 0.7246(4) 0.0184(11) Uani 1 1 d . . . . .
C15 C 1.0563(5) 0.4616(3) 1.0703(4) 0.0150(10) Uani 1 1 d . . . . .
H15 H 1.1143 0.4220 1.1020 0.018 Uiso 1 1 calc R U . . .
C27 C 1.0514(5) 0.6088(3) 1.0930(4) 0.0141(10) Uani 1 1 d . . . . .
C23 C 0.8500(5) 0.7233(4) 0.5937(4) 0.0176(11) Uani 1 1 d . . . . .
H23 H 0.8437 0.7527 0.5386 0.021 Uiso 1 1 calc R U . . .
N19 N 0.5371(4) 0.7779(3) 0.9865(3) 0.0149(9) Uani 1 1 d . . . . .
C11 C 0.8079(5) 0.5805(4) 0.6135(4) 0.0202(12) Uani 1 1 d . . . . .
C5 C 0.6077(5) 0.5006(4) 1.0309(4) 0.0152(10) Uani 1 1 d . . . . .
C4X C 0.2708(5) 0.4159(5) 0.6054(4) 0.0248(13) Uani 1 1 d . . . . .
C36 C 1.1240(5) 0.6917(4) 0.7468(4) 0.0190(11) Uani 1 1 d . . . . .
H36A H 1.1576 0.7444 0.7756 0.023 Uiso 1 1 calc R U . . .
H36B H 1.1645 0.6754 0.7056 0.023 Uiso 1 1 calc R U . . .
C18 C 0.6134(5) 0.6195(3) 1.1186(3) 0.0135(10) Uani 1 1 d . . . . .
H18 H 0.5707 0.6169 1.1613 0.016 Uiso 1 1 calc R U . . .
C25 C 1.1607(5) 0.6411(3) 0.8943(4) 0.0156(10) Uani 1 1 d . . . . .
C31 C 0.5671(5) 0.8423(4) 0.9402(4) 0.0153(10) Uani 1 1 d . . . . .
C8 C 0.3877(5) 0.7071(4) 0.7129(4) 0.0187(11) Uani 1 1 d . . . . .
H8A H 0.3287 0.7485 0.6903 0.022 Uiso 1 1 calc R U . . .
H8B H 0.3619 0.6499 0.6906 0.022 Uiso 1 1 calc R U . . .
C32 C 0.4985(5) 0.9030(4) 0.7956(4) 0.0181(11) Uani 1 1 d . . . . .
H32A H 0.5355 0.9554 0.8227 0.022 Uiso 1 1 calc R U . . .
H32B H 0.4237 0.9190 0.7652 0.022 Uiso 1 1 calc R U . . .
C17 C 0.7214(4) 0.5689(3) 1.1487(4) 0.0143(10) Uani 1 1 d . . . . .
H17 H 0.7354 0.5513 1.2091 0.017 Uiso 1 1 calc R U . . .
C3 C 0.8855(5) 0.4127(3) 0.9926(4) 0.0156(10) Uani 1 1 d . . . . .
C14 C 1.1554(5) 0.4908(4) 0.8787(4) 0.0165(11) Uani 1 1 d . . . . .
H14 H 1.2201 0.4526 0.8926 0.020 Uiso 1 1 calc R U . . .
C4 C 0.7804(5) 0.4264(3) 1.0975(4) 0.0152(10) Uani 1 1 d . . . . .
H4A H 0.8080 0.4082 1.1570 0.018 Uiso 1 1 calc R U . . .
H4B H 0.7422 0.3771 1.0651 0.018 Uiso 1 1 calc R U . . .
C26 C 1.1921(4) 0.5581(4) 1.0265(4) 0.0159(11) Uani 1 1 d . . . . .
H26A H 1.2428 0.5101 1.0459 0.019 Uiso 1 1 calc R U . . .
H26B H 1.2292 0.6113 1.0513 0.019 Uiso 1 1 calc R U . . .
N11 N 0.7655(4) 0.6603(3) 0.5883(3) 0.0193(10) Uani 1 1 d . . . . .
C1 C 0.9914(5) 0.4445(4) 0.7897(4) 0.0190(11) Uani 1 1 d . . . . .
N1X N 0.7265(5) 0.4832(4) 0.7914(4) 0.0299(12) Uani 1 1 d . . . . .
H1X1 H 0.7284 0.4953 0.7377 0.045 Uiso 1 1 calc R U . . .
H1X2 H 0.7567 0.4309 0.8065 0.045 Uiso 1 1 calc R U . . .
H1X3 H 0.7644 0.5237 0.8270 0.045 Uiso 1 1 calc R U . . .
C7 C 0.4139(4) 0.6316(4) 0.8486(4) 0.0146(10) Uani 1 1 d . . . . .
C33 C 0.6613(5) 0.8848(4) 0.7430(4) 0.0164(11) Uani 1 1 d . . . . .
C3X C 0.3715(6) 0.3676(4) 0.6570(4) 0.0226(12) Uani 1 1 d . . . . .
H3X H 0.4075 0.3383 0.6177 0.027 Uiso 1 1 calc R U . . .
N2X N 0.4460(4) 0.4287(4) 0.7084(3) 0.0226(11) Uani 1 1 d . . . . .
H2X H 0.4203 0.4780 0.7200 0.027 Uiso 1 1 calc R U . . .
C13 C 1.1382(5) 0.5335(4) 0.7907(4) 0.0162(11) Uani 1 1 d . . . . .
H13 H 1.1983 0.5192 0.7647 0.019 Uiso 1 1 calc R U . . .
C1X C 0.6136(5) 0.4827(5) 0.7963(4) 0.0248(13) Uani 1 1 d . . . . .
H1X H 0.5806 0.5395 0.7796 0.030 Uiso 1 1 calc R U . . .
H2X2 H 0.6116 0.4714 0.8551 0.030 Uiso 1 1 calc R U . . .
C12 C 0.9878(5) 0.5103(4) 0.6533(4) 0.0182(11) Uani 1 1 d . . . . .
H12A H 0.9461 0.4584 0.6305 0.022 Uiso 1 1 calc R U . . .
H12B H 1.0465 0.5164 0.6249 0.022 Uiso 1 1 calc R U . . .
C2 C 1.0393(5) 0.3837(3) 0.9328(3) 0.0147(10) Uani 1 1 d . . . . .
H2A H 0.9920 0.3366 0.9042 0.018 Uiso 1 1 calc R U . . .
H2B H 1.1098 0.3586 0.9628 0.018 Uiso 1 1 calc R U . . .
C20 C 0.4082(5) 0.7821(4) 0.8544(4) 0.0151(10) Uani 1 1 d . . . . .
H20 H 0.3363 0.8112 0.8369 0.018 Uiso 1 1 calc R U . . .
C10 C 0.6522(5) 0.6763(4) 0.5501(4) 0.0161(11) Uani 1 1 d . . . . .
H10A H 0.6453 0.7132 0.5000 0.019 Uiso 1 1 calc R U . . .
H10B H 0.6163 0.6212 0.5302 0.019 Uiso 1 1 calc R U . . .
C5X C 0.3403(7) 0.3004(5) 0.7155(4) 0.0315(15) Uani 1 1 d . . . . .
H5X1 H 0.4072 0.2801 0.7562 0.038 Uiso 1 1 calc R U . . .
H5X2 H 0.2954 0.3287 0.7482 0.038 Uiso 1 1 calc R U . . .
C6X C 0.2799(7) 0.2244(6) 0.6714(4) 0.0383(19) Uani 1 1 d . . . . .
C7X C 0.1692(8) 0.2236(9) 0.6465(6) 0.061(3) Uani 1 1 d . . . . .
H7X H 0.1292 0.2715 0.6573 0.073 Uiso 1 1 calc R U . . .
C8X C 0.1143(11) 0.1496(9) 0.6040(6) 0.067(4) Uani 1 1 d . . . . .
H8X H 0.0375 0.1481 0.5866 0.081 Uiso 1 1 calc R U . . .
C9X C 0.1727(14) 0.0814(11) 0.5887(7) 0.085(5) Uani 1 1 d . . . . .
H9X H 0.1356 0.0333 0.5595 0.102 Uiso 1 1 calc R U . . .
C10X C 0.2845(13) 0.0804(7) 0.6144(6) 0.070(4) Uani 1 1 d . . . . .
H10X H 0.3243 0.0320 0.6046 0.084 Uiso 1 1 calc R U . . .
C11X C 0.3373(9) 0.1536(6) 0.6555(5) 0.046(2) Uani 1 1 d . . . . .
H11X H 0.4141 0.1547 0.6729 0.055 Uiso 1 1 calc R U . . .
O1W O 0.9421(4) 0.7377(3) 0.9311(3) 0.0312(11) Uani 1 1 d . . . . .
O2W O 0.6689(4) 0.2401(3) 0.8686(3) 0.0283(10) Uani 1 1 d . . . . .
O3W O 0.6117(5) 1.0886(4) 0.7853(3) 0.0365(12) Uani 1 1 d . . . . .
O4W O 0.4939(5) 0.4735(3) 0.5094(4) 0.0387(13) Uani 1 1 d . . . . .
O5W O 0.7866(4) 0.3909(3) 1.3010(4) 0.0345(12) Uani 1 1 d . . . . .
O6W O 0.1598(5) 0.6168(4) 0.5347(4) 0.0418(13) Uani 1 1 d . . . . .
O7W O 0.6196(5) 1.0787(4) 0.6169(4) 0.0446(14) Uani 1 1 d . . . . .
O8W O 1.1593(5) 0.5951(4) 1.3645(4) 0.0443(14) Uani 1 1 d . . . . .
O9W O 1.0005(5) 0.9707(4) 0.6691(4) 0.0403(13) Uani 1 1 d . . . . .
O10W O 0.5738(5) 0.2529(4) 0.5806(4) 0.0408(13) Uani 1 1 d . . . . .
O11W O 0.8404(6) 0.2352(4) 0.7327(4) 0.0437(14) Uani 1 1 d . . . . .
O12W O 0.0027(5) 0.4062(4) 0.4848(4) 0.0429(14) Uani 1 1 d . . . . .
O13W O 0.6884(5) 0.3708(4) 0.5198(4) 0.0448(14) Uani 1 1 d . . . . .
O14W O 0.1704(5) 0.7888(4) 0.5567(4) 0.0432(14) Uani 1 1 d . . . . .
O15W O 0.8044(7) 0.6040(5) 0.9180(5) 0.063(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
O4 C7 1.223(7) . ?
O8 C27 1.244(7) . ?
O2 C3 1.222(7) . ?
O3 C5 1.226(7) . ?
O10 C31 1.218(7) . ?
O7 C25 1.226(7) . ?
O9 C29 1.219(7) . ?
O6 C11 1.240(8) . ?
N17 C29 1.387(7) . ?
N17 C28 1.455(8) . ?
N17 C17 1.472(7) . ?
N14 C25 1.373(7) . ?
N14 C26 1.454(7) . ?
N14 C14 1.455(7) . ?
N15 C27 1.355(7) . ?
N15 C26 1.449(7) . ?
N15 C15 1.454(7) . ?
O11 C33 1.230(7) . ?
N9 C9 1.359(8) . ?
N9 C8 1.455(8) . ?
N9 C21 1.460(7) . ?
O1 C1 1.234(8) . ?
N3 C3 1.359(8) . ?
N3 C15 1.443(7) . ?
N3 C2 1.451(7) . ?
N8 C7 1.369(7) . ?
N8 C8 1.441(7) . ?
N8 C20 1.465(7) . ?
N6 C5 1.381(7) . ?
N6 C6 1.440(8) . ?
N6 C18 1.458(7) . ?
N5 C5 1.378(8) . ?
N5 C17 1.442(7) . ?
N5 C4 1.456(7) . ?
C16 N4 1.454(7) . ?
C16 N16 1.461(7) . ?
C16 C15 1.550(8) . ?
C16 H16 1.0000 . ?
N21 C33 1.361(8) . ?
N21 C21 1.446(7) . ?
N21 C32 1.458(8) . ?
N7 C7 1.384(7) . ?
N7 C19 1.443(7) . ?
N7 C6 1.452(7) . ?
N1 C1 1.369(8) . ?
N1 C12 1.442(7) . ?
N1 C13 1.453(8) . ?
N20 C31 1.384(8) . ?
N20 C20 1.426(8) . ?
N20 C32 1.457(7) . ?
C2X O1X 1.239(8) . ?
C2X N2X 1.301(9) . ?
C2X C1X 1.532(9) . ?
N18 C29 1.368(7) . ?
N18 C18 1.446(7) . ?
N18 C30 1.456(7) . ?
O3X C4X 1.265(8) . ?
O2X C4X 1.251(9) . ?
N12 C11 1.345(8) . ?
N12 C12 1.462(7) . ?
N12 C24 1.463(8) . ?
N23 C35 1.364(8) . ?
N23 C34 1.441(8) . ?
N23 C23 1.467(7) . ?
N2 C1 1.354(8) . ?
N2 C2 1.451(7) . ?
N2 C14 1.453(8) . ?
N24 C35 1.375(8) . ?
N24 C24 1.443(8) . ?
N24 C36 1.450(8) . ?
C30 N19 1.453(7) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
N16 C27 1.363(7) . ?
N16 C28 1.436(7) . ?
C9 O5 1.231(8) . ?
C9 N10 1.368(8) . ?
N10 C22 1.439(8) . ?
N10 C10 1.439(7) . ?
O12 C35 1.235(8) . ?
N13 C25 1.378(8) . ?
N13 C13 1.449(7) . ?
N13 C36 1.452(8) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C22 N22 1.465(8) . ?
C22 C21 1.553(8) . ?
C22 H22 1.0000 . ?
C24 C23 1.557(8) . ?
C24 H24 1.0000 . ?
C34 N22 1.458(8) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C21 H21 1.0000 . ?
C19 N19 1.455(8) . ?
C19 C20 1.565(8) . ?
C19 H19 1.0000 . ?
N22 C33 1.379(8) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
N4 C3 1.377(7) . ?
N4 C4 1.447(7) . ?
C15 H15 1.0000 . ?
C23 N11 1.451(8) . ?
C23 H23 1.0000 . ?
N19 C31 1.377(7) . ?
C11 N11 1.379(8) . ?
C4X C3X 1.542(10) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C18 C17 1.557(8) . ?
C18 H18 1.0000 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C17 H17 1.0000 . ?
C14 C13 1.555(8) . ?
C14 H14 1.0000 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
N11 C10 1.445(8) . ?
N1X C1X 1.471(9) . ?
N1X H1X1 0.9100 . ?
N1X H1X2 0.9100 . ?
N1X H1X3 0.9100 . ?
C3X N2X 1.452(8) . ?
C3X C5X 1.546(9) . ?
C3X H3X 1.0000 . ?
N2X H2X 0.8800 . ?
C13 H13 1.0000 . ?
C1X H1X 0.9900 . ?
C1X H2X2 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C20 H20 1.0000 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C5X C6X 1.497(11) . ?
C5X H5X1 0.9900 . ?
C5X H5X2 0.9900 . ?
C6X C7X 1.369(13) . ?
C6X C11X 1.392(14) . ?
C7X C8X 1.437(17) . ?
C7X H7X 0.9500 . ?
C8X C9X 1.36(2) . ?
C8X H8X 0.9500 . ?
C9X C10X 1.38(2) . ?
C9X H9X 0.9500 . ?
C10X C11X 1.408(13) . ?
C10X H10X 0.9500 . ?
C11X H11X 0.9500 . ?

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
C29 N17 C28 119.3(5) . . ?
C29 N17 C17 110.6(4) . . ?
C28 N17 C17 122.5(5) . . ?
C25 N14 C26 122.0(5) . . ?
C25 N14 C14 113.3(5) . . ?
C26 N14 C14 124.7(5) . . ?
C27 N15 C26 123.9(5) . . ?
C27 N15 C15 112.5(5) . . ?
C26 N15 C15 122.9(5) . . ?
C9 N9 C8 121.2(5) . . ?
C9 N9 C21 112.3(5) . . ?
C8 N9 C21 122.2(5) . . ?
C3 N3 C15 114.2(5) . . ?
C3 N3 C2 122.9(5) . . ?
C15 N3 C2 121.7(5) . . ?
C7 N8 C8 122.9(5) . . ?
C7 N8 C20 112.6(5) . . ?
C8 N8 C20 123.2(5) . . ?
C5 N6 C6 121.2(5) . . ?
C5 N6 C18 111.2(5) . . ?
C6 N6 C18 123.1(5) . . ?
C5 N5 C17 112.9(5) . . ?
C5 N5 C4 122.3(5) . . ?
C17 N5 C4 124.6(5) . . ?
N4 C16 N16 113.5(5) . . ?
N4 C16 C15 103.6(4) . . ?
N16 C16 C15 103.4(4) . . ?
N4 C16 H16 111.9 . . ?
N16 C16 H16 111.9 . . ?
C15 C16 H16 111.9 . . ?
C33 N21 C21 113.4(5) . . ?
C33 N21 C32 123.2(5) . . ?
C21 N21 C32 123.2(5) . . ?
C7 N7 C19 112.6(5) . . ?
C7 N7 C6 122.6(5) . . ?
C19 N7 C6 124.1(5) . . ?
C1 N1 C12 122.0(5) . . ?
C1 N1 C13 111.9(5) . . ?
C12 N1 C13 125.9(5) . . ?
C31 N20 C20 113.3(5) . . ?
C31 N20 C32 122.7(5) . . ?
C20 N20 C32 123.5(5) . . ?
O1X C2X N2X 126.5(6) . . ?
O1X C2X C1X 117.5(6) . . ?
N2X C2X C1X 115.9(6) . . ?
C29 N18 C18 113.1(5) . . ?
C29 N18 C30 122.3(5) . . ?
C18 N18 C30 124.2(5) . . ?
C11 N12 C12 124.3(5) . . ?
C11 N12 C24 112.9(5) . . ?
C12 N12 C24 122.7(5) . . ?
C35 N23 C34 122.5(5) . . ?
C35 N23 C23 112.2(5) . . ?
C34 N23 C23 123.7(5) . . ?
C1 N2 C2 122.5(5) . . ?
C1 N2 C14 112.7(5) . . ?
C2 N2 C14 123.1(5) . . ?
C35 N24 C24 112.0(5) . . ?
C35 N24 C36 123.2(5) . . ?
C24 N24 C36 124.5(5) . . ?
N19 C30 N18 112.7(4) . . ?
N19 C30 H30A 109.0 . . ?
N18 C30 H30A 109.0 . . ?
N19 C30 H30B 109.0 . . ?
N18 C30 H30B 109.0 . . ?
H30A C30 H30B 107.8 . . ?
C27 N16 C28 124.8(5) . . ?
C27 N16 C16 111.6(5) . . ?
C28 N16 C16 122.8(5) . . ?
O5 C9 N9 125.8(6) . . ?
O5 C9 N10 125.8(6) . . ?
N9 C9 N10 108.3(5) . . ?
C9 N10 C22 112.3(5) . . ?
C9 N10 C10 123.3(5) . . ?
C22 N10 C10 124.0(5) . . ?
C25 N13 C13 113.0(5) . . ?
C25 N13 C36 121.9(5) . . ?
C13 N13 C36 124.6(5) . . ?
N6 C6 N7 114.6(5) . . ?
N6 C6 H6A 108.6 . . ?
N7 C6 H6A 108.6 . . ?
N6 C6 H6B 108.6 . . ?
N7 C6 H6B 108.6 . . ?
H6A C6 H6B 107.6 . . ?
N10 C22 N22 114.2(5) . . ?
N10 C22 C21 103.7(5) . . ?
N22 C22 C21 103.3(5) . . ?
N10 C22 H22 111.7 . . ?
N22 C22 H22 111.7 . . ?
C21 C22 H22 111.7 . . ?
N24 C24 N12 114.5(5) . . ?
N24 C24 C23 104.0(5) . . ?
N12 C24 C23 102.5(5) . . ?
N24 C24 H24 111.7 . . ?
N12 C24 H24 111.7 . . ?
C23 C24 H24 111.7 . . ?
N23 C34 N22 113.7(5) . . ?
N23 C34 H34A 108.8 . . ?
N22 C34 H34A 108.8 . . ?
N23 C34 H34B 108.8 . . ?
N22 C34 H34B 108.8 . . ?
H34A C34 H34B 107.7 . . ?
O9 C29 N18 126.0(5) . . ?
O9 C29 N17 125.7(5) . . ?
N18 C29 N17 108.3(5) . . ?
N21 C21 N9 116.1(5) . . ?
N21 C21 C22 102.5(5) . . ?
N9 C21 C22 102.0(5) . . ?
N21 C21 H21 111.8 . . ?
N9 C21 H21 111.8 . . ?
C22 C21 H21 111.8 . . ?
N7 C19 N19 115.4(5) . . ?
N7 C19 C20 103.5(4) . . ?
N19 C19 C20 102.5(4) . . ?
N7 C19 H19 111.6 . . ?
N19 C19 H19 111.6 . . ?
C20 C19 H19 111.6 . . ?
C33 N22 C34 121.3(5) . . ?
C33 N22 C22 111.0(5) . . ?
C34 N22 C22 122.7(5) . . ?
N16 C28 N17 114.0(5) . . ?
N16 C28 H28A 108.8 . . ?
N17 C28 H28A 108.8 . . ?
N16 C28 H28B 108.8 . . ?
N17 C28 H28B 108.8 . . ?
H28A C28 H28B 107.7 . . ?
C3 N4 C4 121.6(5) . . ?
C3 N4 C16 112.2(5) . . ?
C4 N4 C16 121.7(5) . . ?
O12 C35 N23 126.8(6) . . ?
O12 C35 N24 124.2(6) . . ?
N23 C35 N24 109.0(5) . . ?
N3 C15 N15 114.3(5) . . ?
N3 C15 C16 102.4(5) . . ?
N15 C15 C16 103.0(4) . . ?
N3 C15 H15 112.1 . . ?
N15 C15 H15 112.1 . . ?
C16 C15 H15 112.1 . . ?
O8 C27 N15 124.9(5) . . ?
O8 C27 N16 125.7(5) . . ?
N15 C27 N16 109.4(5) . . ?
N11 C23 N23 113.1(5) . . ?
N11 C23 C24 103.8(5) . . ?
N23 C23 C24 102.7(5) . . ?
N11 C23 H23 112.2 . . ?
N23 C23 H23 112.2 . . ?
C24 C23 H23 112.2 . . ?
C31 N19 C30 120.2(5) . . ?
C31 N19 C19 112.0(5) . . ?
C30 N19 C19 120.3(5) . . ?
O6 C11 N12 126.3(6) . . ?
O6 C11 N11 124.5(6) . . ?
N12 C11 N11 109.2(5) . . ?
O3 C5 N5 125.6(5) . . ?
O3 C5 N6 126.1(6) . . ?
N5 C5 N6 108.2(5) . . ?
O2X C4X O3X 127.2(7) . . ?
O2X C4X C3X 117.2(6) . . ?
O3X C4X C3X 115.5(6) . . ?
N24 C36 N13 114.7(5) . . ?
N24 C36 H36A 108.6 . . ?
N13 C36 H36A 108.6 . . ?
N24 C36 H36B 108.6 . . ?
N13 C36 H36B 108.6 . . ?
H36A C36 H36B 107.6 . . ?
N18 C18 N6 115.7(4) . . ?
N18 C18 C17 103.1(4) . . ?
N6 C18 C17 103.7(4) . . ?
N18 C18 H18 111.3 . . ?
N6 C18 H18 111.3 . . ?
C17 C18 H18 111.3 . . ?
O7 C25 N14 126.2(5) . . ?
O7 C25 N13 126.6(5) . . ?
N14 C25 N13 107.2(5) . . ?
O10 C31 N19 127.0(6) . . ?
O10 C31 N20 125.8(5) . . ?
N19 C31 N20 107.1(5) . . ?
N8 C8 N9 113.1(5) . . ?
N8 C8 H8A 109.0 . . ?
N9 C8 H8A 109.0 . . ?
N8 C8 H8B 109.0 . . ?
N9 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
N20 C32 N21 114.0(5) . . ?
N20 C32 H32A 108.7 . . ?
N21 C32 H32A 108.7 . . ?
N20 C32 H32B 108.7 . . ?
N21 C32 H32B 108.7 . . ?
H32A C32 H32B 107.6 . . ?
N5 C17 N17 115.8(5) . . ?
N5 C17 C18 102.8(4) . . ?
N17 C17 C18 103.2(4) . . ?
N5 C17 H17 111.5 . . ?
N17 C17 H17 111.5 . . ?
C18 C17 H17 111.5 . . ?
O2 C3 N3 127.0(6) . . ?
O2 C3 N4 125.6(6) . . ?
N3 C3 N4 107.4(5) . . ?
N2 C14 N14 114.8(5) . . ?
N2 C14 C13 102.8(4) . . ?
N14 C14 C13 102.8(5) . . ?
N2 C14 H14 111.9 . . ?
N14 C14 H14 111.9 . . ?
C13 C14 H14 111.9 . . ?
N4 C4 N5 113.6(4) . . ?
N4 C4 H4A 108.8 . . ?
N5 C4 H4A 108.8 . . ?
N4 C4 H4B 108.8 . . ?
N5 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
N15 C26 N14 115.0(5) . . ?
N15 C26 H26A 108.5 . . ?
N14 C26 H26A 108.5 . . ?
N15 C26 H26B 108.5 . . ?
N14 C26 H26B 108.5 . . ?
H26A C26 H26B 107.5 . . ?
C11 N11 C10 123.9(5) . . ?
C11 N11 C23 111.6(5) . . ?
C10 N11 C23 124.0(5) . . ?
O1 C1 N2 126.4(6) . . ?
O1 C1 N1 124.7(6) . . ?
N2 C1 N1 108.9(5) . . ?
C1X N1X H1X1 109.5 . . ?
C1X N1X H1X2 109.5 . . ?
H1X1 N1X H1X2 109.5 . . ?
C1X N1X H1X3 109.5 . . ?
H1X1 N1X H1X3 109.5 . . ?
H1X2 N1X H1X3 109.5 . . ?
O4 C7 N8 126.4(5) . . ?
O4 C7 N7 125.5(5) . . ?
N8 C7 N7 108.0(5) . . ?
O11 C33 N21 126.6(6) . . ?
O11 C33 N22 125.2(6) . . ?
N21 C33 N22 108.2(5) . . ?
N2X C3X C4X 108.9(5) . . ?
N2X C3X C5X 108.9(5) . . ?
C4X C3X C5X 111.0(6) . . ?
N2X C3X H3X 109.3 . . ?
C4X C3X H3X 109.3 . . ?
C5X C3X H3X 109.3 . . ?
C2X N2X C3X 123.1(6) . . ?
C2X N2X H2X 118.4 . . ?
C3X N2X H2X 118.4 . . ?
N13 C13 N1 114.9(5) . . ?
N13 C13 C14 103.3(5) . . ?
N1 C13 C14 103.3(5) . . ?
N13 C13 H13 111.6 . . ?
N1 C13 H13 111.6 . . ?
C14 C13 H13 111.6 . . ?
N1X C1X C2X 110.3(6) . . ?
N1X C1X H1X 109.6 . . ?
C2X C1X H1X 109.6 . . ?
N1X C1X H2X2 109.6 . . ?
C2X C1X H2X2 109.6 . . ?
H1X C1X H2X2 108.1 . . ?
N1 C12 N12 114.8(5) . . ?
N1 C12 H12A 108.6 . . ?
N12 C12 H12A 108.6 . . ?
N1 C12 H12B 108.6 . . ?
N12 C12 H12B 108.6 . . ?
H12A C12 H12B 107.6 . . ?
N3 C2 N2 113.1(4) . . ?
N3 C2 H2A 109.0 . . ?
N2 C2 H2A 109.0 . . ?
N3 C2 H2B 109.0 . . ?
N2 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
N20 C20 N8 116.1(5) . . ?
N20 C20 C19 103.3(5) . . ?
N8 C20 C19 102.4(4) . . ?
N20 C20 H20 111.4 . . ?
N8 C20 H20 111.4 . . ?
C19 C20 H20 111.4 . . ?
N10 C10 N11 114.4(5) . . ?
N10 C10 H10A 108.7 . . ?
N11 C10 H10A 108.7 . . ?
N10 C10 H10B 108.7 . . ?
N11 C10 H10B 108.7 . . ?
H10A C10 H10B 107.6 . . ?
C6X C5X C3X 115.1(5) . . ?
C6X C5X H5X1 108.5 . . ?
C3X C5X H5X1 108.5 . . ?
C6X C5X H5X2 108.5 . . ?
C3X C5X H5X2 108.5 . . ?
H5X1 C5X H5X2 107.5 . . ?
C7X C6X C11X 119.7(9) . . ?
C7X C6X C5X 120.9(10) . . ?
C11X C6X C5X 119.4(8) . . ?
C6X C7X C8X 119.2(13) . . ?
C6X C7X H7X 120.4 . . ?
C8X C7X H7X 120.4 . . ?
C9X C8X C7X 119.7(12) . . ?
C9X C8X H8X 120.1 . . ?
C7X C8X H8X 120.1 . . ?
C8X C9X C10X 121.9(12) . . ?
C8X C9X H9X 119.0 . . ?
C10X C9X H9X 119.0 . . ?
C9X C10X C11X 117.7(14) . . ?
C9X C10X H10X 121.1 . . ?
C11X C10X H10X 121.1 . . ?
C6X C11X C10X 121.7(11) . . ?
C6X C11X H11X 119.2 . . ?
C10X C11X H11X 119.2 . . ?

_refine_diff_density_max         1.431
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.107

_shelxl_version_number           2013-3

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
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data_q6_mgcl2_glytyr2
_database_code_depnum_ccdc_archive 'CCDC 1548094'
_audit_update_record             
;
2017-05-05 deposited with the CCDC.
2017-06-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            'cucurbit[6]uril/Gly-Tyr exclusion complex'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C47 H50 N26 O29.50'
_chemical_formula_weight         1451.13

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'
O O 0.0106 0.0060 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   12.8204(14)
_cell_length_b                   15.4423(9)
_cell_length_c                   16.4045(11)
_cell_angle_alpha                90
_cell_angle_beta                 103.346(4)
_cell_angle_gamma                90
_cell_volume                     3159.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7568
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      27.3

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_F_000             1500
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.129
_shelx_estimated_absorpt_T_min   0.944
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  KappaApexII
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            49148
_diffrn_reflns_av_unetI/netI     0.0566
_diffrn_reflns_av_R_equivalents  0.073
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_theta_min         2.645
_diffrn_reflns_theta_max         28.982
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             16170
_reflns_number_gt                11643
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.875
_reflns_Friedel_fraction_max     0.933
_reflns_Friedel_fraction_full    0.982

_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
'Collect data collection software (Nonius B.V., 1998)'
_computing_cell_refinement       'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_data_reduction        'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0821P)²+4.1782P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 4300 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.0(7)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         16170
_refine_ls_number_parameters     1151
_refine_ls_number_restraints     323
_refine_ls_R_factor_all          0.1223
_refine_ls_R_factor_gt           0.0807
_refine_ls_wR_factor_ref         0.2098
_refine_ls_wR_factor_gt          0.1811
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O10 O 0.1552(4) 0.4984(3) 0.4695(3) 0.0338(10) Uani 1 1 d . . . . .
O4 O -0.0806(4) 0.1652(3) 0.3245(3) 0.0346(10) Uani 1 1 d . . . . .
O5 O 0.0793(3) 0.0523(3) 0.4802(3) 0.0323(9) Uani 1 1 d . . . . .
O11 O 0.3064(3) 0.3876(3) 0.6259(3) 0.0318(9) Uani 1 1 d . . . . .
O6 O 0.3170(4) -0.0134(3) 0.4389(3) 0.0352(10) Uani 1 1 d . . . . .
N23 N 0.4703(4) 0.1837(3) 0.6243(3) 0.0274(10) Uani 1 1 d . . . . .
N10 N 0.2031(4) 0.1029(3) 0.5950(3) 0.0288(10) Uani 1 1 d . . . . .
N14 N 0.6469(4) 0.2306(3) 0.3023(3) 0.0332(11) Uani 1 1 d . . . . .
N21 N 0.1470(4) 0.3143(3) 0.6124(3) 0.0273(10) Uani 1 1 d . . . . .
O1 O 0.4228(4) 0.0059(3) 0.2597(3) 0.0420(11) Uani 1 1 d . . . . .
O9 O 0.2486(4) 0.5381(3) 0.2928(3) 0.0411(11) Uani 1 1 d . . . . .
O7 O 0.6792(3) 0.3239(3) 0.4160(3) 0.0332(9) Uani 1 1 d . . . . .
N7 N -0.0722(4) 0.3136(3) 0.3070(3) 0.0319(11) Uani 1 1 d . . . . .
O12 O 0.5644(4) 0.2994(3) 0.5871(3) 0.0327(10) Uani 1 1 d . . . . .
C23 C 0.4706(5) 0.0902(4) 0.6186(4) 0.0284(12) Uani 1 1 d . . . . .
H23 H 0.4916 0.0623 0.6751 0.034 Uiso 1 1 calc R U . . .
N24 N 0.5946(4) 0.1581(3) 0.5532(3) 0.0294(11) Uani 1 1 d . . . . .
N9 N 0.0603(4) 0.1833(3) 0.5439(3) 0.0281(10) Uani 1 1 d . . . . .
N22 N 0.2992(4) 0.2392(3) 0.6406(3) 0.0275(10) Uani 1 1 d . . . . .
N2 N 0.5527(4) 0.1004(4) 0.2383(4) 0.0370(12) Uani 1 1 d . . . . .
O15W O 0.4491(5) 0.3536(4) 0.4194(3) 0.0568(14) Uani 1 1 d . . . . .
C19 C -0.0756(5) 0.3910(4) 0.3570(4) 0.0298(12) Uani 1 1 d . . . . .
H19 H -0.1452 0.4226 0.3386 0.036 Uiso 1 1 calc R U . . .
N13 N 0.6687(4) 0.1751(3) 0.4300(3) 0.0292(10) Uani 1 1 d . . . . .
N16 N 0.3806(4) 0.3891(3) 0.1571(3) 0.0315(11) Uani 1 1 d . . . . .
C34 C 0.4125(5) 0.2293(4) 0.6777(4) 0.0277(12) Uani 1 1 d . . . . .
H34A H 0.4212 0.1974 0.7312 0.033 Uiso 1 1 calc R U . . .
H34B H 0.4447 0.2874 0.6907 0.033 Uiso 1 1 calc R U . . .
C21 C 0.1111(5) 0.2276(4) 0.6210(4) 0.0265(12) Uani 1 1 d . . . . .
H21 H 0.0657 0.2246 0.6630 0.032 Uiso 1 1 calc R U . . .
N18 N 0.0830(5) 0.4756(4) 0.2401(3) 0.0354(12) Uani 1 1 d . . . . .
N5 N 0.1259(4) 0.3195(3) 0.1112(3) 0.0314(11) Uani 1 1 d . . . . .
N11 N 0.3728(4) 0.0535(3) 0.5680(3) 0.0290(10) Uani 1 1 d . . . . .
N15 N 0.5340(4) 0.3162(3) 0.1928(3) 0.0359(12) Uani 1 1 d . . . . .
N6 N 0.0059(4) 0.3357(3) 0.1880(3) 0.0338(12) Uani 1 1 d . . . . .
C7 C -0.0719(5) 0.2392(4) 0.3523(4) 0.0283(12) Uani 1 1 d . . . . .
O3 O 0.0404(4) 0.1982(3) 0.1452(3) 0.0394(11) Uani 1 1 d . . . . .
C32 C 0.0756(5) 0.3859(3) 0.5806(4) 0.0262(12) Uani 1 1 d . . . . .
H32A H 0.0111 0.3817 0.6039 0.031 Uiso 1 1 calc R U . . .
H32B H 0.1122 0.4410 0.6004 0.031 Uiso 1 1 calc R U . . .
O2 O 0.2769(4) 0.1165(3) 0.1110(3) 0.0442(12) Uani 1 1 d . . . . .
C8 C -0.0502(5) 0.1990(4) 0.5010(4) 0.0301(13) Uani 1 1 d . . . . .
H8A H -0.0827 0.1434 0.4780 0.036 Uiso 1 1 calc R U . . .
H8B H -0.0897 0.2193 0.5426 0.036 Uiso 1 1 calc R U . . .
C25 C 0.6656(5) 0.2513(4) 0.3859(4) 0.0318(13) Uani 1 1 d . . . . .
C31 C 0.0793(5) 0.4496(4) 0.4445(4) 0.0312(13) Uani 1 1 d . . . . .
N1 N 0.5609(4) 0.0511(3) 0.3665(3) 0.0313(11) Uani 1 1 d . . . . .
N12 N 0.4903(4) 0.0346(3) 0.4890(4) 0.0319(11) Uani 1 1 d . . . . .
C36 C 0.6890(5) 0.1721(4) 0.5202(4) 0.0285(12) Uani 1 1 d . . . . .
H36A H 0.7229 0.2274 0.5429 0.034 Uiso 1 1 calc R U . . .
H36B H 0.7410 0.1251 0.5406 0.034 Uiso 1 1 calc R U . . .
N20 N 0.0427(4) 0.3878(3) 0.4908(3) 0.0282(10) Uani 1 1 d . . . . .
C5 C 0.0565(5) 0.2760(4) 0.1476(4) 0.0338(14) Uani 1 1 d . . . . .
C17 C 0.1190(5) 0.4129(4) 0.1204(4) 0.0340(13) Uani 1 1 d . . . . .
H17 H 0.1004 0.4427 0.0648 0.041 Uiso 1 1 calc R U . . .
C24 C 0.5537(5) 0.0723(3) 0.5648(4) 0.0267(12) Uani 1 1 d . . . . .
H24 H 0.6119 0.0324 0.5939 0.032 Uiso 1 1 calc R U . . .
O8 O 0.5069(4) 0.4311(3) 0.2751(3) 0.0451(12) Uani 1 1 d . . . . .
C26 C 0.6425(5) 0.2967(4) 0.2385(4) 0.0354(14) Uani 1 1 d . . . . .
H26A H 0.6763 0.3503 0.2654 0.042 Uiso 1 1 calc R U . . .
H26B H 0.6846 0.2770 0.1984 0.042 Uiso 1 1 calc R U . . .
C1 C 0.5044(5) 0.0488(4) 0.2867(4) 0.0341(14) Uani 1 1 d . . . . .
C13 C 0.6606(5) 0.0993(4) 0.3764(4) 0.0311(13) Uani 1 1 d . . . . .
H13 H 0.7246 0.0608 0.3935 0.037 Uiso 1 1 calc R U . . .
N17 N 0.2133(5) 0.4506(3) 0.1751(3) 0.0348(12) Uani 1 1 d . . . . .
C11 C 0.3857(5) 0.0213(3) 0.4934(4) 0.0282(12) Uani 1 1 d . . . . .
C15 C 0.4791(5) 0.2739(4) 0.1173(4) 0.0339(14) Uani 1 1 d . . . . .
H15 H 0.5222 0.2744 0.0737 0.041 Uiso 1 1 calc R U . . .
N8 N -0.0651(4) 0.2612(3) 0.4340(3) 0.0282(11) Uani 1 1 d . . . . .
C6 C -0.0882(5) 0.3135(4) 0.2170(4) 0.0322(13) Uani 1 1 d . . . . .
H6A H -0.1126 0.2552 0.1956 0.039 Uiso 1 1 calc R U . . .
H6B H -0.1459 0.3551 0.1931 0.039 Uiso 1 1 calc R U . . .
C35 C 0.5444(5) 0.2220(4) 0.5881(4) 0.0270(12) Uani 1 1 d . . . . .
C20 C -0.0607(5) 0.3540(4) 0.4475(4) 0.0274(12) Uani 1 1 d . . . . .
H20 H -0.1191 0.3740 0.4743 0.033 Uiso 1 1 calc R U . . .
C33 C 0.2560(5) 0.3207(4) 0.6253(4) 0.0276(12) Uani 1 1 d . . . . .
C22 C 0.2178(5) 0.1763(4) 0.6515(4) 0.0265(12) Uani 1 1 d . . . . .
H22 H 0.2283 0.1576 0.7112 0.032 Uiso 1 1 calc R U . . .
C16 C 0.3740(5) 0.3280(4) 0.0898(4) 0.0337(13) Uani 1 1 d . . . . .
H16 H 0.3690 0.3574 0.0347 0.040 Uiso 1 1 calc R U . . .
N19 N 0.0153(5) 0.4488(3) 0.3653(3) 0.0334(11) Uani 1 1 d . . . . .
C9 C 0.1122(5) 0.1070(4) 0.5339(4) 0.0280(12) Uani 1 1 d . . . . .
N3 N 0.4398(4) 0.1875(3) 0.1296(4) 0.0364(12) Uani 1 1 d . . . . .
C27 C 0.4763(5) 0.3842(4) 0.2148(4) 0.0333(13) Uani 1 1 d . . . . .
N4 N 0.2906(4) 0.2619(3) 0.0851(3) 0.0352(12) Uani 1 1 d . . . . .
C3 C 0.3305(5) 0.1823(4) 0.1090(4) 0.0335(13) Uani 1 1 d . . . . .
C10 C 0.2809(5) 0.0334(4) 0.6007(4) 0.0293(12) Uani 1 1 d . . . . .
H10A H 0.3060 0.0168 0.6603 0.035 Uiso 1 1 calc R U . . .
H10B H 0.2444 -0.0175 0.5702 0.035 Uiso 1 1 calc R U . . .
C18 C 0.0312(6) 0.4241(4) 0.1684(4) 0.0349(14) Uani 1 1 d . . . . .
H18 H -0.0328 0.4543 0.1337 0.042 Uiso 1 1 calc R U . . .
C29 C 0.1875(6) 0.4923(4) 0.2421(4) 0.0332(13) Uani 1 1 d . . . . .
C14 C 0.6521(5) 0.1381(4) 0.2884(4) 0.0310(13) Uani 1 1 d . . . . .
H14 H 0.7154 0.1224 0.2655 0.037 Uiso 1 1 calc R U . . .
C4 C 0.1777(5) 0.2791(4) 0.0517(4) 0.0339(14) Uani 1 1 d . . . . .
H4A H 0.1698 0.3171 0.0021 0.041 Uiso 1 1 calc R U . . .
H4B H 0.1408 0.2238 0.0329 0.041 Uiso 1 1 calc R U . . .
C30 C 0.0278(6) 0.5102(4) 0.3009(4) 0.0384(15) Uani 1 1 d . . . . .
H30A H -0.0441 0.5305 0.2708 0.046 Uiso 1 1 calc R U . . .
H30B H 0.0680 0.5612 0.3283 0.046 Uiso 1 1 calc R U . . .
C2 C 0.5095(5) 0.1130(4) 0.1497(4) 0.0367(14) Uani 1 1 d . . . . .
H2A H 0.4690 0.0606 0.1265 0.044 Uiso 1 1 calc R U . . .
H2B H 0.5698 0.1196 0.1217 0.044 Uiso 1 1 calc R U . . .
C12 C 0.5400(5) -0.0078(4) 0.4296(4) 0.0330(13) Uani 1 1 d . . . . .
H12A H 0.4926 -0.0550 0.4017 0.040 Uiso 1 1 calc R U . . .
H12B H 0.6084 -0.0341 0.4598 0.040 Uiso 1 1 calc R U . . .
C28 C 0.3130(6) 0.4659(4) 0.1511(4) 0.0366(14) Uani 1 1 d . . . . .
H28A H 0.3531 0.5118 0.1873 0.044 Uiso 1 1 calc R U . . .
H28B H 0.2971 0.4873 0.0926 0.044 Uiso 1 1 calc R U . . .
O12B O 0.331(3) 0.193(3) 0.374(3) 0.29(4) Uani 0.4 1 d . . P A 1
O12A O 0.234(3) 0.313(2) 0.385(3) 0.090(12) Uani 0.2 1 d . . P B 1
N1X N 0.2183(13) 0.0302(15) 0.2694(12) 0.053(5) Uani 0.393(15) 1 d D U P C 1
H1X1 H 0.2106 0.0083 0.2168 0.080 Uiso 0.393(15) 1 calc R U P C 1
H1X2 H 0.2530 -0.0090 0.3075 0.080 Uiso 0.393(15) 1 calc R U P C 1
H1X3 H 0.2572 0.0801 0.2741 0.080 Uiso 0.393(15) 1 calc R U P C 1
N2X N -0.0656(15) 0.0278(13) 0.2059(13) 0.029(4) Uani 0.393(15) 1 d D U P C 1
H2X H -0.0768 0.0805 0.2225 0.035 Uiso 0.393(15) 1 calc R U P C 1
O1X O 0.0529(14) -0.0777(9) 0.2031(15) 0.064(5) Uani 0.393(15) 1 d D U P C 1
C1X C 0.1135(17) 0.0483(15) 0.285(2) 0.043(6) Uani 0.393(15) 1 d D U P C 1
H1XA H 0.0956 0.1102 0.2734 0.051 Uiso 0.393(15) 1 calc R U P C 1
H1XB H 0.1142 0.0365 0.3442 0.051 Uiso 0.393(15) 1 calc R U P C 1
C2X C 0.0303(16) -0.0077(13) 0.2287(17) 0.036(5) Uani 0.393(15) 1 d D U P C 1
C3X C -0.1515(18) -0.0206(11) 0.1537(14) 0.033(5) Uani 0.393(15) 1 d D U P C 1
H3X H -0.1213 -0.0589 0.1158 0.039 Uiso 0.393(15) 1 calc R U P C 1
C4X C -0.2315(16) 0.0420(9) 0.1006(10) 0.027(4) Uani 0.393(15) 1 d D U P C 1
C5X C -0.206(2) -0.0770(12) 0.2087(16) 0.044(5) Uani 0.393(15) 1 d D U P C 1
H5X1 H -0.1491 -0.1087 0.2489 0.052 Uiso 0.393(15) 1 calc R U P C 1
H5X2 H -0.2416 -0.0383 0.2418 0.052 Uiso 0.393(15) 1 calc R U P C 1
C6X C -0.2856(17) -0.1410(12) 0.1651(19) 0.034(4) Uani 0.393(15) 1 d D U P C 1
C7X C -0.3949(17) -0.1223(16) 0.1508(19) 0.046(6) Uani 0.393(15) 1 d D U P C 1
H7X H -0.4171 -0.0669 0.1654 0.055 Uiso 0.393(15) 1 calc R U P C 1
C8X C -0.4720(17) -0.1837(18) 0.1153(14) 0.048(6) Uani 0.393(15) 1 d D U P C 1
H8X H -0.5457 -0.1684 0.1041 0.057 Uiso 0.393(15) 1 calc R U P C 1
C9X C -0.444(2) -0.2656(18) 0.096(3) 0.047(7) Uani 0.393(15) 1 d D U P C 1
C10X C -0.336(2) -0.2840(15) 0.108(3) 0.035(6) Uani 0.393(15) 1 d D U P C 1
H10X H -0.3145 -0.3396 0.0928 0.042 Uiso 0.393(15) 1 calc R U P C 1
C11X C -0.2573(16) -0.2210(11) 0.1410(15) 0.023(4) Uani 0.393(15) 1 d D U P C 1
H11X H -0.1836 -0.2345 0.1469 0.028 Uiso 0.393(15) 1 calc R U P C 1
O2X O -0.2361(11) 0.1158(10) 0.1287(13) 0.024(5) Uani 0.393(15) 1 d D U P C 1
O3X O -0.2963(12) 0.0092(10) 0.0412(8) 0.039(4) Uani 0.393(15) 1 d D U P C 1
O4X O -0.538(3) -0.322(3) 0.067(3) 0.163(18) Uani 0.393(15) 1 d D U P C 1
H4X H -0.5181 -0.3715 0.0562 0.245 Uiso 0.393(15) 1 calc R U P C 1
N1XA N 0.2291(9) 0.0851(9) 0.2786(9) 0.055(3) Uani 0.607(15) 1 d D U P C 2
H1X4 H 0.2669 0.0373 0.3006 0.082 Uiso 0.607(15) 1 calc R U P C 2
H1X5 H 0.2621 0.1333 0.3041 0.082 Uiso 0.607(15) 1 calc R U P C 2
H1X6 H 0.2259 0.0878 0.2227 0.082 Uiso 0.607(15) 1 calc R U P C 2
N2XA N -0.0506(14) 0.0343(15) 0.2082(16) 0.070(7) Uani 0.607(15) 1 d D U P C 2
H2XA H -0.0732 0.0816 0.2284 0.084 Uiso 0.607(15) 1 calc R U P C 2
O1XA O 0.0970(15) -0.0401(15) 0.2023(16) 0.141(10) Uani 0.607(15) 1 d D U P C 2
C1XA C 0.1208(11) 0.0799(12) 0.2921(11) 0.045(4) Uani 0.607(15) 1 d D U P C 2
H1XC H 0.0880 0.1383 0.2868 0.054 Uiso 0.607(15) 1 calc R U P C 2
H1XD H 0.1235 0.0582 0.3494 0.054 Uiso 0.607(15) 1 calc R U P C 2
C2XA C 0.0536(14) 0.0199(12) 0.2287(12) 0.051(4) Uani 0.607(15) 1 d D U P C 2
C3XA C -0.1312(19) -0.0192(15) 0.1563(16) 0.077(7) Uani 0.607(15) 1 d D U P C 2
H3XA H -0.0992 -0.0558 0.1180 0.093 Uiso 0.607(15) 1 calc R U P C 2
C4XA C -0.219(3) 0.0401(19) 0.1059(17) 0.113(10) Uani 0.607(15) 1 d D U P C 2
C5XA C -0.182(3) -0.0762(19) 0.2137(17) 0.118(11) Uani 0.607(15) 1 d D U P C 2
H5X3 H -0.1240 -0.1064 0.2537 0.142 Uiso 0.607(15) 1 calc R U P C 2
H5X4 H -0.2188 -0.0379 0.2466 0.142 Uiso 0.607(15) 1 calc R U P C 2
C6XA C -0.261(3) -0.1422(18) 0.171(2) 0.112(10) Uani 0.607(15) 1 d D U P C 2
C7XA C -0.371(3) -0.1257(18) 0.157(3) 0.120(10) Uani 0.607(15) 1 d D U P C 2
H7XA H -0.3941 -0.0715 0.1735 0.144 Uiso 0.607(15) 1 calc R U P C 2
C8XA C -0.449(2) -0.1867(14) 0.119(2) 0.103(8) Uani 0.607(15) 1 d D U P C 2
H8XA H -0.5228 -0.1733 0.1093 0.123 Uiso 0.607(15) 1 calc R U P C 2
C9XA C -0.416(2) -0.2660(15) 0.096(2) 0.079(7) Uani 0.607(15) 1 d D U P C 2
C101 C -0.309(2) -0.2830(18) 0.109(3) 0.073(7) Uani 0.607(15) 1 d D U P C 2
H101 H -0.2861 -0.3357 0.0888 0.087 Uiso 0.607(15) 1 calc R U P C 2
C111 C -0.230(2) -0.2237(19) 0.153(2) 0.108(9) Uani 0.607(15) 1 d D U P C 2
H111 H -0.1571 -0.2407 0.1695 0.130 Uiso 0.607(15) 1 calc R U P C 2
O2XA O -0.235(2) 0.1136(17) 0.1312(16) 0.103(8) Uani 0.607(15) 1 d D U P C 2
O3XA O -0.266(4) 0.013(2) 0.0361(15) 0.30(2) Uani 0.607(15) 1 d D U P C 2
O4XA O -0.4998(10) -0.3286(8) 0.0602(7) 0.050(3) Uani 0.607(15) 1 d D U P C 2
H4XA H -0.4717 -0.3767 0.0548 0.075 Uiso 0.607(15) 1 calc R U P C 2
O12W O 0.3063(15) 0.243(2) 0.3053(12) 0.164(11) Uani 0.607(15) 1 d . . P C 2
O6W O -0.6924(9) -0.2739(8) -0.0126(8) 0.078(4) Uani 0.607(15) 1 d . . P C 2
O1W O 0.2487(5) 0.0053(4) 0.8077(4) 0.0591(15) Uani 1 1 d . . . . .
O2W O -0.1712(5) 0.3490(4) 0.6217(4) 0.0580(15) Uani 1 1 d . . . . .
O3W O 0.0042(10) 0.5786(6) -0.0076(6) 0.118(3) Uani 1 1 d . . . . .
O4W O -0.1011(11) 0.6082(7) 0.1198(7) 0.138(4) Uani 1 1 d . . . . .
O9W O 0.2274(10) 0.7083(7) 0.2511(11) 0.119(7) Uani 0.654(19) 1 d . . P D 1
O7W O 0.0162(10) -0.2584(9) 0.2177(9) 0.095(5) Uani 0.654(19) 1 d . . P D 1
O9WA O 0.115(3) 0.7026(16) 0.2892(19) 0.113(12) Uani 0.346(19) 1 d . . P D 2
O5W O -0.5034(18) -0.5087(11) 0.0385(16) 0.063(6) Uani 0.383(19) 1 d . . P E 1
O10W O -0.3278(14) -0.6013(9) 0.0607(9) 0.055(5) Uani 0.383(19) 1 d . . P E 1
O14W O -0.193(5) -0.518(5) -0.011(6) 0.35(6) Uani 0.383(19) 1 d . . P E 1
O14A O -0.288(2) -0.5525(9) -0.0654(13) 0.165(12) Uani 0.617(19) 1 d . . P E 2
O5WA O -0.459(3) -0.503(3) 0.0622(18) 0.25(2) Uani 0.617(19) 1 d . . P E 2
O11W O 0.3165(10) -0.1479(7) 0.2283(10) 0.164(6) Uani 1 1 d . . . . .
O8W O -0.057(5) 0.371(5) -0.059(4) 0.21(3) Uiso 0.404(19) 1 d . . P F 1
O13W O -0.8441(14) -0.2980(11) 0.0767(11) 0.070(6) Uiso 0.404(19) 1 d . . P F 1
O16W O -0.167(3) 0.343(2) 0.0281(14) 0.145(14) Uani 0.404(19) 1 d . . P F 1
O8WA O -0.0512(18) 0.3564(15) -0.0501(19) 0.153(16) Uani 0.596(19) 1 d . . P F
2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
O10 C31 1.225(7) . ?
O4 C7 1.226(7) . ?
O5 C9 1.224(7) . ?
O11 C33 1.217(7) . ?
O6 C11 1.224(8) . ?
N23 C35 1.366(8) . ?
N23 C23 1.447(7) . ?
N23 C34 1.455(7) . ?
N10 C9 1.353(8) . ?
N10 C22 1.447(8) . ?
N10 C10 1.454(7) . ?
N14 C25 1.374(9) . ?
N14 C14 1.450(8) . ?
N14 C26 1.455(8) . ?
N21 C33 1.367(8) . ?
N21 C21 1.434(7) . ?
N21 C32 1.453(7) . ?
O1 C1 1.231(8) . ?
O9 C29 1.225(8) . ?
O7 C25 1.221(7) . ?
N7 C7 1.368(8) . ?
N7 C6 1.443(8) . ?
N7 C19 1.457(8) . ?
O12 C35 1.223(7) . ?
C23 N11 1.449(8) . ?
C23 C24 1.556(9) . ?
C23 H23 1.0000 . ?
N24 C35 1.373(7) . ?
N24 C36 1.451(8) . ?
N24 C24 1.455(7) . ?
N9 C9 1.380(8) . ?
N9 C8 1.449(8) . ?
N9 C21 1.454(8) . ?
N22 C33 1.374(8) . ?
N22 C34 1.447(8) . ?
N22 C22 1.467(7) . ?
N2 C1 1.369(9) . ?
N2 C2 1.445(9) . ?
N2 C14 1.468(8) . ?
C19 N19 1.449(8) . ?
C19 C20 1.562(9) . ?
C19 H19 1.0000 . ?
N13 C25 1.377(8) . ?
N13 C36 1.442(8) . ?
N13 C13 1.454(8) . ?
N16 C27 1.368(8) . ?
N16 C16 1.440(8) . ?
N16 C28 1.459(8) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C21 C22 1.561(8) . ?
C21 H21 1.0000 . ?
N18 C29 1.358(9) . ?
N18 C18 1.448(8) . ?
N18 C30 1.451(8) . ?
N5 C5 1.358(9) . ?
N5 C4 1.443(8) . ?
N5 C17 1.455(8) . ?
N11 C11 1.366(8) . ?
N11 C10 1.437(7) . ?
N15 C27 1.379(8) . ?
N15 C15 1.434(8) . ?
N15 C26 1.451(8) . ?
N6 C5 1.381(8) . ?
N6 C6 1.437(8) . ?
N6 C18 1.455(8) . ?
C7 N8 1.366(8) . ?
O3 C5 1.218(8) . ?
C32 N20 1.435(8) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
O2 C3 1.231(8) . ?
C8 N8 1.438(8) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C31 N19 1.368(9) . ?
C31 N20 1.368(8) . ?
N1 C1 1.343(9) . ?
N1 C12 1.447(8) . ?
N1 C13 1.456(8) . ?
N12 C11 1.376(8) . ?
N12 C12 1.438(8) . ?
N12 C24 1.442(8) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
N20 C20 1.450(8) . ?
C17 N17 1.451(9) . ?
C17 C18 1.524(9) . ?
C17 H17 1.0000 . ?
C24 H24 1.0000 . ?
O8 C27 1.216(8) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C13 C14 1.543(9) . ?
C13 H13 1.0000 . ?
N17 C29 1.378(8) . ?
N17 C28 1.442(9) . ?
C15 N3 1.457(8) . ?
C15 C16 1.560(9) . ?
C15 H15 1.0000 . ?
N8 C20 1.449(7) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C20 H20 1.0000 . ?
C22 H22 1.0000 . ?
C16 N4 1.467(8) . ?
C16 H16 1.0000 . ?
N19 C30 1.456(8) . ?
N3 C3 1.366(9) . ?
N3 C2 1.447(8) . ?
N4 C3 1.354(8) . ?
N4 C4 1.450(9) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C18 H18 1.0000 . ?
C14 H14 1.0000 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
N1X C1X 1.45(2) . ?
N1X H1X1 0.9100 . ?
N1X H1X2 0.9100 . ?
N1X H1X3 0.9100 . ?
N2X C2X 1.319(19) . ?
N2X C3X 1.438(19) . ?
N2X H2X 0.8800 . ?
O1X C2X 1.22(2) . ?
C1X C2X 1.51(2) . ?
C1X H1XA 0.9900 . ?
C1X H1XB 0.9900 . ?
C3X C4X 1.527(18) . ?
C3X C5X 1.532(19) . ?
C3X H3X 1.0000 . ?
C4X O3X 1.235(16) . ?
C4X O2X 1.236(15) . ?
C5X C6X 1.48(2) . ?
C5X H5X1 0.9900 . ?
C5X H5X2 0.9900 . ?
C6X C11X 1.372(17) . ?
C6X C7X 1.40(2) . ?
C7X C8X 1.40(2) . ?
C7X H7X 0.9500 . ?
C8X C9X 1.37(2) . ?
C8X H8X 0.9500 . ?
C9X C10X 1.38(2) . ?
C9X O4X 1.480(19) . ?
C10X C11X 1.42(2) . ?
C10X H10X 0.9500 . ?
C11X H11X 0.9500 . ?
O4X H4X 0.8400 . ?
N1XA C1XA 1.458(16) . ?
N1XA H1X4 0.9100 . ?
N1XA H1X5 0.9100 . ?
N1XA H1X6 0.9100 . ?
N2XA C2XA 1.319(17) . ?
N2XA C3XA 1.438(18) . ?
N2XA H2XA 0.8800 . ?
O1XA C2XA 1.211(17) . ?
C1XA C2XA 1.51(2) . ?
C1XA H1XC 0.9900 . ?
C1XA H1XD 0.9900 . ?
C3XA C4XA 1.53(2) . ?
C3XA C5XA 1.54(2) . ?
C3XA H3XA 1.0000 . ?
C4XA O3XA 1.24(2) . ?
C4XA O2XA 1.24(2) . ?
C5XA C6XA 1.49(2) . ?
C5XA H5X3 0.9900 . ?
C5XA H5X4 0.9900 . ?
C6XA C111 1.37(2) . ?
C6XA C7XA 1.40(3) . ?
C7XA C8XA 1.41(2) . ?
C7XA H7XA 0.9500 . ?
C8XA C9XA 1.38(2) . ?
C8XA H8XA 0.9500 . ?
C9XA C101 1.36(2) . ?
C9XA O4XA 1.462(19) . ?
C101 C111 1.43(2) . ?
C101 H101 0.9500 . ?
C111 H111 0.9500 . ?
O4XA H4XA 0.8400 . ?

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
C35 N23 C23 113.1(5) . . ?
C35 N23 C34 123.6(5) . . ?
C23 N23 C34 122.1(5) . . ?
C9 N10 C22 113.6(5) . . ?
C9 N10 C10 122.9(5) . . ?
C22 N10 C10 123.4(5) . . ?
C25 N14 C14 112.5(5) . . ?
C25 N14 C26 121.5(5) . . ?
C14 N14 C26 125.0(5) . . ?
C33 N21 C21 113.1(5) . . ?
C33 N21 C32 122.5(5) . . ?
C21 N21 C32 123.7(5) . . ?
C7 N7 C6 122.5(5) . . ?
C7 N7 C19 112.3(5) . . ?
C6 N7 C19 124.2(5) . . ?
N23 C23 N11 114.3(5) . . ?
N23 C23 C24 103.1(4) . . ?
N11 C23 C24 102.7(5) . . ?
N23 C23 H23 112.0 . . ?
N11 C23 H23 112.0 . . ?
C24 C23 H23 112.0 . . ?
C35 N24 C36 124.0(5) . . ?
C35 N24 C24 112.5(5) . . ?
C36 N24 C24 122.8(5) . . ?
C9 N9 C8 122.0(5) . . ?
C9 N9 C21 111.9(5) . . ?
C8 N9 C21 122.3(5) . . ?
C33 N22 C34 119.8(5) . . ?
C33 N22 C22 111.2(5) . . ?
C34 N22 C22 123.5(5) . . ?
C1 N2 C2 122.9(6) . . ?
C1 N2 C14 110.9(5) . . ?
C2 N2 C14 126.2(6) . . ?
N19 C19 N7 115.5(5) . . ?
N19 C19 C20 102.6(5) . . ?
N7 C19 C20 102.8(5) . . ?
N19 C19 H19 111.7 . . ?
N7 C19 H19 111.7 . . ?
C20 C19 H19 111.7 . . ?
C25 N13 C36 122.9(5) . . ?
C25 N13 C13 112.4(5) . . ?
C36 N13 C13 124.5(5) . . ?
C27 N16 C16 112.3(5) . . ?
C27 N16 C28 121.1(5) . . ?
C16 N16 C28 123.5(5) . . ?
N22 C34 N23 113.5(5) . . ?
N22 C34 H34A 108.9 . . ?
N23 C34 H34A 108.9 . . ?
N22 C34 H34B 108.9 . . ?
N23 C34 H34B 108.9 . . ?
H34A C34 H34B 107.7 . . ?
N21 C21 N9 116.4(5) . . ?
N21 C21 C22 103.2(5) . . ?
N9 C21 C22 102.9(5) . . ?
N21 C21 H21 111.3 . . ?
N9 C21 H21 111.3 . . ?
C22 C21 H21 111.3 . . ?
C29 N18 C18 112.9(5) . . ?
C29 N18 C30 123.2(6) . . ?
C18 N18 C30 123.8(6) . . ?
C5 N5 C4 122.2(5) . . ?
C5 N5 C17 112.5(5) . . ?
C4 N5 C17 123.2(5) . . ?
C11 N11 C10 122.3(5) . . ?
C11 N11 C23 112.9(5) . . ?
C10 N11 C23 123.1(5) . . ?
C27 N15 C15 112.8(5) . . ?
C27 N15 C26 122.1(5) . . ?
C15 N15 C26 124.9(5) . . ?
C5 N6 C6 121.5(5) . . ?
C5 N6 C18 111.5(5) . . ?
C6 N6 C18 123.0(5) . . ?
O4 C7 N8 125.2(6) . . ?
O4 C7 N7 126.2(6) . . ?
N8 C7 N7 108.5(5) . . ?
N20 C32 N21 113.3(5) . . ?
N20 C32 H32A 108.9 . . ?
N21 C32 H32A 108.9 . . ?
N20 C32 H32B 108.9 . . ?
N21 C32 H32B 108.9 . . ?
H32A C32 H32B 107.7 . . ?
N8 C8 N9 115.2(5) . . ?
N8 C8 H8A 108.5 . . ?
N9 C8 H8A 108.5 . . ?
N8 C8 H8B 108.5 . . ?
N9 C8 H8B 108.5 . . ?
H8A C8 H8B 107.5 . . ?
O7 C25 N14 126.4(6) . . ?
O7 C25 N13 126.0(6) . . ?
N14 C25 N13 107.6(5) . . ?
O10 C31 N19 125.4(6) . . ?
O10 C31 N20 126.2(6) . . ?
N19 C31 N20 108.3(5) . . ?
C1 N1 C12 122.2(5) . . ?
C1 N1 C13 112.5(5) . . ?
C12 N1 C13 123.0(5) . . ?
C11 N12 C12 123.9(5) . . ?
C11 N12 C24 112.1(5) . . ?
C12 N12 C24 121.3(5) . . ?
N13 C36 N24 114.8(5) . . ?
N13 C36 H36A 108.6 . . ?
N24 C36 H36A 108.6 . . ?
N13 C36 H36B 108.6 . . ?
N24 C36 H36B 108.6 . . ?
H36A C36 H36B 107.6 . . ?
C31 N20 C32 121.8(5) . . ?
C31 N20 C20 111.8(5) . . ?
C32 N20 C20 121.0(5) . . ?
O3 C5 N5 126.7(6) . . ?
O3 C5 N6 125.4(6) . . ?
N5 C5 N6 107.9(5) . . ?
N17 C17 N5 113.6(5) . . ?
N17 C17 C18 104.1(5) . . ?
N5 C17 C18 103.6(5) . . ?
N17 C17 H17 111.7 . . ?
N5 C17 H17 111.7 . . ?
C18 C17 H17 111.7 . . ?
N12 C24 N24 113.7(5) . . ?
N12 C24 C23 103.8(5) . . ?
N24 C24 C23 103.2(4) . . ?
N12 C24 H24 111.9 . . ?
N24 C24 H24 111.9 . . ?
C23 C24 H24 111.9 . . ?
N15 C26 N14 113.0(5) . . ?
N15 C26 H26A 109.0 . . ?
N14 C26 H26A 109.0 . . ?
N15 C26 H26B 109.0 . . ?
N14 C26 H26B 109.0 . . ?
H26A C26 H26B 107.8 . . ?
O1 C1 N1 125.9(6) . . ?
O1 C1 N2 124.4(6) . . ?
N1 C1 N2 109.6(5) . . ?
N13 C13 N1 114.6(5) . . ?
N13 C13 C14 103.5(5) . . ?
N1 C13 C14 103.0(5) . . ?
N13 C13 H13 111.7 . . ?
N1 C13 H13 111.7 . . ?
C14 C13 H13 111.7 . . ?
C29 N17 C28 122.2(5) . . ?
C29 N17 C17 111.3(5) . . ?
C28 N17 C17 124.1(5) . . ?
O6 C11 N11 126.8(6) . . ?
O6 C11 N12 125.0(6) . . ?
N11 C11 N12 108.3(5) . . ?
N15 C15 N3 114.5(5) . . ?
N15 C15 C16 103.0(5) . . ?
N3 C15 C16 103.1(5) . . ?
N15 C15 H15 111.9 . . ?
N3 C15 H15 111.9 . . ?
C16 C15 H15 111.9 . . ?
C7 N8 C8 123.4(5) . . ?
C7 N8 C20 112.8(5) . . ?
C8 N8 C20 123.4(5) . . ?
N6 C6 N7 114.0(5) . . ?
N6 C6 H6A 108.7 . . ?
N7 C6 H6A 108.7 . . ?
N6 C6 H6B 108.7 . . ?
N7 C6 H6B 108.7 . . ?
H6A C6 H6B 107.6 . . ?
O12 C35 N23 126.8(5) . . ?
O12 C35 N24 125.2(6) . . ?
N23 C35 N24 108.0(5) . . ?
N8 C20 N20 115.5(5) . . ?
N8 C20 C19 103.0(5) . . ?
N20 C20 C19 103.4(5) . . ?
N8 C20 H20 111.4 . . ?
N20 C20 H20 111.4 . . ?
C19 C20 H20 111.4 . . ?
O11 C33 N21 125.8(5) . . ?
O11 C33 N22 125.7(5) . . ?
N21 C33 N22 108.4(5) . . ?
N10 C22 N22 115.7(5) . . ?
N10 C22 C21 102.6(5) . . ?
N22 C22 C21 102.7(4) . . ?
N10 C22 H22 111.7 . . ?
N22 C22 H22 111.7 . . ?
C21 C22 H22 111.7 . . ?
N16 C16 N4 114.2(5) . . ?
N16 C16 C15 103.6(5) . . ?
N4 C16 C15 102.3(5) . . ?
N16 C16 H16 112.0 . . ?
N4 C16 H16 112.0 . . ?
C15 C16 H16 112.0 . . ?
C31 N19 C19 112.8(5) . . ?
C31 N19 C30 122.8(5) . . ?
C19 N19 C30 123.6(5) . . ?
O5 C9 N10 126.6(5) . . ?
O5 C9 N9 125.4(6) . . ?
N10 C9 N9 108.0(5) . . ?
C3 N3 C2 123.7(5) . . ?
C3 N3 C15 112.8(5) . . ?
C2 N3 C15 123.0(5) . . ?
O8 C27 N16 126.8(6) . . ?
O8 C27 N15 125.1(6) . . ?
N16 C27 N15 108.1(5) . . ?
C3 N4 C4 123.6(6) . . ?
C3 N4 C16 113.3(5) . . ?
C4 N4 C16 123.0(5) . . ?
O2 C3 N4 125.5(6) . . ?
O2 C3 N3 126.1(6) . . ?
N4 C3 N3 108.4(6) . . ?
N11 C10 N10 115.2(5) . . ?
N11 C10 H10A 108.5 . . ?
N10 C10 H10A 108.5 . . ?
N11 C10 H10B 108.5 . . ?
N10 C10 H10B 108.5 . . ?
H10A C10 H10B 107.5 . . ?
N18 C18 N6 114.7(5) . . ?
N18 C18 C17 103.2(5) . . ?
N6 C18 C17 103.7(5) . . ?
N18 C18 H18 111.6 . . ?
N6 C18 H18 111.6 . . ?
C17 C18 H18 111.6 . . ?
O9 C29 N18 126.7(6) . . ?
O9 C29 N17 125.3(7) . . ?
N18 C29 N17 107.9(5) . . ?
N14 C14 N2 114.4(5) . . ?
N14 C14 C13 103.4(5) . . ?
N2 C14 C13 103.5(5) . . ?
N14 C14 H14 111.6 . . ?
N2 C14 H14 111.6 . . ?
C13 C14 H14 111.6 . . ?
N5 C4 N4 113.6(5) . . ?
N5 C4 H4A 108.9 . . ?
N4 C4 H4A 108.9 . . ?
N5 C4 H4B 108.9 . . ?
N4 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
N18 C30 N19 114.2(5) . . ?
N18 C30 H30A 108.7 . . ?
N19 C30 H30A 108.7 . . ?
N18 C30 H30B 108.7 . . ?
N19 C30 H30B 108.7 . . ?
H30A C30 H30B 107.6 . . ?
N2 C2 N3 114.2(5) . . ?
N2 C2 H2A 108.7 . . ?
N3 C2 H2A 108.7 . . ?
N2 C2 H2B 108.7 . . ?
N3 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
N12 C12 N1 112.4(5) . . ?
N12 C12 H12A 109.1 . . ?
N1 C12 H12A 109.1 . . ?
N12 C12 H12B 109.1 . . ?
N1 C12 H12B 109.1 . . ?
H12A C12 H12B 107.8 . . ?
N17 C28 N16 113.5(5) . . ?
N17 C28 H28A 108.9 . . ?
N16 C28 H28A 108.9 . . ?
N17 C28 H28B 108.9 . . ?
N16 C28 H28B 108.9 . . ?
H28A C28 H28B 107.7 . . ?
C1X N1X H1X1 109.5 . . ?
C1X N1X H1X2 109.5 . . ?
H1X1 N1X H1X2 109.5 . . ?
C1X N1X H1X3 109.5 . . ?
H1X1 N1X H1X3 109.5 . . ?
H1X2 N1X H1X3 109.5 . . ?
C2X N2X C3X 119.3(18) . . ?
C2X N2X H2X 120.4 . . ?
C3X N2X H2X 120.4 . . ?
N1X C1X C2X 109.7(17) . . ?
N1X C1X H1XA 109.7 . . ?
C2X C1X H1XA 109.7 . . ?
N1X C1X H1XB 109.7 . . ?
C2X C1X H1XB 109.7 . . ?
H1XA C1X H1XB 108.2 . . ?
O1X C2X N2X 124(2) . . ?
O1X C2X C1X 121.8(17) . . ?
N2X C2X C1X 114.6(17) . . ?
N2X C3X C4X 109.4(13) . . ?
N2X C3X C5X 109.5(16) . . ?
C4X C3X C5X 111.1(17) . . ?
N2X C3X H3X 108.9 . . ?
C4X C3X H3X 108.9 . . ?
C5X C3X H3X 108.9 . . ?
O3X C4X O2X 126.3(17) . . ?
O3X C4X C3X 115.6(13) . . ?
O2X C4X C3X 117.0(14) . . ?
C6X C5X C3X 116.9(18) . . ?
C6X C5X H5X1 108.1 . . ?
C3X C5X H5X1 108.1 . . ?
C6X C5X H5X2 108.1 . . ?
C3X C5X H5X2 108.1 . . ?
H5X1 C5X H5X2 107.3 . . ?
C11X C6X C7X 117.4(16) . . ?
C11X C6X C5X 122.7(17) . . ?
C7X C6X C5X 119.9(16) . . ?
C6X C7X C8X 121.1(15) . . ?
C6X C7X H7X 119.5 . . ?
C8X C7X H7X 119.5 . . ?
C9X C8X C7X 121.5(16) . . ?
C9X C8X H8X 119.3 . . ?
C7X C8X H8X 119.3 . . ?
C8X C9X C10X 117.9(17) . . ?
C8X C9X O4X 112(2) . . ?
C10X C9X O4X 130(2) . . ?
C9X C10X C11X 120.8(16) . . ?
C9X C10X H10X 119.6 . . ?
C11X C10X H10X 119.6 . . ?
C6X C11X C10X 121.1(16) . . ?
C6X C11X H11X 119.4 . . ?
C10X C11X H11X 119.4 . . ?
C9X O4X H4X 109.5 . . ?
C1XA N1XA H1X4 109.5 . . ?
C1XA N1XA H1X5 109.5 . . ?
H1X4 N1XA H1X5 109.5 . . ?
C1XA N1XA H1X6 109.5 . . ?
H1X4 N1XA H1X6 109.5 . . ?
H1X5 N1XA H1X6 109.5 . . ?
C2XA N2XA C3XA 127.0(19) . . ?
C2XA N2XA H2XA 116.5 . . ?
C3XA N2XA H2XA 116.5 . . ?
N1XA C1XA C2XA 110.0(13) . . ?
N1XA C1XA H1XC 109.7 . . ?
C2XA C1XA H1XC 109.7 . . ?
N1XA C1XA H1XD 109.7 . . ?
C2XA C1XA H1XD 109.7 . . ?
H1XC C1XA H1XD 108.2 . . ?
O1XA C2XA N2XA 124.0(18) . . ?
O1XA C2XA C1XA 118.7(15) . . ?
N2XA C2XA C1XA 117.2(14) . . ?
N2XA C3XA C4XA 108.2(18) . . ?
N2XA C3XA C5XA 108.3(18) . . ?
C4XA C3XA C5XA 108(2) . . ?
N2XA C3XA H3XA 110.7 . . ?
C4XA C3XA H3XA 110.7 . . ?
C5XA C3XA H3XA 110.7 . . ?
O3XA C4XA O2XA 122(2) . . ?
O3XA C4XA C3XA 116(2) . . ?
O2XA C4XA C3XA 122(2) . . ?
C6XA C5XA C3XA 116(2) . . ?
C6XA C5XA H5X3 108.3 . . ?
C3XA C5XA H5X3 108.3 . . ?
C6XA C5XA H5X4 108.3 . . ?
C3XA C5XA H5X4 108.3 . . ?
H5X3 C5XA H5X4 107.4 . . ?
C111 C6XA C7XA 117(2) . . ?
C111 C6XA C5XA 122(3) . . ?
C7XA C6XA C5XA 120(2) . . ?
C6XA C7XA C8XA 122(2) . . ?
C6XA C7XA H7XA 118.8 . . ?
C8XA C7XA H7XA 118.8 . . ?
C9XA C8XA C7XA 119(2) . . ?
C9XA C8XA H8XA 120.4 . . ?
C7XA C8XA H8XA 120.4 . . ?
C101 C9XA C8XA 119.1(18) . . ?
C101 C9XA O4XA 123.8(17) . . ?
C8XA C9XA O4XA 117(2) . . ?
C9XA C101 C111 122(2) . . ?
C9XA C101 H101 119.1 . . ?
C111 C101 H101 119.1 . . ?
C6XA C111 C101 120(2) . . ?
C6XA C111 H111 120.2 . . ?
C101 C111 H111 120.2 . . ?
C9XA O4XA H4XA 109.5 . . ?

_refine_diff_density_max         0.612
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.078

_shelxl_version_number           2013-3

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_q6_cacl2_glygly2
_database_code_depnum_ccdc_archive 'CCDC 1548095'
_audit_update_record             
;
2017-05-05 deposited with the CCDC.
2017-06-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            'cucurbit[6]uril/Gly-Gly exclusion complex'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H26 Ca0.25 Cl0.5 N14 O18.38'
_chemical_formula_weight         808.31

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'
O O 0.0106 0.0060 '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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z'
'-y+3/4, x+1/4, z+1/4'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-1/4'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   31.3154(5)
_cell_length_b                   31.3154(5)
_cell_length_c                   14.3835(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     14105.4(5)
_cell_formula_units_Z            16
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7476
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      26.37

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_F_000             6664
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.750
_exptl_crystal_size_mid          0.650
_exptl_crystal_size_min          0.550
_exptl_absorpt_coefficient_mu    0.204
_shelx_estimated_absorpt_T_min   0.862
_shelx_estimated_absorpt_T_max   0.896
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  KappaApexII
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            13959
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.602
_diffrn_reflns_theta_max         26.352
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             7167
_reflns_number_gt                5876
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
'Collect data collection software (Nonius B.V., 1998)'
_computing_cell_refinement       'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_data_reduction        'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1188P)²+50.3020P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7167
_refine_ls_number_parameters     673
_refine_ls_number_restraints     216
_refine_ls_R_factor_all          0.0906
_refine_ls_R_factor_gt           0.0769
_refine_ls_wR_factor_ref         0.2234
_refine_ls_wR_factor_gt          0.2081
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.5000 0.7500 0.1250 0.0444(4) Uani 1 4 d S T P . .
O5 O 0.73648(7) 0.78857(7) 0.07292(15) 0.0319(5) Uani 1 1 d . . . . .
O2 O 0.64995(7) 0.85876(7) -0.27481(15) 0.0335(5) Uani 1 1 d . . . . .
O3 O 0.74278(7) 0.88447(7) -0.36075(15) 0.0343(5) Uani 1 1 d . . . . .
O1 O 0.61524(8) 0.76230(8) -0.33218(16) 0.0368(5) Uani 1 1 d . . . . .
O4 O 0.69993(8) 0.68612(7) 0.00457(16) 0.0387(6) Uani 1 1 d . . . . .
O6 O 0.83139(7) 0.81576(8) -0.01307(16) 0.0356(5) Uani 1 1 d . . . . .
N9 N 0.72093(8) 0.85037(8) -0.00802(17) 0.0269(5) Uani 1 1 d . . . . .
N5 N 0.80931(8) 0.88117(9) -0.29176(17) 0.0302(6) Uani 1 1 d . . . . .
N3 N 0.68317(8) 0.88156(9) -0.14034(17) 0.0300(6) Uani 1 1 d . . . . .
N6 N 0.65167(8) 0.66861(9) -0.11032(18) 0.0308(6) Uani 1 1 d . . . . .
N1 N 0.60776(9) 0.76044(9) -0.17259(19) 0.0348(6) Uani 1 1 d . . . . .
N12 N 0.61753(8) 0.69986(9) -0.24775(18) 0.0310(6) Uani 1 1 d . . . . .
N11 N 0.84191(8) 0.84843(8) -0.15554(18) 0.0279(5) Uani 1 1 d . . . . .
N10 N 0.79088(8) 0.87316(8) -0.06196(18) 0.0293(6) Uani 1 1 d . . . . .
N4 N 0.75345(8) 0.89561(8) -0.20332(17) 0.0283(5) Uani 1 1 d . . . . .
N8 N 0.67044(8) 0.80131(9) 0.00746(17) 0.0303(6) Uani 1 1 d . . . . .
N7 N 0.64496(9) 0.73128(9) -0.03900(18) 0.0332(6) Uani 1 1 d . . . . .
C15 C 0.71185(9) 0.81095(10) 0.02795(19) 0.0265(6) Uani 1 1 d . . . . .
N2 N 0.63541(8) 0.82968(9) -0.13076(17) 0.0308(6) Uani 1 1 d . . . . .
C18 C 0.61692(10) 0.67039(10) -0.3251(2) 0.0311(7) Uani 1 1 d . . . . .
H18A H 0.5962 0.6473 -0.3116 0.037 Uiso 1 1 calc R U . . .
H18B H 0.6069 0.6857 -0.3813 0.037 Uiso 1 1 calc R U . . .
C2 C 0.65575(9) 0.85655(10) -0.1905(2) 0.0292(6) Uani 1 1 d . . . . .
C17 C 0.82223(10) 0.84292(10) -0.0714(2) 0.0295(6) Uani 1 1 d . . . . .
C10 C 0.78909(10) 0.90157(10) -0.1411(2) 0.0289(6) Uani 1 1 d . . . . .
H10 H 0.7917 0.9321 -0.1215 0.035 Uiso 1 1 calc R U . . .
C11 C 0.82788(10) 0.88745(10) -0.2005(2) 0.0288(6) Uani 1 1 d . . . . .
H11 H 0.8509 0.9096 -0.2014 0.035 Uiso 1 1 calc R U . . .
C16 C 0.76039(10) 0.87299(11) 0.0133(2) 0.0306(6) Uani 1 1 d . . . . .
H16A H 0.7534 0.9029 0.0297 0.037 Uiso 1 1 calc R U . . .
H16B H 0.7738 0.8596 0.0684 0.037 Uiso 1 1 calc R U . . .
C12 C 0.83443(10) 0.87478(10) -0.3751(2) 0.0317(7) Uani 1 1 d . . . . .
H12A H 0.8173 0.8839 -0.4295 0.038 Uiso 1 1 calc R U . . .
H12B H 0.8599 0.8935 -0.3721 0.038 Uiso 1 1 calc R U . . .
C8 C 0.64819(9) 0.83648(10) -0.0348(2) 0.0293(6) Uani 1 1 d . . . . .
H8 H 0.6236 0.8462 0.0043 0.035 Uiso 1 1 calc R U . . .
C3 C 0.76649(10) 0.88654(9) -0.2918(2) 0.0293(6) Uani 1 1 d . . . . .
C14 C 0.65002(11) 0.76185(11) 0.0354(2) 0.0345(7) Uani 1 1 d . . . . .
H14A H 0.6671 0.7486 0.0855 0.041 Uiso 1 1 calc R U . . .
H14B H 0.6215 0.7686 0.0613 0.041 Uiso 1 1 calc R U . . .
C9 C 0.68303(9) 0.87153(10) -0.0425(2) 0.0270(6) Uani 1 1 d . . . . .
H9 H 0.6757 0.8971 -0.0040 0.032 Uiso 1 1 calc R U . . .
C4 C 0.59860(10) 0.80515(11) -0.1589(2) 0.0343(7) Uani 1 1 d . . . . .
H4A H 0.5761 0.8080 -0.1109 0.041 Uiso 1 1 calc R U . . .
H4B H 0.5872 0.8172 -0.2176 0.041 Uiso 1 1 calc R U . . .
C5 C 0.71124(10) 0.91199(10) -0.1835(2) 0.0312(7) Uani 1 1 d . . . . .
H5A H 0.7140 0.9371 -0.1423 0.037 Uiso 1 1 calc R U . . .
H5B H 0.6981 0.9218 -0.2424 0.037 Uiso 1 1 calc R U . . .
C13 C 0.66874(10) 0.69457(10) -0.0440(2) 0.0316(7) Uani 1 1 d . . . . .
C7 C 0.60794(10) 0.72939(11) -0.0990(2) 0.0333(7) Uani 1 1 d . . . . .
H7 H 0.5808 0.7302 -0.0624 0.040 Uiso 1 1 calc R U . . .
C1 C 0.61376(9) 0.74278(11) -0.2584(2) 0.0299(6) Uani 1 1 d . . . . .
C6 C 0.61317(10) 0.68641(11) -0.1512(2) 0.0317(7) Uani 1 1 d . . . . .
H6 H 0.5879 0.6673 -0.1420 0.038 Uiso 1 1 calc R U . . .
C4A C 0.47384(12) 0.95876(12) -0.2926(2) 0.0375(7) Uani 1 1 d G . . . .
H4A1 H 0.4783 0.9911 -0.2831 0.045 Uiso 0.742(3) 1 d G U P A .
H4A2 H 0.5032 0.9452 -0.3064 0.045 Uiso 0.742(3) 1 d G U P A .
H4AA H 0.4852 0.9897 -0.2928 0.045 Uiso 0.258(3) 1 d G U P A .
H4AB H 0.4996 0.9382 -0.2963 0.045 Uiso 0.258(3) 1 d G U P A .
N2A N 0.44893(10) 0.94987(11) -0.3760(2) 0.0415(7) Uani 1 1 d G . . . .
H2A1 H 0.4462 0.9240 -0.3837 0.062 Uiso 0.742(3) 1 d G U P . .
H2A2 H 0.4601 0.9605 -0.4224 0.062 Uiso 0.742(3) 1 d G U P . .
H2A3 H 0.4253 0.9608 -0.3677 0.062 Uiso 0.742(3) 1 d G U P . .
H2AA H 0.4474 0.9240 -0.3857 0.062 Uiso 0.258(3) 1 d G U P . .
H2AB H 0.4593 0.9618 -0.4217 0.062 Uiso 0.258(3) 1 d G U P . .
H2AC H 0.4249 0.9594 -0.3663 0.062 Uiso 0.258(3) 1 d G U P . .
O1A O 0.48820(14) 0.86604(12) -0.0559(3) 0.0578(11) Uani 0.742(3) 1 d D U P A 1
C1A C 0.4589(3) 0.8870(2) -0.0233(5) 0.0344(15) Uani 0.742(3) 1 d D U P A 1
O2A O 0.42956(11) 0.87141(11) 0.0300(2) 0.0412(8) Uani 0.742(3) 1 d D U P A 1
C2A C 0.45549(17) 0.93477(17) -0.0403(3) 0.0372(10) Uani 0.742(3) 1 d D U P A 1
H2A5 H 0.4250 0.9431 -0.0397 0.045 Uiso 0.742(3) 1 calc R U P A 1
H2A6 H 0.4699 0.9501 0.0110 0.045 Uiso 0.742(3) 1 calc R U P A 1
N1A N 0.47427(16) 0.94786(16) -0.1278(3) 0.0343(10) Uani 0.742(3) 1 d D U P A 1
H1A H 0.4989 0.9615 -0.1282 0.041 Uiso 0.742(3) 1 calc R U P A 1
C3A C 0.4546(2) 0.9395(2) -0.2071(5) 0.0290(16) Uani 0.742(3) 1 d D U P A 1
O3A O 0.4212(2) 0.9183(2) -0.2116(7) 0.0392(14) Uani 0.742(3) 1 d D U P A 1
O1W O 0.36017(13) 0.91791(12) 0.0817(2) 0.0455(9) Uani 0.742(3) 1 d . . P A 1
O2W O 0.65695(14) 0.51347(14) 0.9671(3) 0.0541(10) Uani 0.742(3) 1 d . . P A 1
O4W O 0.72989(16) 0.93294(15) 0.4741(3) 0.0562(11) Uani 0.742(3) 1 d . . P A 1
O7W O 0.76064(18) 1.01489(17) 0.4953(6) 0.102(2) Uani 0.742(3) 1 d . . P A 1
O11W O 0.34646(15) 0.81852(14) 0.3226(3) 0.0635(12) Uani 0.742(3) 1 d . . P A 1
O9W O 0.43729(12) 0.79606(13) 0.1167(3) 0.0541(10) Uani 0.742(3) 1 d . . P A 1
O10W O 0.4692(2) 0.7512(2) 0.2778(4) 0.0354(14) Uani 0.3708(17) 1 d . . P A 1
O8W O 0.5006(4) 0.7641(3) 0.4383(6) 0.062(2) Uani 0.3708(17) 1 d . . P A 1
O5W O 0.57973(16) 0.75968(17) 0.4921(3) 0.0692(13) Uani 0.742(3) 1 d . . P A 1
O3W O 0.39361(12) 1.05546(13) -0.0784(3) 0.0497(9) Uani 0.742(3) 1 d . . P A 1
Cl1 Cl 0.5114(3) 0.97992(13) -0.5141(5) 0.105(2) Uani 0.3708(17) 1 d . . P A 1
O1A1 O 0.4651(10) 0.8857(9) -0.026(2) 0.102(8) Uani 0.258(3) 1 d D U P A 2
C1A1 C 0.4371(5) 0.9121(6) -0.0078(12) 0.060(4) Uani 0.258(3) 1 d D U P A 2
O2A1 O 0.4061(5) 0.9035(5) 0.0490(9) 0.072(4) Uani 0.258(3) 1 d D U P A 2
C2A1 C 0.4400(7) 0.9583(6) -0.0379(11) 0.061(4) Uani 0.258(3) 1 d D U P A 2
H2A7 H 0.4107 0.9702 -0.0422 0.073 Uiso 0.258(3) 1 calc R U P A 2
H2A4 H 0.4555 0.9747 0.0104 0.073 Uiso 0.258(3) 1 calc R U P A 2
N1A1 N 0.4614(6) 0.9643(6) -0.1266(10) 0.054(4) Uani 0.258(3) 1 d D U P A 2
H1A1 H 0.4860 0.9780 -0.1279 0.065 Uiso 0.258(3) 1 calc R U P A 2
C3A1 C 0.4451(7) 0.9500(8) -0.2052(14) 0.037(5) Uani 0.258(3) 1 d D U P A 2
O3A1 O 0.4107(7) 0.9310(7) -0.210(2) 0.056(6) Uani 0.258(3) 1 d D U P A 2
O1W1 O 0.3357(5) 0.9451(7) 0.0834(9) 0.088(5) Uani 0.258(3) 1 d . . P A 2
O12W O 0.3867(5) 0.8282(5) 0.1083(11) 0.080(4) Uiso 0.258(3) 1 d . . P A 2
O2WA O 0.6679(10) 0.4856(10) 0.967(3) 0.204(18) Uani 0.258(3) 1 d . . P A 2
O4W1 O 0.7491(6) 0.9164(10) 0.4608(14) 0.128(10) Uani 0.258(3) 1 d . . P A 2
O7W1 O 0.7500(4) 0.9964(4) 0.4678(9) 0.050(3) Uiso 0.258(3) 1 d . . P A 2
O11A O 0.3701(3) 0.8060(3) 0.2381(7) 0.040(2) Uani 0.258(3) 1 d . . P A 2
O10A O 0.4482(4) 0.7293(4) 0.2484(8) 0.056(3) Uani 0.258(3) 1 d . . P A 2
O5WA O 0.6173(6) 0.7570(5) 0.4628(11) 0.088(5) Uani 0.258(3) 1 d . . P A 2
O8WA O 0.5327(6) 0.7578(6) 0.4374(15) 0.041(5) Uani 0.1292(17) 1 d . . P A 2
O9WA O 0.4444(3) 0.7808(3) 0.1989(7) 0.046(3) Uani 0.258(3) 1 d . . P A 2
O3WA O 0.4157(15) 1.0378(15) -0.063(3) 0.224(18) Uiso 0.258(3) 1 d . . P A 2
Cl1A Cl 0.4814(5) 0.9893(7) -0.5425(9) 0.089(5) Uani 0.1292(17) 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Ca1 O9WA 2.256(10) 2_665 ?
Ca1 O9WA 2.256(10) . ?
Ca1 O9WA 2.256(10) 16_655 ?
Ca1 O9WA 2.256(10) 15_565 ?
Ca1 O10W 2.401(6) . ?
Ca1 O10W 2.401(6) 2_665 ?
Ca1 O10W 2.401(6) 16_655 ?
Ca1 O10W 2.401(6) 15_565 ?
Ca1 O9W 2.440(4) 15_565 ?
Ca1 O9W 2.440(4) 16_655 ?
Ca1 O9W 2.440(4) 2_665 ?
Ca1 O9W 2.440(4) . ?
O5 C15 1.227(4) . ?
O2 C2 1.228(4) . ?
O3 C3 1.241(4) . ?
O1 C1 1.226(4) . ?
O4 C13 1.230(4) . ?
O6 C17 1.229(4) . ?
N9 C15 1.368(4) . ?
N9 C9 1.447(4) . ?
N9 C16 1.457(4) . ?
N5 C3 1.351(4) . ?
N5 C12 1.448(4) . ?
N5 C11 1.449(4) . ?
N3 C2 1.368(4) . ?
N3 C5 1.438(4) . ?
N3 C9 1.442(4) . ?
N6 C13 1.363(4) . ?
N6 C12 1.442(4) 13_664 ?
N6 C6 1.452(4) . ?
N1 C1 1.365(4) . ?
N1 C7 1.437(4) . ?
N1 C4 1.443(4) . ?
N12 C1 1.358(4) . ?
N12 C18 1.446(4) . ?
N12 C6 1.458(4) . ?
N11 C17 1.369(4) . ?
N11 C18 1.444(4) 13_664 ?
N11 C11 1.451(4) . ?
N10 C17 1.371(4) . ?
N10 C16 1.444(4) . ?
N10 C10 1.446(4) . ?
N4 C3 1.367(4) . ?
N4 C10 1.443(4) . ?
N4 C5 1.446(4) . ?
N8 C15 1.364(4) . ?
N8 C8 1.438(4) . ?
N8 C14 1.448(4) . ?
N7 C13 1.372(4) . ?
N7 C14 1.444(4) . ?
N7 C7 1.446(4) . ?
N2 C2 1.361(4) . ?
N2 C4 1.444(4) . ?
N2 C8 1.452(4) . ?
C18 N11 1.444(4) 13_664 ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C10 C11 1.550(4) . ?
C10 H10 1.0000 . ?
C11 H11 1.0000 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C12 N6 1.442(4) 13_664 ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C8 C9 1.552(4) . ?
C8 H8 1.0000 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C9 H9 1.0000 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C7 C6 1.550(5) . ?
C7 H7 1.0000 . ?
C6 H6 1.0000 . ?
C4A N2A 1.457(4) . ?
C4A C3A 1.496(9) . ?
C4A C3A1 1.57(2) . ?
C4A H4A1 1.0321 . ?
C4A H4A2 1.0321 . ?
C4A H4AA 1.0320 . ?
C4A H4AB 1.0320 . ?
N2A H2A1 0.8231 . ?
N2A H2A2 0.8231 . ?
N2A H2A3 0.8231 . ?
N2A H2AA 0.8231 . ?
N2A H2AB 0.8230 . ?
N2A H2AC 0.8230 . ?
O1A C1A 1.223(10) . ?
C1A O2A 1.291(8) . ?
C1A C2A 1.520(9) . ?
C2A N1A 1.448(6) . ?
C2A H2A5 0.9900 . ?
C2A H2A6 0.9900 . ?
N1A C3A 1.323(7) . ?
N1A H1A 0.8800 . ?
C3A O3A 1.240(7) . ?
O8W O8W 0.884(16) 2_665 ?
Cl1 Cl1 1.501(8) 9_674 ?
O1A1 C1A1 1.23(2) . ?
C1A1 O2A1 1.298(16) . ?
C1A1 C2A1 1.514(17) . ?
C2A1 N1A1 1.454(15) . ?
C2A1 H2A7 0.9900 . ?
C2A1 H2A4 0.9900 . ?
N1A1 C3A1 1.319(15) . ?
N1A1 H1A1 0.8800 . ?
C3A1 O3A1 1.234(16) . ?
O10A O9WA 1.765(15) . ?
Cl1A Cl1A 1.82(3) 9_674 ?

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
O9WA Ca1 O9WA 123.8(6) 2_665 . ?
O9WA Ca1 O9WA 102.8(2) 2_665 16_655 ?
O9WA Ca1 O9WA 102.8(2) . 16_655 ?
O9WA Ca1 O9WA 102.8(2) 2_665 15_565 ?
O9WA Ca1 O9WA 102.8(2) . 15_565 ?
O9WA Ca1 O9WA 123.7(6) 16_655 15_565 ?
O10W Ca1 O10W 47.4(3) . 2_665 ?
O10W Ca1 O10W 147.0(2) . 16_655 ?
O10W Ca1 O10W 147.0(2) 2_665 16_655 ?
O10W Ca1 O10W 147.0(2) . 15_565 ?
O10W Ca1 O10W 147.0(2) 2_665 15_565 ?
O10W Ca1 O10W 47.4(3) 16_655 15_565 ?
O10W Ca1 O9W 100.37(19) . 15_565 ?
O10W Ca1 O9W 74.39(18) 2_665 15_565 ?
O10W Ca1 O9W 112.16(19) 16_655 15_565 ?
O10W Ca1 O9W 73.25(19) 15_565 15_565 ?
O10W Ca1 O9W 74.39(18) . 16_655 ?
O10W Ca1 O9W 100.38(19) 2_665 16_655 ?
O10W Ca1 O9W 73.25(19) 16_655 16_655 ?
O10W Ca1 O9W 112.16(19) 15_565 16_655 ?
O9W Ca1 O9W 174.43(19) 15_565 16_655 ?
O10W Ca1 O9W 112.17(19) . 2_665 ?
O10W Ca1 O9W 73.26(19) 2_665 2_665 ?
O10W Ca1 O9W 74.38(18) 16_655 2_665 ?
O10W Ca1 O9W 100.37(19) 15_565 2_665 ?
O9W Ca1 O9W 90.136(11) 15_565 2_665 ?
O9W Ca1 O9W 90.136(10) 16_655 2_665 ?
O10W Ca1 O9W 73.26(19) . . ?
O10W Ca1 O9W 112.17(19) 2_665 . ?
O10W Ca1 O9W 100.37(19) 16_655 . ?
O10W Ca1 O9W 74.38(18) 15_565 . ?
O9W Ca1 O9W 90.133(10) 15_565 . ?
O9W Ca1 O9W 90.138(11) 16_655 . ?
O9W Ca1 O9W 174.41(19) 2_665 . ?
C15 N9 C9 111.8(2) . . ?
C15 N9 C16 122.4(3) . . ?
C9 N9 C16 123.0(3) . . ?
C3 N5 C12 123.8(3) . . ?
C3 N5 C11 112.5(2) . . ?
C12 N5 C11 123.4(3) . . ?
C2 N3 C5 122.4(3) . . ?
C2 N3 C9 112.8(3) . . ?
C5 N3 C9 124.6(3) . . ?
C13 N6 C12 123.0(3) . 13_664 ?
C13 N6 C6 112.3(3) . . ?
C12 N6 C6 123.6(3) 13_664 . ?
C1 N1 C7 113.0(3) . . ?
C1 N1 C4 122.9(3) . . ?
C7 N1 C4 123.8(3) . . ?
C1 N12 C18 123.0(3) . . ?
C1 N12 C6 112.6(3) . . ?
C18 N12 C6 123.2(3) . . ?
C17 N11 C18 121.4(3) . 13_664 ?
C17 N11 C11 111.3(2) . . ?
C18 N11 C11 121.9(2) 13_664 . ?
C17 N10 C16 123.1(3) . . ?
C17 N10 C10 112.0(2) . . ?
C16 N10 C10 124.5(3) . . ?
C3 N4 C10 111.9(3) . . ?
C3 N4 C5 122.0(3) . . ?
C10 N4 C5 122.6(2) . . ?
C15 N8 C8 112.5(3) . . ?
C15 N8 C14 123.3(3) . . ?
C8 N8 C14 123.8(3) . . ?
C13 N7 C14 122.3(3) . . ?
C13 N7 C7 111.7(3) . . ?
C14 N7 C7 123.9(3) . . ?
O5 C15 N8 125.8(3) . . ?
O5 C15 N9 125.7(3) . . ?
N8 C15 N9 108.4(3) . . ?
C2 N2 C4 121.7(3) . . ?
C2 N2 C8 112.4(3) . . ?
C4 N2 C8 124.4(3) . . ?
N11 C18 N12 113.4(2) 13_664 . ?
N11 C18 H18A 108.9 13_664 . ?
N12 C18 H18A 108.9 . . ?
N11 C18 H18B 108.9 13_664 . ?
N12 C18 H18B 108.9 . . ?
H18A C18 H18B 107.7 . . ?
O2 C2 N2 126.1(3) . . ?
O2 C2 N3 125.6(3) . . ?
N2 C2 N3 108.3(3) . . ?
O6 C17 N11 125.9(3) . . ?
O6 C17 N10 125.2(3) . . ?
N11 C17 N10 108.9(3) . . ?
N4 C10 N10 116.0(2) . . ?
N4 C10 C11 103.1(2) . . ?
N10 C10 C11 103.2(2) . . ?
N4 C10 H10 111.3 . . ?
N10 C10 H10 111.3 . . ?
C11 C10 H10 111.3 . . ?
N5 C11 N11 114.3(2) . . ?
N5 C11 C10 102.9(2) . . ?
N11 C11 C10 103.4(2) . . ?
N5 C11 H11 111.9 . . ?
N11 C11 H11 111.9 . . ?
C10 C11 H11 111.9 . . ?
N10 C16 N9 113.9(2) . . ?
N10 C16 H16A 108.8 . . ?
N9 C16 H16A 108.8 . . ?
N10 C16 H16B 108.8 . . ?
N9 C16 H16B 108.8 . . ?
H16A C16 H16B 107.7 . . ?
N6 C12 N5 114.5(3) 13_664 . ?
N6 C12 H12A 108.6 13_664 . ?
N5 C12 H12A 108.6 . . ?
N6 C12 H12B 108.6 13_664 . ?
N5 C12 H12B 108.6 . . ?
H12A C12 H12B 107.6 . . ?
N8 C8 N2 115.0(3) . . ?
N8 C8 C9 103.3(2) . . ?
N2 C8 C9 103.3(2) . . ?
N8 C8 H8 111.5 . . ?
N2 C8 H8 111.5 . . ?
C9 C8 H8 111.5 . . ?
O3 C3 N5 126.0(3) . . ?
O3 C3 N4 125.2(3) . . ?
N5 C3 N4 108.8(3) . . ?
N7 C14 N8 114.1(3) . . ?
N7 C14 H14A 108.7 . . ?
N8 C14 H14A 108.7 . . ?
N7 C14 H14B 108.7 . . ?
N8 C14 H14B 108.7 . . ?
H14A C14 H14B 107.6 . . ?
N3 C9 N9 115.6(2) . . ?
N3 C9 C8 103.0(2) . . ?
N9 C9 C8 103.2(2) . . ?
N3 C9 H9 111.5 . . ?
N9 C9 H9 111.5 . . ?
C8 C9 H9 111.5 . . ?
N1 C4 N2 113.3(3) . . ?
N1 C4 H4A 108.9 . . ?
N2 C4 H4A 108.9 . . ?
N1 C4 H4B 108.9 . . ?
N2 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
N3 C5 N4 114.1(3) . . ?
N3 C5 H5A 108.7 . . ?
N4 C5 H5A 108.7 . . ?
N3 C5 H5B 108.7 . . ?
N4 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
O4 C13 N6 125.5(3) . . ?
O4 C13 N7 125.6(3) . . ?
N6 C13 N7 108.9(3) . . ?
N1 C7 N7 114.5(3) . . ?
N1 C7 C6 103.4(2) . . ?
N7 C7 C6 103.9(3) . . ?
N1 C7 H7 111.5 . . ?
N7 C7 H7 111.5 . . ?
C6 C7 H7 111.5 . . ?
O1 C1 N12 126.0(3) . . ?
O1 C1 N1 125.9(3) . . ?
N12 C1 N1 108.2(3) . . ?
N6 C6 N12 114.7(2) . . ?
N6 C6 C7 103.0(2) . . ?
N12 C6 C7 102.7(3) . . ?
N6 C6 H6 111.9 . . ?
N12 C6 H6 111.9 . . ?
C7 C6 H6 111.9 . . ?
N2A C4A C3A 112.6(4) . . ?
N2A C4A C3A1 108.6(8) . . ?
N2A C4A H4A1 111.7 . . ?
C3A C4A H4A1 110.0 . . ?
C3A1 C4A H4A1 98.2 . . ?
N2A C4A H4A2 103.9 . . ?
C3A C4A H4A2 110.5 . . ?
C3A1 C4A H4A2 126.3 . . ?
H4A1 C4A H4A2 107.9 . . ?
N2A C4A H4AA 111.2 . . ?
C3A C4A H4AA 121.3 . . ?
C3A1 C4A H4AA 111.3 . . ?
H4A1 C4A H4AA 14.5 . . ?
H4A2 C4A H4AA 94.4 . . ?
N2A C4A H4AB 104.9 . . ?
C3A C4A H4AB 96.0 . . ?
C3A1 C4A H4AB 112.3 . . ?
H4A1 C4A H4AB 120.8 . . ?
H4A2 C4A H4AB 16.0 . . ?
H4AA C4A H4AB 108.3 . . ?
C4A N2A H2A1 110.8 . . ?
C4A N2A H2A2 111.2 . . ?
H2A1 N2A H2A2 109.5 . . ?
C4A N2A H2A3 106.3 . . ?
H2A1 N2A H2A3 109.5 . . ?
H2A2 N2A H2A3 109.5 . . ?
C4A N2A H2AA 111.0 . . ?
H2A1 N2A H2AA 3.4 . . ?
H2A2 N2A H2AA 106.5 . . ?
H2A3 N2A H2AA 112.4 . . ?
C4A N2A H2AB 111.0 . . ?
H2A1 N2A H2AB 112.4 . . ?
H2A2 N2A H2AB 3.4 . . ?
H2A3 N2A H2AB 106.5 . . ?
H2AA N2A H2AB 109.5 . . ?
C4A N2A H2AC 106.3 . . ?
H2A1 N2A H2AC 106.5 . . ?
H2A2 N2A H2AC 112.4 . . ?
H2A3 N2A H2AC 3.4 . . ?
H2AA N2A H2AC 109.5 . . ?
H2AB N2A H2AC 109.5 . . ?
O1A C1A O2A 124.0(6) . . ?
O1A C1A C2A 121.2(6) . . ?
O2A C1A C2A 114.7(6) . . ?
N1A C2A C1A 113.0(5) . . ?
N1A C2A H2A5 109.0 . . ?
C1A C2A H2A5 109.0 . . ?
N1A C2A H2A6 109.0 . . ?
C1A C2A H2A6 109.0 . . ?
H2A5 C2A H2A6 107.8 . . ?
C3A N1A C2A 120.3(5) . . ?
C3A N1A H1A 119.9 . . ?
C2A N1A H1A 119.9 . . ?
O3A C3A N1A 122.9(8) . . ?
O3A C3A C4A 120.8(7) . . ?
N1A C3A C4A 116.2(6) . . ?
O1A1 C1A1 O2A1 122(2) . . ?
O1A1 C1A1 C2A1 123(2) . . ?
O2A1 C1A1 C2A1 115.0(14) . . ?
N1A1 C2A1 C1A1 113.7(15) . . ?
N1A1 C2A1 H2A7 108.8 . . ?
C1A1 C2A1 H2A7 108.8 . . ?
N1A1 C2A1 H2A4 108.8 . . ?
C1A1 C2A1 H2A4 108.8 . . ?
H2A7 C2A1 H2A4 107.7 . . ?
C3A1 N1A1 C2A1 122.0(16) . . ?
C3A1 N1A1 H1A1 119.0 . . ?
C2A1 N1A1 H1A1 119.0 . . ?
O3A1 C3A1 N1A1 123(2) . . ?
O3A1 C3A1 C4A 123(2) . . ?
N1A1 C3A1 C4A 113.9(17) . . ?
O9WA O10A Ca1 61.2(4) . . ?
O10A O9WA Ca1 75.4(5) . . ?

_refine_diff_density_max         1.183
_refine_diff_density_min         -1.099
_refine_diff_density_rms         0.087

_shelxl_version_number           2013-3

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_q6_glytrp_lepszy
_database_code_depnum_ccdc_archive 'CCDC 1548096'
_audit_update_record             
;
2017-05-05 deposited with the CCDC.
2017-06-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            'cucurbit[6]uril/Gly-Trp exclusion complex'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C49 H51 N27 O27.50'
_chemical_formula_weight         1458.17

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   12.6736(2)
_cell_length_b                   15.6598(2)
_cell_length_c                   16.4846(3)
_cell_angle_alpha                90
_cell_angle_beta                 108.761(2)
_cell_angle_gamma                90
_cell_volume                     3097.81(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    100.0(1)
_cell_measurement_reflns_used    13787
_cell_measurement_theta_min      3.68
_cell_measurement_theta_max      71.76

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_F_000             1508
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    1.128
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.778
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           ?
_diffrn_ambient_temperature      100.0(1)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 16.3
_diffrn_reflns_number            21272
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.683
_diffrn_reflns_theta_max         71.914
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11900
_reflns_number_gt                11327
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.902
_reflns_Friedel_fraction_max     0.965
_reflns_Friedel_fraction_full    0.998

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1322P)²+1.5274P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 5102 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.27(19)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         11900
_refine_ls_number_parameters     1182
_refine_ls_number_restraints     321
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0647
_refine_ls_wR_factor_ref         0.1820
_refine_ls_wR_factor_gt          0.1792
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1W O 0.1562(4) 0.3515(3) -0.1307(3) 0.0428(9) Uani 1 1 d . . . . .
O2W O 0.3225(4) 0.4993(3) 0.3082(3) 0.0559(12) Uani 1 1 d . . . . .
O3W O 0.4333(4) 0.8518(3) -0.0803(3) 0.0466(10) Uani 1 1 d . . . . .
O4W O 0.2952(9) 0.7146(6) -0.0925(6) 0.123(4) Uani 1 1 d . . . . .
O7W O 0.733(3) 0.8423(8) 0.2635(8) 0.074(7) Uani 0.57(5) 1 d . . P A 1
O7WA O 0.666(3) 0.8493(13) 0.2654(18) 0.106(9) Uani 0.43(5) 1 d . . P A 2
O9WA O 0.413(2) 0.4360(16) 0.4849(13) 0.138(9) Uani 0.473(7) 1 d . . P B 1
O8WA O 0.3327(17) 1.2152(11) -0.3585(11) 0.098(5) Uani 0.473(7) 1 d . . P B 1
O14A O 0.3604(14) 1.2653(9) -0.5150(10) 0.082(4) Uani 0.473(7) 1 d . . P B 1
O6W O 0.1141(11) 0.2011(7) -0.2167(8) 0.066(3) Uani 0.473(7) 1 d . . P B 1
O13W O 0.1168(13) 1.2008(11) -0.3818(10) 0.089(4) Uani 0.473(7) 1 d . . P B 1
O5WA O -0.060(4) 0.5834(18) -0.494(2) 0.153(17) Uani 0.473(7) 1 d . . P B 1
O12A O 0.2072(16) 0.4668(9) -0.4709(9) 0.090(5) Uani 0.473(7) 1 d . . P B 1
O15W O 0.0793(14) 0.3697(10) -0.4152(10) 0.098(5) Uani 0.473(7) 1 d . . P B 1
C8X C -0.356(2) 0.2311(14) -0.392(2) 0.032(4) Uani 0.473(7) 1 d D U P B 1
C9X C -0.3577(13) 0.1505(7) -0.4258(9) 0.051(3) Uani 0.473(7) 1 d D U P B 1
H9X H -0.4247 0.1202 -0.4529 0.061 Uiso 0.473(7) 1 calc R U P B 1
C10X C -0.2528(14) 0.1176(11) -0.4169(12) 0.057(4) Uani 0.473(7) 1 d D U P B 1
H10X H -0.2476 0.0613 -0.4365 0.069 Uiso 0.473(7) 1 calc R U P B 1
C11X C -0.1546(19) 0.1638(11) -0.380(2) 0.055(4) Uani 0.473(7) 1 d D U P B 1
H11X H -0.0848 0.1392 -0.3771 0.066 Uiso 0.473(7) 1 calc R U P B 1
C12X C -0.1586(11) 0.2447(9) -0.3489(8) 0.043(3) Uani 0.473(7) 1 d D U P B 1
H12X H -0.0919 0.2752 -0.3214 0.052 Uiso 0.473(7) 1 calc R U P B 1
C13X C -0.2627(11) 0.2811(7) -0.3582(7) 0.032(2) Uani 0.473(7) 1 d D U P B 1
N3X N -0.4496(9) 0.2800(6) -0.3937(6) 0.038(2) Uani 0.473(7) 1 d . U P B 1
H3X H -0.5198 0.2641 -0.4146 0.045 Uiso 0.473(7) 1 calc R U P B 1
C7X C -0.4104(12) 0.3583(8) -0.3564(7) 0.037(2) Uani 0.473(7) 1 d . U P B 1
H7X H -0.4560 0.4021 -0.3455 0.044 Uiso 0.473(7) 1 calc R U P B 1
C6X C -0.294(2) 0.3640(12) -0.337(2) 0.031(4) Uani 0.473(7) 1 d . U P B 1
C5X C -0.2194(15) 0.4317(11) -0.2911(12) 0.031(3) Uani 0.473(7) 1 d . U P B 1
H5X1 H -0.1518 0.4055 -0.2506 0.037 Uiso 0.473(7) 1 calc R U P B 1
H5X2 H -0.2571 0.4646 -0.2571 0.037 Uiso 0.473(7) 1 calc R U P B 1
N2X N -0.101(2) 0.549(2) -0.306(2) 0.032(4) Uani 0.473(7) 1 d . U P B 1
H2X H -0.1204 0.6019 -0.3004 0.038 Uiso 0.473(7) 1 calc R U P B 1
C3X C -0.1843(18) 0.4932(19) -0.3504(17) 0.030(4) Uani 0.473(7) 1 d . U P B 1
H3XA H -0.1547 0.4581 -0.3890 0.036 Uiso 0.473(7) 1 calc R U P B 1
O1X O 0.0490(9) 0.4542(6) -0.2705(6) 0.039(2) Uani 0.473(7) 1 d . U P B 1
C2X C 0.0099(14) 0.5294(11) -0.2684(11) 0.019(3) Uani 0.473(7) 1 d . U P B 1
O2X O -0.288(3) 0.6248(19) -0.388(2) 0.112(10) Uani 0.473(7) 1 d . U P B 1
C4X C -0.285(3) 0.555(3) -0.412(2) 0.041(6) Uani 0.473(7) 1 d . U P B 1
O3X O -0.353(3) 0.517(2) -0.4752(15) 0.100(10) Uani 0.473(7) 1 d . U P B 1
C1X C 0.0890(15) 0.5950(15) -0.2103(11) 0.028(4) Uani 0.473(7) 1 d . U P B 1
H1X1 H 0.0603 0.6533 -0.2272 0.034 Uiso 0.473(7) 1 calc R U P B 1
H1X2 H 0.0923 0.5856 -0.1502 0.034 Uiso 0.473(7) 1 calc R U P B 1
N1X N 0.1985(13) 0.5873(7) -0.2169(8) 0.022(2) Uani 0.473(7) 1 d . U P B 1
H1XA H 0.2444 0.6262 -0.1819 0.033 Uiso 0.473(7) 1 calc R U P B 1
H1XB H 0.1956 0.5970 -0.2720 0.033 Uiso 0.473(7) 1 calc R U P B 1
H1XC H 0.2250 0.5337 -0.2011 0.033 Uiso 0.473(7) 1 calc R U P B 1
O10W O -0.4686(10) 0.6006(8) -0.6126(9) 0.083(4) Uani 0.527(7) 1 d . . P B 2
O5W O -0.0946(17) 0.5985(18) -0.5169(18) 0.101(9) Uani 0.527(7) 1 d . . P B 2
O9W O 0.4578(10) 0.4285(8) 0.4399(8) 0.070(3) Uani 0.527(7) 1 d . . P B 2
O11W O 0.2788(14) 0.3812(14) 0.4870(9) 0.108(5) Uani 0.527(7) 1 d . . P B 2
O12W O 0.1720(16) 0.4508(9) -0.4125(12) 0.105(5) Uani 0.527(7) 1 d . . P B 2
O8W O 0.2796(16) 1.1778(8) -0.3182(14) 0.114(6) Uani 0.527(7) 1 d . . P B 2
O14W O 0.3355(16) 1.2151(15) -0.4703(13) 0.124(7) Uani 0.527(7) 1 d . . P B 2
C8XA C -0.2544(18) 0.2171(8) -0.3799(9) 0.069(5) Uani 0.527(7) 1 d D . P B 2
C9XA C -0.194(3) 0.1470(15) -0.3947(19) 0.083(10) Uani 0.527(7) 1 d D . P B 2
H9XA H -0.2324 0.0965 -0.4193 0.100 Uiso 0.527(7) 1 calc R U P B 2
C10A C -0.080(3) 0.1496(14) -0.3747(14) 0.119(11) Uani 0.527(7) 1 d D . P B 2
H10A H -0.0411 0.1034 -0.3892 0.143 Uiso 0.527(7) 1 calc R U P B 2
C11A C -0.023(2) 0.2210(14) -0.3328(12) 0.102(8) Uani 0.527(7) 1 d D U P B 2
H11A H 0.0557 0.2212 -0.3144 0.122 Uiso 0.527(7) 1 calc R U P B 2
C12A C -0.0785(13) 0.2913(13) -0.3174(9) 0.077(5) Uani 0.527(7) 1 d D U P B 2
H12A H -0.0380 0.3405 -0.2911 0.092 Uiso 0.527(7) 1 calc R U P B 2
C13A C -0.1956(14) 0.2899(10) -0.3408(8) 0.054(3) Uani 0.527(7) 1 d D U P B 2
C7XA C -0.3760(16) 0.3127(13) -0.3659(9) 0.065(3) Uani 0.527(7) 1 d . U P B 2
H7XA H -0.4445 0.3395 -0.3691 0.078 Uiso 0.527(7) 1 calc R U P B 2
N3XA N -0.367(3) 0.2321(19) -0.397(2) 0.064(7) Uani 0.527(7) 1 d . U P B 2
H3X3 H -0.4218 0.1972 -0.4227 0.076 Uiso 0.527(7) 1 calc R U P B 2
C6XA C -0.276(2) 0.3475(16) -0.331(3) 0.052(5) Uani 0.527(7) 1 d . U P B 2
C5XA C -0.255(3) 0.4430(16) -0.3043(17) 0.072(7) Uani 0.527(7) 1 d . U P B 2
H5X3 H -0.2115 0.4461 -0.2426 0.087 Uiso 0.527(7) 1 calc R U P B 2
H5X4 H -0.3279 0.4712 -0.3122 0.087 Uiso 0.527(7) 1 calc R U P B 2
N2XA N -0.099(3) 0.543(2) -0.293(2) 0.051(5) Uani 0.527(7) 1 d . U P B 2
H2XA H -0.1142 0.5861 -0.2650 0.061 Uiso 0.527(7) 1 calc R U P B 2
C3XA C -0.192(3) 0.4932(18) -0.357(2) 0.056(6) Uani 0.527(7) 1 d . U P B 2
H3X4 H -0.1622 0.4539 -0.3926 0.067 Uiso 0.527(7) 1 calc R U P B 2
O1XA O 0.033(2) 0.4807(17) -0.323(2) 0.188(15) Uani 0.527(7) 1 d . U P B 2
C2XA C 0.000(3) 0.521(3) -0.282(2) 0.081(8) Uani 0.527(7) 1 d . U P B 2
C4XA C -0.280(3) 0.545(2) -0.4085(17) 0.044(6) Uani 0.527(7) 1 d . U P B 2
O3XA O -0.3426(15) 0.5082(10) -0.4731(12) 0.044(3) Uani 0.527(7) 1 d . U P B 2
O2XA O -0.2898(8) 0.6232(8) -0.3855(5) 0.026(2) Uani 0.527(7) 1 d . U P B 2
C1XA C 0.077(2) 0.576(2) -0.215(2) 0.070(6) Uani 0.527(7) 1 d . U P B 2
H1X3 H 0.0904 0.5479 -0.1581 0.084 Uiso 0.527(7) 1 calc R U P B 2
H1X4 H 0.0395 0.6309 -0.2131 0.084 Uiso 0.527(7) 1 calc R U P B 2
N1XA N 0.194(2) 0.594(2) -0.228(2) 0.117(11) Uani 0.527(7) 1 d . U P B 2
H1X6 H 0.2358 0.6290 -0.1862 0.176 Uiso 0.527(7) 1 calc R U P B 2
H1X7 H 0.1828 0.6189 -0.2802 0.176 Uiso 0.527(7) 1 calc R U P B 2
H1X8 H 0.2314 0.5436 -0.2263 0.176 Uiso 0.527(7) 1 calc R U P B 2
O8 O 0.3249(3) 0.8903(2) 0.1296(2) 0.0274(7) Uani 1 1 d . . . . .
O1 O -0.1136(3) 0.6761(2) -0.1818(2) 0.0346(8) Uani 1 1 d . . . . .
O10 O 0.6687(3) 0.8233(2) -0.0794(2) 0.0324(7) Uani 1 1 d . . . . .
O6 O -0.0122(4) 0.7072(3) -0.3627(3) 0.0475(11) Uani 1 1 d . . . . .
O12 O 0.2200(3) 1.0439(2) -0.2167(2) 0.0345(8) Uani 1 1 d . . . . .
O7 O 0.1528(3) 1.0022(2) -0.0342(2) 0.0294(7) Uani 1 1 d . . . . .
O3 O 0.3055(3) 0.4908(2) -0.0609(2) 0.0293(7) Uani 1 1 d . . . . .
O9 O 0.5774(3) 0.7992(2) 0.0930(2) 0.0282(7) Uani 1 1 d . . . . .
O2 O 0.0685(3) 0.5625(2) -0.0210(2) 0.0281(7) Uani 1 1 d . . . . .
O5 O 0.2234(3) 0.6246(2) -0.3889(3) 0.0400(9) Uani 1 1 d . . . . .
N15 N 0.1586(3) 0.8210(2) 0.1134(2) 0.0243(7) Uani 1 1 d . . . . .
N3 N 0.0597(3) 0.6923(2) 0.0435(3) 0.0256(8) Uani 1 1 d . . . . .
N2 N -0.0780(3) 0.7706(2) -0.0691(3) 0.0277(8) Uani 1 1 d . . . . .
O11 O 0.4720(4) 0.9315(2) -0.2266(3) 0.0397(9) Uani 1 1 d . . . . .
N20 N 0.6198(4) 0.7326(3) -0.1970(3) 0.0313(9) Uani 1 1 d . . . . .
N17 N 0.4855(3) 0.6860(2) 0.1314(3) 0.0248(8) Uani 1 1 d . . . . .
N16 N 0.3142(3) 0.7435(2) 0.1441(3) 0.0245(8) Uani 1 1 d . . . . .
N18 N 0.5994(3) 0.6595(2) 0.0569(3) 0.0265(8) Uani 1 1 d . . . . .
N12 N -0.0400(4) 0.8432(3) -0.3212(3) 0.0312(9) Uani 1 1 d . . . . .
N19 N 0.6628(3) 0.6763(3) -0.0672(3) 0.0299(8) Uani 1 1 d . . . . .
N7 N 0.5431(3) 0.5550(2) -0.1319(3) 0.0291(8) Uani 1 1 d . . . . .
O4 O 0.3869(3) 0.5114(2) -0.2415(3) 0.0381(8) Uani 1 1 d . . . . .
N11 N 0.0693(4) 0.8254(3) -0.4006(3) 0.0302(9) Uani 1 1 d . . . . .
C27 C 0.2713(4) 0.8251(3) 0.1286(3) 0.0228(8) Uani 1 1 d . . . . .
C29 C 0.5555(4) 0.7230(3) 0.0930(3) 0.0229(9) Uani 1 1 d . . . . .
N23 N 0.1699(4) 0.9530(3) -0.3340(3) 0.0286(8) Uani 1 1 d . . . . .
N6 N 0.4888(3) 0.5345(3) -0.0056(3) 0.0288(8) Uani 1 1 d . . . . .
N5 N 0.3752(3) 0.5614(2) 0.0684(3) 0.0263(8) Uani 1 1 d . . . . .
N24 N 0.0453(4) 0.9817(3) -0.2692(3) 0.0309(9) Uani 1 1 d . . . . .
N1 N -0.1042(3) 0.8219(3) -0.1991(3) 0.0306(9) Uani 1 1 d . . . . .
C7 C 0.4738(4) 0.5534(3) -0.2138(4) 0.0313(10) Uani 1 1 d . . . . .
N13 N -0.0039(4) 0.9543(3) -0.1409(3) 0.0281(8) Uani 1 1 d . . . . .
N22 N 0.3378(4) 0.8934(3) -0.3530(3) 0.0288(8) Uani 1 1 d . . . . .
N14 N 0.0399(3) 0.8940(2) -0.0116(2) 0.0232(7) Uani 1 1 d . . . . .
C15 C 0.1213(4) 0.7357(3) 0.1227(3) 0.0234(9) Uani 1 1 d . . . . .
H15 H 0.0800 0.7339 0.1651 0.028 Uiso 1 1 calc R U . . .
C17 C 0.4817(4) 0.5942(3) 0.1233(3) 0.0243(9) Uani 1 1 d . . . . .
H17 H 0.5066 0.5652 0.1804 0.029 Uiso 1 1 calc R U . . .
C1 C -0.0989(4) 0.7490(3) -0.1526(3) 0.0271(9) Uani 1 1 d . . . . .
C25 C 0.0715(4) 0.9552(3) -0.0595(3) 0.0261(9) Uani 1 1 d . . . . .
N10 N 0.2361(4) 0.7671(3) -0.4208(3) 0.0295(9) Uani 1 1 d . . . . .
C31 C 0.6511(4) 0.7519(3) -0.1113(3) 0.0302(10) Uani 1 1 d . . . . .
N4 N 0.2092(3) 0.6107(2) 0.0982(3) 0.0252(8) Uani 1 1 d . . . . .
N9 N 0.3908(4) 0.6908(3) -0.3759(3) 0.0328(9) Uani 1 1 d . . . . .
C3 C 0.1086(4) 0.6166(3) 0.0337(3) 0.0255(9) Uani 1 1 d . . . . .
N8 N 0.5167(4) 0.6043(3) -0.2620(3) 0.0349(9) Uani 1 1 d . . . . .
C11 C 0.0042(4) 0.7845(3) -0.3621(3) 0.0321(10) Uani 1 1 d . . . . .
N21 N 0.4927(4) 0.8175(3) -0.3087(3) 0.0331(9) Uani 1 1 d . . . . .
C30 C 0.6927(4) 0.6725(3) 0.0253(3) 0.0287(10) Uani 1 1 d . . . . .
H30A H 0.7305 0.7265 0.0496 0.034 Uiso 1 1 calc R U . . .
H30B H 0.7467 0.6255 0.0466 0.034 Uiso 1 1 calc R U . . .
C33 C 0.4377(4) 0.8857(3) -0.2897(3) 0.0306(10) Uani 1 1 d . . . . .
C26 C 0.0861(4) 0.8936(3) 0.0808(3) 0.0249(9) Uani 1 1 d . . . . .
H26A H 0.0244 0.8927 0.1054 0.030 Uiso 1 1 calc R U . . .
H26B H 0.1289 0.9469 0.0999 0.030 Uiso 1 1 calc R U . . .
C4 C 0.2861(4) 0.5416(3) 0.1020(3) 0.0274(9) Uani 1 1 d . . . . .
H4A H 0.3193 0.5237 0.1625 0.033 Uiso 1 1 calc R U . . .
H4B H 0.2438 0.4924 0.0699 0.033 Uiso 1 1 calc R U . . .
C18 C 0.5607(4) 0.5752(3) 0.0706(3) 0.0275(9) Uani 1 1 d . . . . .
H18 H 0.6238 0.5372 0.1025 0.033 Uiso 1 1 calc R U . . .
C21 C 0.4306(4) 0.7755(3) -0.3877(3) 0.0315(10) Uani 1 1 d . . . . .
H21 H 0.4719 0.7755 -0.4302 0.038 Uiso 1 1 calc R U . . .
C5 C 0.3824(4) 0.5258(3) -0.0048(3) 0.0270(9) Uani 1 1 d . . . . .
C19 C 0.6448(4) 0.6022(3) -0.1227(3) 0.0289(10) Uani 1 1 d . . . . .
H19 H 0.7113 0.5638 -0.1068 0.035 Uiso 1 1 calc R U . . .
C34 C 0.2671(4) 0.9677(3) -0.3609(3) 0.0294(10) Uani 1 1 d . . . . .
H34A H 0.2418 0.9866 -0.4214 0.035 Uiso 1 1 calc R U . . .
H34B H 0.3118 1.0146 -0.3260 0.035 Uiso 1 1 calc R U . . .
C23 C 0.0667(4) 0.9171(3) -0.3919(3) 0.0286(10) Uani 1 1 d . . . . .
H23 H 0.0418 0.9467 -0.4487 0.034 Uiso 1 1 calc R U . . .
C8 C 0.4620(5) 0.6168(3) -0.3537(3) 0.0336(11) Uani 1 1 d . . . . .
H8A H 0.5199 0.6216 -0.3818 0.040 Uiso 1 1 calc R U . . .
H8B H 0.4168 0.5655 -0.3771 0.040 Uiso 1 1 calc R U . . .
C12 C -0.1331(4) 0.8222(4) -0.2911(3) 0.0324(10) Uani 1 1 d . . . . .
H121 H -0.1936 0.8641 -0.3150 0.039 Uiso 1 1 calc R U . . .
H122 H -0.1620 0.7651 -0.3132 0.039 Uiso 1 1 calc R U . . .
C35 C 0.1526(4) 0.9969(3) -0.2676(3) 0.0275(9) Uani 1 1 d . . . . .
C13 C -0.0978(4) 0.8979(3) -0.1479(3) 0.0274(9) Uani 1 1 d . . . . .
H13 H -0.1699 0.9300 -0.1659 0.033 Uiso 1 1 calc R U . . .
C9 C 0.2782(4) 0.6880(3) -0.3936(3) 0.0312(10) Uani 1 1 d . . . . .
C20 C 0.6229(4) 0.6420(3) -0.2132(3) 0.0299(10) Uani 1 1 d . . . . .
H20 H 0.6831 0.6272 -0.2378 0.036 Uiso 1 1 calc R U . . .
C22 C 0.3216(4) 0.8288(3) -0.4192(3) 0.0284(10) Uani 1 1 d . . . . .
H22 H 0.3102 0.8546 -0.4769 0.034 Uiso 1 1 calc R U . . .
C2 C -0.0582(4) 0.7087(3) -0.0008(3) 0.0293(10) Uani 1 1 d . . . . .
H2A H -0.0949 0.6543 -0.0250 0.035 Uiso 1 1 calc R U . . .
H2B H -0.0932 0.7293 0.0413 0.035 Uiso 1 1 calc R U . . .
C10 C 0.1179(4) 0.7831(3) -0.4580(3) 0.0314(10) Uani 1 1 d . . . . .
H101 H 0.1052 0.8187 -0.5098 0.038 Uiso 1 1 calc R U . . .
H102 H 0.0791 0.7280 -0.4761 0.038 Uiso 1 1 calc R U . . .
C16 C 0.2317(4) 0.6838(3) 0.1548(3) 0.0239(9) Uani 1 1 d . . . . .
H16 H 0.2489 0.6662 0.2160 0.029 Uiso 1 1 calc R U . . .
C36 C -0.0006(4) 1.0152(3) -0.2061(3) 0.0299(10) Uani 1 1 d . . . . .
H36A H -0.0774 1.0354 -0.2358 0.036 Uiso 1 1 calc R U . . .
H36B H 0.0442 1.0651 -0.1780 0.036 Uiso 1 1 calc R U . . .
C14 C -0.0708(4) 0.8619(3) -0.0558(3) 0.0237(9) Uani 1 1 d . . . . .
H14 H -0.1257 0.8822 -0.0280 0.028 Uiso 1 1 calc R U . . .
C32 C 0.6079(4) 0.7975(3) -0.2608(4) 0.0336(11) Uani 1 1 d . . . . .
H32A H 0.6461 0.7784 -0.3013 0.040 Uiso 1 1 calc R U . . .
H32B H 0.6453 0.8501 -0.2325 0.040 Uiso 1 1 calc R U . . .
C24 C -0.0163(4) 0.9299(3) -0.3413(3) 0.0275(9) Uani 1 1 d . . . . .
H24 H -0.0856 0.9596 -0.3769 0.033 Uiso 1 1 calc R U . . .
C28 C 0.4332(4) 0.7318(3) 0.1838(3) 0.0254(9) Uani 1 1 d . . . . .
H28A H 0.4688 0.7886 0.1976 0.030 Uiso 1 1 calc R U . . .
H28B H 0.4465 0.7006 0.2384 0.030 Uiso 1 1 calc R U . . .
C6 C 0.5312(4) 0.4958(3) -0.0681(3) 0.0292(10) Uani 1 1 d . . . . .
H6A H 0.4803 0.4492 -0.0973 0.035 Uiso 1 1 calc R U . . .
H6B H 0.6048 0.4700 -0.0382 0.035 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C8X C13X 1.38(2) . ?
C8X C9X 1.378(18) . ?
C8X N3X 1.40(3) . ?
C9X C10X 1.389(17) . ?
C10X C11X 1.397(19) . ?
C11X C12X 1.375(18) . ?
C12X C13X 1.400(15) . ?
C13X C6X 1.43(2) . ?
N3X C7X 1.390(15) . ?
C7X C6X 1.41(3) . ?
C6X C5X 1.46(3) . ?
C5X C3X 1.54(3) . ?
N2X C2X 1.37(3) . ?
N2X C3X 1.39(4) . ?
C3X C4X 1.66(5) . ?
O1X C2X 1.28(2) . ?
C2X C1X 1.535(16) . ?
O2X C4X 1.17(5) . ?
C4X O3X 1.26(5) . ?
C1X N1X 1.43(2) . ?
C8XA N3XA 1.38(4) . ?
C8XA C13A 1.400(16) . ?
C8XA C9XA 1.407(19) . ?
C9XA C10A 1.37(2) . ?
C10A C11A 1.39(2) . ?
C11A C12A 1.370(19) . ?
C12A C13A 1.409(18) . ?
C13A C6XA 1.41(3) . ?
C7XA C6XA 1.33(3) . ?
C7XA N3XA 1.38(4) . ?
C6XA C5XA 1.56(4) . ?
C5XA C3XA 1.58(4) . ?
N2XA C2XA 1.25(5) . ?
N2XA C3XA 1.51(4) . ?
C3XA C4XA 1.42(5) . ?
O1XA C2XA 1.11(4) . ?
C2XA C1XA 1.49(4) . ?
C4XA O3XA 1.24(3) . ?
C4XA O2XA 1.31(3) . ?
C1XA N1XA 1.61(4) . ?
O8 C27 1.224(6) . ?
O1 C1 1.229(6) . ?
O10 C31 1.224(6) . ?
O6 C11 1.229(7) . ?
O12 C35 1.231(6) . ?
O7 C25 1.225(6) . ?
O3 C5 1.235(6) . ?
O9 C29 1.224(6) . ?
O2 C3 1.222(6) . ?
O5 C9 1.229(6) . ?
N15 C27 1.370(6) . ?
N15 C15 1.442(6) . ?
N15 C26 1.451(6) . ?
N3 C3 1.371(6) . ?
N3 C15 1.456(6) . ?
N3 C2 1.460(6) . ?
N2 C1 1.359(6) . ?
N2 C2 1.445(7) . ?
N2 C14 1.445(6) . ?
O11 C33 1.223(6) . ?
N20 C31 1.373(7) . ?
N20 C32 1.434(7) . ?
N20 C20 1.447(6) . ?
N17 C29 1.372(6) . ?
N17 C28 1.439(6) . ?
N17 C17 1.444(6) . ?
N16 C27 1.380(6) . ?
N16 C28 1.449(6) . ?
N16 C16 1.455(6) . ?
N18 C29 1.367(6) . ?
N18 C30 1.451(6) . ?
N18 C18 1.451(6) . ?
N12 C11 1.363(7) . ?
N12 C24 1.451(6) . ?
N12 C12 1.457(6) . ?
N19 C31 1.374(7) . ?
N19 C19 1.449(6) . ?
N19 C30 1.450(7) . ?
N7 C7 1.354(7) . ?
N7 C6 1.445(7) . ?
N7 C19 1.451(6) . ?
O4 C7 1.237(6) . ?
N11 C11 1.352(7) . ?
N11 C23 1.445(6) . ?
N11 C10 1.445(6) . ?
N23 C35 1.370(6) . ?
N23 C34 1.455(6) . ?
N23 C23 1.461(6) . ?
N6 C5 1.360(6) . ?
N6 C18 1.441(6) . ?
N6 C6 1.441(6) . ?
N5 C5 1.359(6) . ?
N5 C4 1.442(6) . ?
N5 C17 1.456(6) . ?
N24 C35 1.372(7) . ?
N24 C36 1.443(6) . ?
N24 C24 1.444(6) . ?
N1 C1 1.364(7) . ?
N1 C12 1.441(6) . ?
N1 C13 1.446(6) . ?
C7 N8 1.357(7) . ?
N13 C25 1.374(7) . ?
N13 C36 1.448(6) . ?
N13 C13 1.457(6) . ?
N22 C33 1.362(7) . ?
N22 C34 1.449(6) . ?
N22 C22 1.453(6) . ?
N14 C25 1.380(6) . ?
N14 C26 1.445(6) . ?
N14 C14 1.446(6) . ?
C15 C16 1.556(6) . ?
C17 C18 1.552(7) . ?
N10 C9 1.365(7) . ?
N10 C10 1.446(7) . ?
N10 C22 1.446(6) . ?
N4 C3 1.376(6) . ?
N4 C4 1.444(6) . ?
N4 C16 1.446(6) . ?
N9 C9 1.363(7) . ?
N9 C8 1.441(7) . ?
N9 C21 1.454(6) . ?
N8 C20 1.453(6) . ?
N8 C8 1.459(7) . ?
N21 C33 1.366(7) . ?
N21 C21 1.446(6) . ?
N21 C32 1.453(7) . ?
C21 C22 1.554(7) . ?
C19 C20 1.557(7) . ?
C23 C24 1.552(7) . ?
C13 C14 1.552(7) . ?

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
C13X C8X C9X 126(2) . . ?
C13X C8X N3X 108.0(14) . . ?
C9X C8X N3X 125.9(19) . . ?
C8X C9X C10X 114.0(17) . . ?
C9X C10X C11X 122.9(17) . . ?
C12X C11X C10X 120(2) . . ?
C11X C12X C13X 118.8(14) . . ?
C8X C13X C12X 118.0(15) . . ?
C8X C13X C6X 110.2(16) . . ?
C12X C13X C6X 131.8(14) . . ?
C7X N3X C8X 107.0(12) . . ?
N3X C7X C6X 110.8(13) . . ?
C7X C6X C13X 103.8(16) . . ?
C7X C6X C5X 128.2(18) . . ?
C13X C6X C5X 127.0(19) . . ?
C6X C5X C3X 113(2) . . ?
C2X N2X C3X 127(3) . . ?
N2X C3X C5X 112(2) . . ?
N2X C3X C4X 105(3) . . ?
C5X C3X C4X 115.3(17) . . ?
O1X C2X N2X 122.6(18) . . ?
O1X C2X C1X 116.8(15) . . ?
N2X C2X C1X 120(2) . . ?
O2X C4X O3X 129(3) . . ?
O2X C4X C3X 116(3) . . ?
O3X C4X C3X 115(3) . . ?
N1X C1X C2X 110.5(12) . . ?
N3XA C8XA C13A 108.5(17) . . ?
N3XA C8XA C9XA 133(2) . . ?
C13A C8XA C9XA 118.4(19) . . ?
C10A C9XA C8XA 122(2) . . ?
C9XA C10A C11A 119(2) . . ?
C12A C11A C10A 122(2) . . ?
C11A C12A C13A 119.5(19) . . ?
C8XA C13A C12A 119.7(18) . . ?
C8XA C13A C6XA 106.0(18) . . ?
C12A C13A C6XA 134.2(19) . . ?
C6XA C7XA N3XA 111(2) . . ?
C7XA N3XA C8XA 106.5(19) . . ?
C7XA C6XA C13A 108(2) . . ?
C7XA C6XA C5XA 125(2) . . ?
C13A C6XA C5XA 126(3) . . ?
C6XA C5XA C3XA 113(3) . . ?
C2XA N2XA C3XA 119(3) . . ?
C4XA C3XA N2XA 114(3) . . ?
C4XA C3XA C5XA 99(3) . . ?
N2XA C3XA C5XA 107(3) . . ?
O1XA C2XA N2XA 128(4) . . ?
O1XA C2XA C1XA 120(3) . . ?
N2XA C2XA C1XA 110(3) . . ?
O3XA C4XA O2XA 126(3) . . ?
O3XA C4XA C3XA 115(3) . . ?
O2XA C4XA C3XA 119(3) . . ?
C2XA C1XA N1XA 114(3) . . ?
C27 N15 C15 112.4(4) . . ?
C27 N15 C26 122.0(4) . . ?
C15 N15 C26 125.1(4) . . ?
C3 N3 C15 112.1(4) . . ?
C3 N3 C2 121.4(4) . . ?
C15 N3 C2 122.3(4) . . ?
C1 N2 C2 123.4(4) . . ?
C1 N2 C14 112.5(4) . . ?
C2 N2 C14 124.0(4) . . ?
C31 N20 C32 121.7(4) . . ?
C31 N20 C20 112.9(4) . . ?
C32 N20 C20 124.2(4) . . ?
C29 N17 C28 123.9(4) . . ?
C29 N17 C17 112.7(4) . . ?
C28 N17 C17 122.9(4) . . ?
C27 N16 C28 119.4(4) . . ?
C27 N16 C16 111.2(4) . . ?
C28 N16 C16 123.2(4) . . ?
C29 N18 C30 123.1(4) . . ?
C29 N18 C18 112.9(4) . . ?
C30 N18 C18 122.6(4) . . ?
C11 N12 C24 111.7(4) . . ?
C11 N12 C12 121.5(4) . . ?
C24 N12 C12 122.6(4) . . ?
C31 N19 C19 112.8(4) . . ?
C31 N19 C30 122.6(4) . . ?
C19 N19 C30 124.5(4) . . ?
C7 N7 C6 121.9(4) . . ?
C7 N7 C19 112.5(4) . . ?
C6 N7 C19 123.2(4) . . ?
C11 N11 C23 112.8(4) . . ?
C11 N11 C10 122.9(4) . . ?
C23 N11 C10 123.2(4) . . ?
O8 C27 N15 125.7(4) . . ?
O8 C27 N16 125.8(4) . . ?
N15 C27 N16 108.5(4) . . ?
O9 C29 N18 125.8(4) . . ?
O9 C29 N17 126.3(4) . . ?
N18 C29 N17 107.9(4) . . ?
C35 N23 C34 122.2(4) . . ?
C35 N23 C23 112.0(4) . . ?
C34 N23 C23 122.0(4) . . ?
C5 N6 C18 112.8(4) . . ?
C5 N6 C6 124.3(4) . . ?
C18 N6 C6 122.2(4) . . ?
C5 N5 C4 122.5(4) . . ?
C5 N5 C17 112.6(4) . . ?
C4 N5 C17 121.3(4) . . ?
C35 N24 C36 123.4(4) . . ?
C35 N24 C24 112.6(4) . . ?
C36 N24 C24 124.1(4) . . ?
C1 N1 C12 122.9(4) . . ?
C1 N1 C13 112.2(4) . . ?
C12 N1 C13 124.0(5) . . ?
O4 C7 N7 126.3(5) . . ?
O4 C7 N8 125.0(5) . . ?
N7 C7 N8 108.6(4) . . ?
C25 N13 C36 122.9(4) . . ?
C25 N13 C13 112.2(4) . . ?
C36 N13 C13 123.9(4) . . ?
C33 N22 C34 122.4(4) . . ?
C33 N22 C22 112.7(4) . . ?
C34 N22 C22 123.9(4) . . ?
C25 N14 C26 120.8(4) . . ?
C25 N14 C14 111.5(4) . . ?
C26 N14 C14 121.9(4) . . ?
N15 C15 N3 115.9(4) . . ?
N15 C15 C16 103.3(3) . . ?
N3 C15 C16 103.0(3) . . ?
N17 C17 N5 113.9(4) . . ?
N17 C17 C18 103.5(4) . . ?
N5 C17 C18 102.7(4) . . ?
O1 C1 N2 125.7(5) . . ?
O1 C1 N1 125.7(5) . . ?
N2 C1 N1 108.6(4) . . ?
O7 C25 N13 125.6(4) . . ?
O7 C25 N14 126.2(4) . . ?
N13 C25 N14 108.3(4) . . ?
C9 N10 C10 122.6(4) . . ?
C9 N10 C22 112.9(4) . . ?
C10 N10 C22 124.0(4) . . ?
O10 C31 N20 126.5(5) . . ?
O10 C31 N19 125.9(5) . . ?
N20 C31 N19 107.5(4) . . ?
C3 N4 C4 121.9(4) . . ?
C3 N4 C16 112.8(4) . . ?
C4 N4 C16 125.1(4) . . ?
C9 N9 C8 123.8(4) . . ?
C9 N9 C21 112.6(4) . . ?
C8 N9 C21 123.5(4) . . ?
O2 C3 N3 126.2(5) . . ?
O2 C3 N4 125.8(4) . . ?
N3 C3 N4 108.0(4) . . ?
C7 N8 C20 112.9(4) . . ?
C7 N8 C8 122.6(4) . . ?
C20 N8 C8 124.5(4) . . ?
O6 C11 N11 126.2(5) . . ?
O6 C11 N12 124.9(5) . . ?
N11 C11 N12 108.8(4) . . ?
C33 N21 C21 113.1(4) . . ?
C33 N21 C32 122.8(4) . . ?
C21 N21 C32 123.5(4) . . ?
N19 C30 N18 114.5(4) . . ?
O11 C33 N22 126.0(5) . . ?
O11 C33 N21 125.9(5) . . ?
N22 C33 N21 108.1(4) . . ?
N14 C26 N15 112.8(4) . . ?
N5 C4 N4 115.0(4) . . ?
N6 C18 N18 114.6(4) . . ?
N6 C18 C17 103.4(4) . . ?
N18 C18 C17 103.0(4) . . ?
N21 C21 N9 113.9(4) . . ?
N21 C21 C22 102.9(4) . . ?
N9 C21 C22 103.1(4) . . ?
O3 C5 N5 125.8(5) . . ?
O3 C5 N6 125.8(5) . . ?
N5 C5 N6 108.5(4) . . ?
N19 C19 N7 115.3(4) . . ?
N19 C19 C20 103.2(4) . . ?
N7 C19 C20 103.0(4) . . ?
N22 C34 N23 113.9(4) . . ?
N11 C23 N23 113.7(4) . . ?
N11 C23 C24 102.8(4) . . ?
N23 C23 C24 102.7(4) . . ?
N9 C8 N8 115.0(4) . . ?
N1 C12 N12 113.5(4) . . ?
O12 C35 N23 126.2(5) . . ?
O12 C35 N24 125.7(5) . . ?
N23 C35 N24 108.1(4) . . ?
N1 C13 N13 115.9(4) . . ?
N1 C13 C14 103.0(4) . . ?
N13 C13 C14 102.9(4) . . ?
O5 C9 N9 125.9(5) . . ?
O5 C9 N10 125.7(5) . . ?
N9 C9 N10 108.3(4) . . ?
N20 C20 N8 115.2(4) . . ?
N20 C20 C19 102.9(4) . . ?
N8 C20 C19 102.5(4) . . ?
N10 C22 N22 113.7(4) . . ?
N10 C22 C21 103.1(4) . . ?
N22 C22 C21 103.2(4) . . ?
N2 C2 N3 113.6(4) . . ?
N11 C10 N10 113.8(4) . . ?
N4 C16 N16 115.6(4) . . ?
N4 C16 C15 103.0(4) . . ?
N16 C16 C15 103.1(3) . . ?
N24 C36 N13 114.2(4) . . ?
N2 C14 N14 115.1(4) . . ?
N2 C14 C13 103.1(4) . . ?
N14 C14 C13 103.9(4) . . ?
N20 C32 N21 113.7(4) . . ?
N24 C24 N12 115.7(4) . . ?
N24 C24 C23 103.5(4) . . ?
N12 C24 C23 103.2(4) . . ?
N17 C28 N16 113.9(4) . . ?
N6 C6 N7 113.6(4) . . ?

_refine_diff_density_max         0.690
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.072

_shelxl_version_number           2013-3

