# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_hh_plcycage138rr_130k
_audit_block_doi                 10.5517/ccdc.csd.cc2665p9
_database_code_depnum_ccdc_archive 'CCDC 2031730'
loop_
_citation_id
_citation_doi
_citation_year
1 10.26434/chemrxiv.12957314.v1 2020
loop_
_audit_author_name
_audit_author_address
'Prescimone A.'
;University of Basel
Switzerland
;
_audit_update_record             
;
2020-09-13 deposited with the CCDC.	2021-02-11 downloaded from the CCDC.
;
_audit_creation_date             2019-08-20
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
loop_
_audit_author_email
alessandro.prescimone@unibas.ch
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C84 H78 N12 O12, 4.8(C7 H5 O2), C0.5 H3.5 O0.5, 0.9(C H4 O)'
_chemical_formula_sum            'C119 H109.10 N12 O23'
_chemical_formula_weight         2075.28
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0148 0.0070 '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 0.0253 0.0136 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0412 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 1 2 1'
_space_group_name_Hall           'C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   31.9058(6)
_cell_length_b                   17.2344(3)
_cell_length_c                   20.9913(4)
_cell_angle_alpha                90
_cell_angle_beta                 102.3150(10)
_cell_angle_gamma                90
_cell_volume                     11277.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    130
_cell_measurement_reflns_used    99325
_cell_measurement_theta_min      2.76
_cell_measurement_theta_max      57.45
_shelx_estimated_absorpt_T_max   0.956
_shelx_estimated_absorpt_T_min   0.907
_exptl_absorpt_coefficient_mu    0.451
_exptl_absorpt_correction_T_max  0.9954
_exptl_absorpt_correction_T_min  0.9837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 -2 2 0.1220
5 3 5 0.0730
-2 -1 -2 0.0610
2 4 -5 0.1420
-4 3 1 0.1030
4 -3 -1 0.0310
-5 -3 2 0.1140
2 1 -1 0.1360

_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4364
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            60720
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         57.230
_diffrn_reflns_theta_min         3.004
_diffrn_ambient_temperature      130
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_measurement_details      
; 4172 frames, detector distance = 60 mm
;
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34143
_diffrn_source                   'Metaljet D2'
_diffrn_source_current           3.570
_diffrn_source_power             0.250
_diffrn_source_voltage           70
_reflns_Friedel_coverage         0.862
_reflns_Friedel_fraction_full    0.968
_reflns_Friedel_fraction_max     0.895
_reflns_number_gt                19674
_reflns_number_total             21729
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       
;
X-Area Pilatus3_SV 1.31.153.0 (STOE, 2018)
;
_computing_cell_refinement       
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_reduction        
;
X-Area Integrate 1.74.2.0 (STOE, 2018)
X-Area LANA 1.75.3.0 (STOE, 2018)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.297
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details 
;
 Flack x determined using 8008 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1395
_refine_ls_number_reflns         21729
_refine_ls_number_restraints     98
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0879
_refine_ls_restrained_S_all      1.087
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1679P)²+22.1789P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2449
_refine_ls_wR_factor_ref         0.2617
_refine_special_details          
;
Most of the solvent molecules are disordered and non fully occupied.
Restraints had to be used
;


# start Validation Reply Form
_vrf_PLAT410_hh_plcycage138rr_130k 
;
PROBLEM: Short Intra H...H Contact  H28A     ..H28A     .       1.25 Ang.
RESPONSE: this is actually not an issue as this methanol solvent molecule is not
fully occupied: the two H atoms won't be present at the same time.
;
# end Validation Reply Form




_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O136-H136
 0.82 with sigma of 0.02
 O27-H27A
 0.82 with sigma of 0.02
 O1A-H1A
 0.82 with sigma of 0.02
 C97-C96 = C96-C95 = C95-C94 = C94-C93 = C98-C93 = C98-C97 = C93-C92
 1.38 with sigma of 0.002
 C103-C102 \\sim C103-C104 \\sim C105-C104 \\sim C105-C100 \\sim C100-C101
\\sim C102-C101
 with sigma of 0.02
 C94-C95 \\sim C96-C95 \\sim C97-C96 \\sim C93-C94 \\sim C98-C93 \\sim C98-C97
 with sigma of 0.02
 C88-C89 \\sim C88-C87 \\sim C87-C86 \\sim C91-C86 \\sim C90-C91 \\sim C90-C89
 with sigma of 0.02
 C107-C108 \\sim C111-C110 \\sim C108-C109 \\sim C110-C109 \\sim C111-C112
\\sim C107-C112
 with sigma of 0.02
 O24-C119 \\sim O1A_$1-C120_$1 \\sim C121_$1-O27_$1
 with sigma of 0.02
 C117-C109 \\sim C113-C109 \\sim C117-C116 \\sim C114-C113 \\sim C115-C116
\\sim C115-C114
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
: with sigma of 0.1 and sigma for terminal atoms of 0.2
: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 O22, C99, O21, C100, C105, C104, C103, C102, C101
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C101(0.5) H101(0.5) O136(0.5) H136(0.5) C99(0.5) C102(0.5)
 H102(0.5) C95(0.5) H95(0.5) C100(0.5) C104(0.5) H104(0.5) C103(0.5) H103(0.5)
 C105(0.5) H105(0.5) O21(0.5) C94(0.5) H94(0.5) O18(0.5) C92(0.5) C96(0.5)
 H96(0.5) C93(0.5) C97(0.5) H97(0.5) O22(0.5) O17(0.5) C98(0.5) H98(0.5)
 C109(0.8) H109(0.5) H10A(0.3) C106(0.5) C107(0.5) O26(0.5) C108(0.5) H108(0.5)
 C110(0.5) H110(0.5) C112(0.5) H112(0.5) O25(0.5) C111(0.5) H111(0.5) O1A(0.5)
 H1A(0.5) C120(0.5) H12C(0.5) H12D(0.5) H12E(0.5) O24(0.3) C119(0.3) O27(0.4)
 H27A(0.4) C121(0.4) H12F(0.4) H12G(0.4) H12H(0.4) C117(0.3) H117(0.3)
 C116(0.3) C115(0.3) H115(0.3) C114(0.3) H114(0.3) C113(0.3) H113(0.3) O23(0.3)
6.a Riding coordinates:
 C28(H28A,H28B,H28C), O136(H136), O27(H27A), C121(H12F,H12G,H12H)
6.b Ternary CH refined with riding coordinates:
 C42(H42), C80(H80), C58(H58), C41(H41), C79(H79), C64(H64), C59(H59),
 C63(H63), C11(H11), C10(H10), C27(H27), C26(H26)
6.c Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B), C67(H67A,H67B), C43(H43A,H43B), C81(H81A,H81B), C44(H44A,
 H44B), C68(H68A,H68B), C57(H57A,H57B), C62(H62A,H62B), C84(H84A,H84B),
 C83(H83A,H83B), C65(H65A,H65B), C45(H45A,H45B), C66(H66A,H66B), C82(H82A,H82B),
  C60(H60A,H60B), C12(H12A,H12B), C61(H61A,H61B), C15(H15A,H15B), C30(H30A,
 H30B), C13(H13A,H13B), C0AA(H0AA,H0AB), C31(H31A,H31B), C29(H29A,H29B),
 C14(H14A,H14B)
6.d Aromatic/amide H refined with riding coordinates:
 C36(H36), C3(H3), C5(H5), C49(H49), C53(H53), C7(H7), C9(H9), C1(H1), C8(H8),
 C37(H37), C34(H34), C73(H73), C39(H39), C32(H32), C78(H78), C40(H40), C20(H20),
  C25(H25), C131(H131), C135(H135), C132(H132), C134(H134), C133(H133),
 C124(H124), C125(H125), C101(H101), C89(H89), C87(H87), C126(H126), C128(H128),
  C91(H91), C102(H102), C95(H95), C104(H104), C103(H103), C90(H90), C105(H105),
 C127(H127), C94(H94), C88(H88), C96(H96), C97(H97), C98(H98), C109(H109),
 C109(H10A), C108(H108), C110(H110), C112(H112), C111(H111), C117(H117),
 C115(H115), C114(H114), C113(H113)
6.e Idealised Me refined as rotating group:
 C120(H12C,H12D,H12E)
6.f Idealised tetrahedral OH refined as rotating group:
 O1A(H1A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
O8 O 0.55907(14) 0.7476(3) -0.0400(2) 0.0393(10) Uani 1 1 d . . . . .
O11 O 0.34785(15) 0.7510(3) 0.09887(19) 0.0379(9) Uani 1 1 d . . . . .
O12 O 0.32281(16) 0.7581(3) 0.3062(2) 0.0418(10) Uani 1 1 d . . . . .
O6 O 0.54726(14) 0.3968(3) -0.0560(2) 0.0374(9) Uani 1 1 d . . . . .
O5 O 0.67148(14) 0.3799(3) 0.1013(2) 0.0395(10) Uani 1 1 d . . . . .
O7 O 0.67960(14) 0.7255(3) 0.1224(2) 0.0413(10) Uani 1 1 d . . . . .
O9 O 0.36416(18) 0.4076(3) 0.1150(2) 0.0468(11) Uani 1 1 d . . . . .
O10 O 0.33080(15) 0.4138(3) 0.31665(19) 0.0379(9) Uani 1 1 d . . . . .
N10 N 0.61864(15) 0.7576(3) 0.0448(2) 0.0289(9) Uani 1 1 d . . . . .
N2 N 0.40145(14) 0.8858(3) 0.2150(2) 0.0296(9) Uani 1 1 d . . . . .
N12 N 0.33323(15) 0.7766(3) 0.2012(2) 0.0290(9) Uani 1 1 d . . . . .
N7 N 0.57047(15) 0.2680(3) 0.1079(2) 0.0310(10) Uani 1 1 d . . . . .
O1 O 0.56161(18) 0.7425(3) 0.5871(3) 0.0543(13) Uani 1 1 d . . . . .
N3 N 0.58206(15) 0.8537(3) 0.1367(2) 0.0305(9) Uani 1 1 d . . . . .
O3 O 0.58441(18) 0.3926(3) 0.5732(3) 0.0542(12) Uani 1 1 d . . . . .
O2 O 0.68219(17) 0.7743(4) 0.5055(3) 0.0593(14) Uani 1 1 d . . . . .
N1 N 0.57020(17) 0.8702(4) 0.4357(2) 0.0382(11) Uani 1 1 d . . . . .
N4 N 0.61995(17) 0.7803(3) 0.5444(2) 0.0378(11) Uani 1 1 d . . . . .
N8 N 0.41328(16) 0.2698(3) 0.2454(2) 0.0339(10) Uani 1 1 d . . . . .
N11 N 0.34693(16) 0.3886(3) 0.2155(2) 0.0322(10) Uani 1 1 d . . . . .
O16 O 0.26656(18) 0.4769(4) 0.0984(3) 0.0640(15) Uani 1 1 d . . . . .
N9 N 0.60868(15) 0.3669(3) 0.0222(2) 0.0280(9) Uani 1 1 d . . . . .
N6 N 0.60684(18) 0.2913(4) 0.4174(2) 0.0439(12) Uani 1 1 d . . . . .
O4 O 0.70372(19) 0.4338(4) 0.4899(3) 0.0604(14) Uani 1 1 d . . . . .
C4 C 0.47440(18) 0.8456(4) 0.2269(3) 0.0342(12) Uani 1 1 d . . . . .
C129 C 0.26951(19) 0.5122(4) 0.0489(3) 0.0406(14) Uani 1 1 d . . . . .
O15 O 0.2820(2) 0.4822(4) 0.0031(3) 0.0714(17) Uani 1 1 d . . . . .
C42 C 0.60828(18) 0.2812(3) 0.0188(3) 0.0285(11) Uani 1 1 d . . . . .
H42 H 0.6339 0.2622 0.0512 0.034 Uiso 1 1 calc R . . . .
N5 N 0.64515(18) 0.3927(4) 0.5294(2) 0.0429(12) Uani 1 1 d . . . . .
C77 C 0.33090(18) 0.7334(3) 0.2563(3) 0.0317(11) Uani 1 1 d . . . . .
C2 C 0.52504(18) 0.8446(4) 0.3307(3) 0.0355(12) Uani 1 1 d . . . . .
C36 C 0.53576(18) 0.2829(4) 0.1245(3) 0.0325(11) Uani 1 1 d . . . . .
H36 H 0.5104 0.2871 0.0914 0.039 Uiso 1 1 calc R . . . .
C3 C 0.48292(18) 0.8466(4) 0.2948(3) 0.0338(12) Uani 1 1 d . . . . .
H3 H 0.4598 0.8486 0.3168 0.041 Uiso 1 1 calc R . . . .
C6 C 0.55035(19) 0.8372(4) 0.2300(3) 0.0369(13) Uani 1 1 d . . . . .
C5 C 0.50747(18) 0.8391(4) 0.1947(3) 0.0332(12) Uani 1 1 d . . . . .
H5 H 0.5014 0.8360 0.1484 0.040 Uiso 1 1 calc R . . . .
C49 C 0.57532(17) 0.5679(3) -0.0189(2) 0.0283(11) Uani 1 1 d . . . . .
H49 H 0.5501 0.5719 -0.0523 0.034 Uiso 1 1 calc R . . . .
C80 C 0.36018(17) 0.9038(3) 0.1730(3) 0.0284(10) Uani 1 1 d . . . . .
H80 H 0.3600 0.8871 0.1273 0.034 Uiso 1 1 calc R . . . .
C51 C 0.58714(18) 0.7180(3) -0.0007(3) 0.0300(11) Uani 1 1 d . . . . .
C48 C 0.59318(17) 0.4967(3) 0.0035(2) 0.0274(10) Uani 1 1 d . . . . .
C53 C 0.65139(18) 0.5565(3) 0.0834(3) 0.0314(11) Uani 1 1 d . . . . .
H53 H 0.6763 0.5526 0.1173 0.038 Uiso 1 1 calc R . . . .
C75 C 0.34388(18) 0.7304(3) 0.1522(3) 0.0312(11) Uani 1 1 d . . . . .
C54 C 0.63007(17) 0.4915(3) 0.0527(3) 0.0291(11) Uani 1 1 d . . . . .
C50 C 0.59711(17) 0.6331(3) 0.0110(2) 0.0269(10) Uani 1 1 d . . . . .
C74 C 0.34842(18) 0.6499(3) 0.1789(3) 0.0290(10) Uani 1 1 d . . . . .
C52 C 0.63350(17) 0.6271(3) 0.0608(3) 0.0289(11) Uani 1 1 d . . . . .
C7 C 0.58645(19) 0.8417(4) 0.1973(3) 0.0379(13) Uani 1 1 d . . . . .
H7 H 0.6146 0.8353 0.2229 0.045 Uiso 1 1 calc R . . . .
C46 C 0.5681(2) 0.1598(4) 0.0332(3) 0.0373(13) Uani 1 1 d . . . . .
H46A H 0.5924 0.1383 0.0659 0.045 Uiso 1 1 calc R . . . .
H46B H 0.5412 0.1391 0.0431 0.045 Uiso 1 1 calc R . . . .
C76 C 0.33953(17) 0.6518(3) 0.2405(3) 0.0298(11) Uani 1 1 d . . . . .
C70 C 0.34433(18) 0.5168(4) 0.2460(3) 0.0306(11) Uani 1 1 d . . . . .
C9 C 0.43018(18) 0.8595(4) 0.1887(3) 0.0315(11) Uani 1 1 d . . . . .
H9 H 0.4236 0.8482 0.1434 0.038 Uiso 1 1 calc R . . . .
C55 C 0.64087(17) 0.4085(4) 0.0641(3) 0.0300(11) Uani 1 1 d . . . . .
C56 C 0.64822(18) 0.7073(4) 0.0823(3) 0.0307(11) Uani 1 1 d . . . . .
C58 C 0.62156(17) 0.8428(3) 0.0476(2) 0.0281(10) Uani 1 1 d . . . . .
H58 H 0.5957 0.8638 0.0169 0.034 Uiso 1 1 calc R . . . .
C47 C 0.57892(17) 0.4167(3) -0.0157(2) 0.0281(10) Uani 1 1 d . . . . .
C35 C 0.5326(2) 0.2942(4) 0.1926(3) 0.0359(12) Uani 1 1 d . . . . .
C1 C 0.53301(19) 0.8550(4) 0.4017(3) 0.0372(13) Uani 1 1 d . . . . .
H1 H 0.5097 0.8502 0.4230 0.045 Uiso 1 1 calc R . . . .
C41 C 0.56820(18) 0.2487(3) 0.0394(3) 0.0297(11) Uani 1 1 d . . . . .
H41 H 0.5416 0.2710 0.0114 0.036 Uiso 1 1 calc R . . . .
C79 C 0.32514(18) 0.8612(3) 0.1981(3) 0.0307(11) Uani 1 1 d . . . . .
H79 H 0.3262 0.8796 0.2436 0.037 Uiso 1 1 calc R . . . .
C64 C 0.33854(19) 0.3045(3) 0.2110(3) 0.0318(11) Uani 1 1 d . . . . .
H64 H 0.3425 0.2871 0.1672 0.038 Uiso 1 1 calc R . . . .
C59 C 0.62122(18) 0.8748(3) 0.1153(3) 0.0301(11) Uani 1 1 d . . . . .
H59 H 0.6467 0.8548 0.1473 0.036 Uiso 1 1 calc R . . . .
C8 C 0.55837(19) 0.8398(4) 0.2976(3) 0.0379(13) Uani 1 1 d . . . . .
H8 H 0.5872 0.8383 0.3217 0.046 Uiso 1 1 calc R . . . .
C72 C 0.35663(19) 0.4328(4) 0.1647(3) 0.0341(12) Uani 1 1 d . . . . .
C67 C 0.3140(2) 0.1586(4) 0.2629(3) 0.0383(13) Uani 1 1 d . . . . .
H67A H 0.3081 0.1022 0.2591 0.046 Uiso 1 1 calc R . . . .
H67B H 0.3095 0.1759 0.3060 0.046 Uiso 1 1 calc R . . . .
C37 C 0.49245(19) 0.2923(4) 0.2081(3) 0.0347(12) Uani 1 1 d . . . . .
H37 H 0.4676 0.2875 0.1742 0.042 Uiso 1 1 calc R . . . .
C34 C 0.56888(18) 0.3012(4) 0.2430(3) 0.0342(12) Uani 1 1 d . . . . .
H34 H 0.5964 0.3037 0.2327 0.041 Uiso 1 1 calc R . . . .
C71 C 0.35454(18) 0.5151(3) 0.1845(3) 0.0304(11) Uani 1 1 d . . . . .
C73 C 0.35704(19) 0.5823(4) 0.1481(3) 0.0325(11) Uani 1 1 d . . . . .
H73 H 0.3640 0.5818 0.1062 0.039 Uiso 1 1 calc R . . . .
C85 C 0.4559(2) 0.5563(5) 0.2717(4) 0.0468(15) Uani 1 1 d . . . . .
C43 C 0.6130(2) 0.2534(3) -0.0483(3) 0.0332(12) Uani 1 1 d . . . . .
H43A H 0.6404 0.2729 -0.0572 0.040 Uiso 1 1 calc R . . . .
H43B H 0.5893 0.2746 -0.0821 0.040 Uiso 1 1 calc R . . . .
C33 C 0.5657(2) 0.3045(4) 0.3077(3) 0.0360(12) Uani 1 1 d . . . . .
C39 C 0.4453(2) 0.2919(4) 0.2892(3) 0.0367(12) Uani 1 1 d . . . . .
H39 H 0.4416 0.3046 0.3317 0.044 Uiso 1 1 calc R . . . .
C81 C 0.3518(2) 0.9910(4) 0.1748(3) 0.0354(12) Uani 1 1 d . . . . .
H81A H 0.3549 1.0077 0.2207 0.042 Uiso 1 1 calc R . . . .
H81B H 0.3735 1.0190 0.1563 0.042 Uiso 1 1 calc R . . . .
C44 C 0.6124(2) 0.1645(4) -0.0517(3) 0.0405(14) Uani 1 1 d . . . . .
H44A H 0.6139 0.1477 -0.0963 0.049 Uiso 1 1 calc R . . . .
H44B H 0.6377 0.1435 -0.0210 0.049 Uiso 1 1 calc R . . . .
C19 C 0.5933(2) 0.7269(4) 0.5669(3) 0.0415(14) Uani 1 1 d . . . . .
C16 C 0.6536(2) 0.7435(4) 0.5245(3) 0.0418(14) Uani 1 1 d . . . . .
C32 C 0.6058(2) 0.3035(4) 0.3582(3) 0.0401(13) Uani 1 1 d . . . . .
H32 H 0.6322 0.3126 0.3451 0.048 Uiso 1 1 calc R . . . .
C68 C 0.3603(2) 0.1738(4) 0.2586(3) 0.0377(13) Uani 1 1 d . . . . .
H68A H 0.3653 0.1524 0.2171 0.045 Uiso 1 1 calc R . . . .
H68B H 0.3797 0.1465 0.2948 0.045 Uiso 1 1 calc R . . . .
C63 C 0.37125(18) 0.2607(4) 0.2622(3) 0.0312(11) Uani 1 1 d . . . . .
H63 H 0.3717 0.2816 0.3068 0.037 Uiso 1 1 calc R . . . .
C38 C 0.4879(2) 0.2974(4) 0.2733(3) 0.0357(12) Uani 1 1 d . . . . .
C11 C 0.6158(2) 0.8658(4) 0.5444(3) 0.0376(13) Uani 1 1 d . . . . .
H11 H 0.6387 0.8874 0.5234 0.045 Uiso 1 1 calc R . . . .
C69 C 0.34010(19) 0.4356(4) 0.2668(3) 0.0326(11) Uani 1 1 d . . . . .
C57 C 0.66128(19) 0.8729(4) 0.0250(3) 0.0343(12) Uani 1 1 d . . . . .
H57A H 0.6876 0.8548 0.0555 0.041 Uiso 1 1 calc R . . . .
H57B H 0.6616 0.8518 -0.0188 0.041 Uiso 1 1 calc R . . . .
C78 C 0.33691(19) 0.5854(4) 0.2769(3) 0.0319(11) Uani 1 1 d . . . . .
H78 H 0.3306 0.5866 0.3192 0.038 Uiso 1 1 calc R . . . .
C62 C 0.6610(2) 0.9605(4) 0.0224(3) 0.0414(14) Uani 1 1 d . . . . .
H62A H 0.6354 0.9784 -0.0096 0.050 Uiso 1 1 calc R . . . .
H62B H 0.6868 0.9790 0.0077 0.050 Uiso 1 1 calc R . . . .
C84 C 0.28074(19) 0.8800(4) 0.1578(3) 0.0372(13) Uani 1 1 d . . . . .
H84A H 0.2587 0.8514 0.1753 0.045 Uiso 1 1 calc R . . . .
H84B H 0.2787 0.8636 0.1121 0.045 Uiso 1 1 calc R . . . .
C83 C 0.2727(2) 0.9677(4) 0.1604(3) 0.0402(14) Uani 1 1 d . . . . .
H83A H 0.2443 0.9803 0.1328 0.048 Uiso 1 1 calc R . . . .
H83B H 0.2725 0.9831 0.2058 0.048 Uiso 1 1 calc R . . . .
C65 C 0.2922(2) 0.2879(4) 0.2141(3) 0.0388(13) Uani 1 1 d . . . . .
H65A H 0.2727 0.3149 0.1779 0.047 Uiso 1 1 calc R . . . .
H65B H 0.2865 0.3081 0.2556 0.047 Uiso 1 1 calc R . . . .
C45 C 0.5718(2) 0.1325(4) -0.0346(3) 0.0427(14) Uani 1 1 d . . . . .
H45A H 0.5723 0.0751 -0.0358 0.051 Uiso 1 1 calc R . . . .
H45B H 0.5464 0.1504 -0.0672 0.051 Uiso 1 1 calc R . . . .
C22 C 0.6123(2) 0.4262(4) 0.5546(3) 0.0403(14) Uani 1 1 d . . . . .
C18 C 0.6111(2) 0.6478(4) 0.5573(3) 0.0387(13) Uani 1 1 d . . . . .
C66 C 0.2830(2) 0.2010(4) 0.2096(4) 0.0442(15) Uani 1 1 d . . . . .
H66A H 0.2532 0.1912 0.2140 0.053 Uiso 1 1 calc R . . . .
H66B H 0.2860 0.1815 0.1664 0.053 Uiso 1 1 calc R . . . .
C24 C 0.6721(2) 0.4464(5) 0.5125(3) 0.0456(15) Uani 1 1 d . . . . .
C10 C 0.5729(2) 0.8921(4) 0.5037(3) 0.0406(14) Uani 1 1 d . . . . .
H10 H 0.5489 0.8676 0.5204 0.049 Uiso 1 1 calc R . . . .
C130 C 0.2568(2) 0.5947(5) 0.0438(3) 0.0465(16) Uani 1 1 d . . . . .
C40 C 0.5247(2) 0.3042(4) 0.3228(3) 0.0373(13) Uani 1 1 d . . . . .
H40 H 0.5221 0.3088 0.3669 0.045 Uiso 1 1 calc R . . . .
C27 C 0.6501(2) 0.2791(5) 0.4578(3) 0.0465(16) Uani 1 1 d . . . . .
H27 H 0.6714 0.3088 0.4388 0.056 Uiso 1 1 calc R . . . .
C82 C 0.3072(2) 1.0125(4) 0.1366(3) 0.0412(14) Uani 1 1 d . . . . .
H82A H 0.3025 1.0688 0.1412 0.049 Uiso 1 1 calc R . . . .
H82B H 0.3052 1.0013 0.0898 0.049 Uiso 1 1 calc R . . . .
C17 C 0.6472(2) 0.6588(5) 0.5321(3) 0.0432(14) Uani 1 1 d . . . . .
C23 C 0.6554(2) 0.5240(4) 0.5259(3) 0.0428(14) Uani 1 1 d . . . . .
C60 C 0.6224(2) 0.9636(4) 0.1142(3) 0.0376(13) Uani 1 1 d . . . . .
H60A H 0.5955 0.9832 0.0862 0.045 Uiso 1 1 calc R . . . .
H60B H 0.6240 0.9835 0.1589 0.045 Uiso 1 1 calc R . . . .
C20 C 0.5957(2) 0.5746(4) 0.5683(3) 0.0404(14) Uani 1 1 d . . . . .
H20 H 0.5709 0.5676 0.5860 0.049 Uiso 1 1 calc R . . . .
C122 C 0.7637(3) 0.5411(7) 0.6996(5) 0.064(2) Uani 1 1 d . . . . .
C26 C 0.6517(2) 0.3076(4) 0.5276(3) 0.0416(14) Uani 1 1 d . . . . .
H26 H 0.6278 0.2819 0.5437 0.050 Uiso 1 1 calc R . . . .
C12 C 0.6242(2) 0.8973(4) 0.6142(3) 0.0443(15) Uani 1 1 d . . . . .
H12A H 0.6033 0.8743 0.6375 0.053 Uiso 1 1 calc R . . . .
H12B H 0.6533 0.8820 0.6375 0.053 Uiso 1 1 calc R . . . .
C25 C 0.6712(2) 0.5972(4) 0.5158(3) 0.0462(15) Uani 1 1 d . . . . .
H25 H 0.6964 0.6046 0.4991 0.055 Uiso 1 1 calc R . . . .
C131 C 0.2592(2) 0.6346(5) -0.0120(3) 0.0499(17) Uani 1 1 d . . . . .
H131 H 0.2698 0.6103 -0.0460 0.060 Uiso 1 1 calc R . . . .
C61 C 0.6605(2) 0.9945(4) 0.0887(3) 0.0414(14) Uani 1 1 d . . . . .
H61A H 0.6588 1.0518 0.0855 0.050 Uiso 1 1 calc R . . . .
H61B H 0.6875 0.9809 0.1197 0.050 Uiso 1 1 calc R . . . .
O19 O 0.7616(3) 0.5521(8) 0.7558(5) 0.119(4) Uani 1 1 d . . . . .
C135 C 0.2415(2) 0.6286(5) 0.0941(4) 0.0512(17) Uani 1 1 d . . . . .
H135 H 0.2404 0.6000 0.1325 0.061 Uiso 1 1 calc R . . . .
O13 O 0.4417(3) 0.6152(7) 0.2899(5) 0.106(3) Uani 1 1 d . . . . .
C21 C 0.6190(2) 0.5121(4) 0.5518(3) 0.0401(13) Uani 1 1 d . . . . .
O14 O 0.4485(3) 0.4924(6) 0.2898(5) 0.105(3) Uani 1 1 d . . . . .
C15 C 0.5694(3) 0.9809(5) 0.5061(3) 0.0555(19) Uani 1 1 d . . . . .
H15A H 0.5913 1.0042 0.4847 0.067 Uiso 1 1 calc R . . . .
H15B H 0.5408 0.9970 0.4812 0.067 Uiso 1 1 calc R . . . .
O20 O 0.7532(3) 0.5907(6) 0.6582(6) 0.116(3) Uani 1 1 d . . . . .
C132 C 0.2458(2) 0.7118(5) -0.0173(4) 0.0518(17) Uani 1 1 d . . . . .
H132 H 0.2474 0.7408 -0.0552 0.062 Uiso 1 1 calc R . . . .
C134 C 0.2277(2) 0.7053(5) 0.0875(4) 0.057(2) Uani 1 1 d . . . . .
H134 H 0.2165 0.7294 0.1210 0.068 Uiso 1 1 calc R . . . .
C133 C 0.2303(2) 0.7462(5) 0.0321(4) 0.0538(18) Uani 1 1 d . . . . .
H133 H 0.2213 0.7989 0.0280 0.065 Uiso 1 1 calc R . . . .
C30 C 0.7032(3) 0.1981(5) 0.5709(4) 0.062(2) Uani 1 1 d . . . . .
H30A H 0.6807 0.1683 0.5860 0.074 Uiso 1 1 calc R . . . .
H30B H 0.7312 0.1860 0.6001 0.074 Uiso 1 1 calc R . . . .
C13 C 0.6203(3) 0.9853(5) 0.6145(4) 0.0551(18) Uani 1 1 d . . . . .
H13A H 0.6430 1.0085 0.5951 0.066 Uiso 1 1 calc R . . . .
H13B H 0.6245 1.0038 0.6601 0.066 Uiso 1 1 calc R . . . .
C0AA C 0.6604(3) 0.1927(6) 0.4570(4) 0.063(2) Uani 1 1 d . . . . .
H0AA H 0.6604 0.1764 0.4118 0.076 Uiso 1 1 calc R . . . .
H0AB H 0.6378 0.1628 0.4721 0.076 Uiso 1 1 calc R . . . .
C31 C 0.6940(3) 0.2848(5) 0.5736(3) 0.0538(19) Uani 1 1 d . . . . .
H31A H 0.7178 0.3143 0.5616 0.065 Uiso 1 1 calc R . . . .
H31B H 0.6927 0.2992 0.6188 0.065 Uiso 1 1 calc R . . . .
C29 C 0.7043(3) 0.1744(6) 0.5011(4) 0.070(3) Uani 1 1 d . . . . .
H29A H 0.7106 0.1183 0.4993 0.084 Uiso 1 1 calc R . . . .
H29B H 0.7272 0.2035 0.4859 0.084 Uiso 1 1 calc R . . . .
C124 C 0.7849(3) 0.4075(7) 0.7237(4) 0.071(3) Uani 1 1 d . . . . .
H124 H 0.7798 0.4146 0.7663 0.085 Uiso 1 1 calc R . . . .
C14 C 0.5758(3) 1.0121(6) 0.5757(4) 0.062(2) Uani 1 1 d . . . . .
H14A H 0.5530 0.9923 0.5967 0.075 Uiso 1 1 calc R . . . .
H14B H 0.5744 1.0695 0.5751 0.075 Uiso 1 1 calc R . . . .
C123 C 0.7790(2) 0.4679(6) 0.6807(4) 0.062(2) Uani 1 1 d . . . . .
C86 C 0.4850(3) 0.5642(5) 0.2255(4) 0.065(2) Uani 1 1 d D . . . .
C28 C 0.5000 0.9344(9) 0.0000 0.067(3) Uiso 1 2 d S T P . .
H28A H 0.5029 0.9767 -0.0286 0.101 Uiso 1 1 d R . . . .
H28B H 0.5176 0.8919 -0.0080 0.101 Uiso 1 1 d R . . . .
H28C H 0.4706 0.9181 -0.0080 0.101 Uiso 1 1 d R . . . .
C125 C 0.7977(3) 0.3382(7) 0.7063(6) 0.080(3) Uani 1 1 d . . . . .
H125 H 0.7997 0.2949 0.7349 0.096 Uiso 1 1 calc R . . . .
C101 C 0.7485(4) 0.3550(7) 0.3792(7) 0.045(3) Uiso 0.5 1 d D U . . .
H101 H 0.7686 0.3568 0.4196 0.054 Uiso 0.5 1 calc R . . . .
C89 C 0.5391(4) 0.5765(6) 0.1420(6) 0.086(3) Uani 1 1 d D . . . .
H89 H 0.5600 0.5812 0.1160 0.103 Uiso 1 1 calc R . . . .
C87 C 0.4999(4) 0.4990(6) 0.2036(6) 0.087(3) Uani 1 1 d D . . . .
H87 H 0.4914 0.4497 0.2166 0.105 Uiso 1 1 calc R . . . .
C126 C 0.8086(3) 0.3307(9) 0.6423(7) 0.093(4) Uani 1 1 d . . . . .
H126 H 0.8200 0.2837 0.6296 0.111 Uiso 1 1 calc R . . . .
O136 O 0.5121(4) 0.9561(8) 0.0600(6) 0.065(3) Uiso 0.5 1 d D . . . .
H136 H 0.5308 0.9262 0.0944 0.097 Uiso 0.5 1 d DR . . . .
C99 C 0.7447(7) 0.4938(11) 0.3884(14) 0.081(5) Uani 0.5 1 d . U . . .
C128 C 0.7873(4) 0.4625(8) 0.6188(5) 0.084(3) Uani 1 1 d . . . . .
H128 H 0.7830 0.5055 0.5898 0.101 Uiso 1 1 calc R . . . .
C91 C 0.4942(4) 0.6356(6) 0.2040(6) 0.084(3) Uani 1 1 d D . . . .
H91 H 0.4827 0.6810 0.2195 0.101 Uiso 1 1 calc R . . . .
C102 C 0.7377(4) 0.2842(8) 0.3524(6) 0.043(3) Uiso 0.5 1 d D U . . .
H102 H 0.7475 0.2383 0.3760 0.052 Uiso 0.5 1 calc R . . . .
C95 C 0.5697(5) 0.5015(9) 0.3790(7) 0.058(4) Uiso 0.5 1 d D . . . .
H95 H 0.5676 0.4499 0.3940 0.070 Uiso 0.5 1 calc R . . . .
C100 C 0.7325(5) 0.4234(9) 0.3526(7) 0.055(3) Uiso 0.5 1 d D U . . .
C104 C 0.6980(5) 0.3496(8) 0.2610(8) 0.059(4) Uiso 0.5 1 d D U . . .
H104 H 0.6808 0.3479 0.2180 0.071 Uiso 0.5 1 calc R . . . .
C103 C 0.7128(5) 0.2800(9) 0.2912(7) 0.053(3) Uiso 0.5 1 d D U . . .
H103 H 0.7058 0.2316 0.2699 0.064 Uiso 0.5 1 calc R . . . .
C90 C 0.5201(5) 0.6411(7) 0.1599(6) 0.094(4) Uani 1 1 d D . . . .
H90 H 0.5247 0.6900 0.1418 0.113 Uiso 1 1 calc R . . . .
C105 C 0.7069(6) 0.4206(11) 0.2904(8) 0.073(5) Uiso 0.5 1 d D U . . .
H105 H 0.6958 0.4669 0.2685 0.087 Uiso 0.5 1 calc R . . . .
C127 C 0.8019(4) 0.3933(9) 0.6011(6) 0.093(4) Uani 1 1 d . . . . .
H127 H 0.8076 0.3882 0.5587 0.112 Uiso 1 1 calc R . . . .
O21 O 0.7769(6) 0.4935(10) 0.4325(11) 0.101(5) Uani 0.5 1 d . U . . .
C94 C 0.5947(5) 0.5158(8) 0.3342(7) 0.061(4) Uiso 0.5 1 d D . . . .
H94 H 0.6078 0.4745 0.3157 0.073 Uiso 0.5 1 calc R . . . .
O18 O 0.6335(6) 0.5578(13) 0.2391(9) 0.104(5) Uiso 0.5 1 d . . . . .
C88 C 0.5284(6) 0.5048(8) 0.1612(8) 0.116(5) Uani 1 1 d D . . . .
H88 H 0.5400 0.4594 0.1460 0.139 Uiso 1 1 calc R . . . .
C92 C 0.6243(7) 0.6044(15) 0.2706(10) 0.083(6) Uiso 0.5 1 d D . . . .
C96 C 0.5477(6) 0.5600(8) 0.4025(10) 0.079(5) Uiso 0.5 1 d D . . . .
H96 H 0.5278 0.5480 0.4288 0.095 Uiso 0.5 1 calc R . . . .
C93 C 0.6003(7) 0.5918(8) 0.3171(10) 0.080(5) Uiso 0.5 1 d D . . . .
C97 C 0.5550(7) 0.6361(10) 0.3876(10) 0.077(5) Uiso 0.5 1 d D . . . .
H97 H 0.5410 0.6774 0.4047 0.093 Uiso 0.5 1 calc R . . . .
O22 O 0.7212(7) 0.5495(10) 0.3766(12) 0.115(6) Uani 0.5 1 d . U . . .
O17 O 0.6306(11) 0.676(2) 0.2624(16) 0.173(11) Uiso 0.5 1 d . . . . .
C98 C 0.5830(9) 0.6511(13) 0.3473(14) 0.122(10) Uiso 0.5 1 d D . . . .
H98 H 0.5904 0.7033 0.3402 0.147 Uiso 0.5 1 calc R . . . .
C109 C 0.4945(3) 0.0495(7) 0.2049(5) 0.063(3) Uiso 0.8 1 d D . . . .
H109 H 0.4808 0.0387 0.1610 0.076 Uiso 0.5 1 calc R . . A 1
H10A H 0.4744 0.0349 0.1666 0.076 Uiso 0.3 1 calc R . . B 2
C106 C 0.5990(4) 0.0238(8) 0.3172(6) 0.042(3) Uiso 0.5 1 d . . . C 1
C107 C 0.5549(5) 0.0471(9) 0.2913(6) 0.052(3) Uiso 0.5 1 d D . . C 1
O26 O 0.6175(5) -0.0138(9) 0.2816(7) 0.074(3) Uiso 0.5 1 d . . . C 1
C108 C 0.5361(5) 0.0301(12) 0.2276(8) 0.064(4) Uiso 0.5 1 d D . . C 1
H108 H 0.5521 0.0052 0.2001 0.077 Uiso 0.5 1 calc R . . C 1
C110 C 0.4725(7) 0.0846(14) 0.2459(9) 0.076(5) Uiso 0.5 1 d D . . C 1
H110 H 0.4430 0.0965 0.2305 0.091 Uiso 0.5 1 calc R . . C 1
C112 C 0.5342(6) 0.0858(11) 0.3316(9) 0.062(4) Uiso 0.5 1 d D . . C 1
H112 H 0.5487 0.1005 0.3742 0.074 Uiso 0.5 1 calc R . . C 1
O25 O 0.6177(5) 0.0430(10) 0.3734(8) 0.087(4) Uiso 0.5 1 d . . . C 1
C111 C 0.4918(7) 0.1032(15) 0.3089(10) 0.083(6) Uiso 0.5 1 d D . . C 1
H111 H 0.4758 0.1279 0.3365 0.100 Uiso 0.5 1 calc R . . C 1
O1A O 0.6487(3) 0.2053(6) 0.1775(5) 0.051(2) Uiso 0.5 1 d D . . D 1
H1A H 0.6297 0.2399 0.1718 0.077 Uiso 0.5 1 calc DGR . . D 1
C120 C 0.6379(5) 0.1468(9) 0.2174(7) 0.051(3) Uiso 0.5 1 d D . . D 1
H12C H 0.6096 0.1257 0.1974 0.076 Uiso 0.5 1 calc GR . . D 1
H12D H 0.6371 0.1684 0.2603 0.076 Uiso 0.5 1 calc GR . . D 1
H12E H 0.6593 0.1053 0.2224 0.076 Uiso 0.5 1 calc GR . . D 1
O24 O 0.6172(6) 0.1177(11) 0.2016(8) 0.049(4) Uiso 0.3 1 d D . . C 2
C119 C 0.6091(5) 0.1081(10) 0.2585(7) 0.026(3) Uiso 0.3 1 d D . . C 2
O27 O 0.5445(6) 0.1920(12) 0.4700(9) 0.080(5) Uiso 0.4 1 d D . . . .
H27A H 0.5687 0.2211 0.4603 0.120 Uiso 0.4 1 d DR . . . .
C121 C 0.5171(11) 0.228(2) 0.501(2) 0.112(11) Uiso 0.4 1 d D . . . .
H12F H 0.4936 0.2492 0.4697 0.168 Uiso 0.4 1 d R . . . .
H12G H 0.5064 0.1914 0.5282 0.168 Uiso 0.4 1 d R . . . .
H12H H 0.5314 0.2696 0.5282 0.168 Uiso 0.4 1 d R . . . .
C117 C 0.5362(5) 0.0704(13) 0.2035(9) 0.039(4) Uiso 0.3 1 d D . . C 2
H117 H 0.5456 0.0716 0.1636 0.047 Uiso 0.3 1 calc R . . C 2
C116 C 0.5634(6) 0.0892(11) 0.2612(7) 0.031(4) Uiso 0.3 1 d D . . C 2
C115 C 0.5550(8) 0.0921(14) 0.3225(10) 0.047(5) Uiso 0.3 1 d D . . C 2
H115 H 0.5759 0.1045 0.3605 0.056 Uiso 0.3 1 calc R . . C 2
C114 C 0.5124(8) 0.0747(16) 0.3228(12) 0.053(6) Uiso 0.3 1 d D . . C 2
H114 H 0.5029 0.0792 0.3625 0.063 Uiso 0.3 1 calc R . . C 2
C113 C 0.4835(9) 0.0510(18) 0.2668(9) 0.056(6) Uiso 0.3 1 d D . . C 2
H113 H 0.4555 0.0354 0.2703 0.067 Uiso 0.3 1 calc R . . C 2
O23 O 0.6348(8) 0.1141(14) 0.3047(11) 0.073(5) Uiso 0.3 1 d . . . C 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
O8 C51 1.196(7) . ?
O11 C75 1.206(7) . ?
O12 C77 1.209(7) . ?
O6 C47 1.220(7) . ?
O5 C55 1.217(7) . ?
O7 C56 1.204(7) . ?
O9 C72 1.202(7) . ?
O10 C69 1.208(7) . ?
N10 C51 1.406(7) . ?
N10 C56 1.395(7) . ?
N10 C58 1.472(7) . ?
N2 C80 1.453(7) . ?
N2 C9 1.252(7) . ?
N12 C77 1.391(7) . ?
N12 C75 1.399(7) . ?
N12 C79 1.480(7) . ?
N7 C36 1.256(8) . ?
N7 C41 1.463(7) . ?
O1 C19 1.207(8) . ?
N3 C7 1.269(8) . ?
N3 C59 1.461(7) . ?
O3 C22 1.195(9) . ?
O2 C16 1.195(9) . ?
N1 C1 1.275(8) . ?
N1 C10 1.461(8) . ?
N4 C19 1.401(9) . ?
N4 C16 1.386(9) . ?
N4 C11 1.481(9) . ?
N8 C39 1.278(8) . ?
N8 C63 1.465(7) . ?
N11 C64 1.473(7) . ?
N11 C72 1.399(7) . ?
N11 C69 1.401(7) . ?
O16 C129 1.225(9) . ?
N9 C42 1.479(7) . ?
N9 C55 1.399(7) . ?
N9 C47 1.395(7) . ?
N6 C32 1.255(8) . ?
N6 C27 1.473(8) . ?
O4 C24 1.223(9) . ?
C4 C3 1.393(8) . ?
C4 C5 1.374(8) . ?
C4 C9 1.486(8) . ?
C129 O15 1.231(9) . ?
C129 C130 1.477(11) . ?
C42 C41 1.541(8) . ?
C42 C43 1.526(7) . ?
N5 C22 1.396(8) . ?
N5 C24 1.361(10) . ?
N5 C26 1.483(9) . ?
C77 C76 1.483(8) . ?
C2 C3 1.394(8) . ?
C2 C1 1.468(8) . ?
C2 C8 1.392(8) . ?
C36 C35 1.468(8) . ?
C6 C5 1.411(8) . ?
C6 C7 1.463(8) . ?
C6 C8 1.387(8) . ?
C49 C48 1.392(8) . ?
C49 C50 1.398(8) . ?
C80 C79 1.522(8) . ?
C80 C81 1.528(8) . ?
C51 C50 1.506(8) . ?
C48 C54 1.393(7) . ?
C48 C47 1.482(8) . ?
C53 C54 1.395(8) . ?
C53 C52 1.384(8) . ?
C75 C74 1.492(8) . ?
C54 C55 1.478(8) . ?
C50 C52 1.390(7) . ?
C74 C76 1.382(7) . ?
C74 C73 1.388(8) . ?
C52 C56 1.498(8) . ?
C46 C41 1.538(8) . ?
C46 C45 1.528(9) . ?
C76 C78 1.389(8) . ?
C70 C71 1.398(7) . ?
C70 C69 1.480(8) . ?
C70 C78 1.392(8) . ?
C58 C59 1.526(7) . ?
C58 C57 1.536(8) . ?
C35 C37 1.388(9) . ?
C35 C34 1.398(8) . ?
C79 C84 1.522(8) . ?
C64 C63 1.528(8) . ?
C64 C65 1.523(9) . ?
C59 C60 1.532(8) . ?
C72 C71 1.482(8) . ?
C67 C68 1.524(9) . ?
C67 C66 1.514(10) . ?
C37 C38 1.409(8) . ?
C34 C33 1.385(8) . ?
C71 C73 1.400(8) . ?
C85 O13 1.206(12) . ?
C85 O14 1.204(12) . ?
C85 C86 1.488(12) . ?
C43 C44 1.534(8) . ?
C33 C32 1.478(9) . ?
C33 C40 1.409(9) . ?
C39 C38 1.469(8) . ?
C81 C82 1.522(9) . ?
C44 C45 1.520(10) . ?
C19 C18 1.506(10) . ?
C16 C17 1.487(10) . ?
C68 C63 1.536(8) . ?
C38 C40 1.398(8) . ?
C11 C10 1.520(9) . ?
C11 C12 1.531(8) . ?
C57 C62 1.512(9) . ?
C62 C61 1.514(9) . ?
C84 C83 1.536(9) . ?
C83 C82 1.516(10) . ?
C65 C66 1.525(9) . ?
C22 C21 1.499(10) . ?
C18 C17 1.379(9) . ?
C18 C20 1.391(10) . ?
C24 C23 1.487(10) . ?
C10 C15 1.537(11) . ?
C130 C131 1.376(11) . ?
C130 C135 1.384(10) . ?
C27 C26 1.536(8) . ?
C27 C0AA 1.525(11) . ?
C17 C25 1.395(10) . ?
C23 C25 1.392(11) . ?
C23 C21 1.398(9) . ?
C60 C61 1.525(9) . ?
C20 C21 1.394(10) . ?
C122 O19 1.212(12) . ?
C122 O20 1.214(15) . ?
C122 C123 1.438(15) . ?
C26 C31 1.535(9) . ?
C12 C13 1.521(11) . ?
C131 C132 1.395(12) . ?
C135 C134 1.391(13) . ?
C15 C14 1.530(10) . ?
C132 C133 1.375(12) . ?
C134 C133 1.377(13) . ?
C30 C31 1.528(11) . ?
C30 C29 1.528(11) . ?
C13 C14 1.548(12) . ?
C0AA C29 1.539(12) . ?
C124 C123 1.365(15) . ?
C124 C125 1.338(16) . ?
C123 C128 1.383(12) . ?
C86 C87 1.339(12) . ?
C86 C91 1.362(12) . ?
C28 O136 1.291(13) . ?
C28 O136 1.291(13) 2_655 ?
C125 C126 1.464(18) . ?
C101 C102 1.356(15) . ?
C101 C100 1.357(15) . ?
C89 C90 1.360(13) . ?
C89 C88 1.365(14) . ?
C87 C88 1.405(14) . ?
C126 C127 1.37(2) . ?
C99 C100 1.44(3) . ?
C99 O21 1.23(3) . ?
C99 O22 1.21(3) . ?
C128 C127 1.360(19) . ?
C91 C90 1.370(13) . ?
C102 C103 1.362(15) . ?
C95 C94 1.378(3) . ?
C95 C96 1.380(3) . ?
C100 C105 1.385(17) . ?
C104 C103 1.391(16) . ?
C104 C105 1.374(17) . ?
C94 C93 1.380(3) . ?
O18 C92 1.12(3) . ?
C92 C93 1.380(3) . ?
C92 O17 1.27(4) . ?
C96 C97 1.380(3) . ?
C93 C98 1.380(3) . ?
C97 C98 1.379(3) . ?
C109 C108 1.355(15) . ?
C109 C110 1.362(17) . ?
C109 C117 1.385(16) . ?
C109 C113 1.416(18) . ?
C106 C107 1.45(2) . ?
C106 O26 1.231(19) . ?
C106 O25 1.25(2) . ?
C107 C108 1.374(16) . ?
C107 C112 1.354(17) . ?
C110 C111 1.371(18) . ?
C112 C111 1.370(18) . ?
O1A C120 1.401(17) . ?
O24 C119 1.29(2) . ?
C119 C116 1.51(2) . ?
C119 O23 1.13(3) . ?
O27 C121 1.36(2) . ?
C121 C121 1.08(6) 2_656 ?
C117 C116 1.370(17) . ?
C116 C115 1.370(18) . ?
C115 C114 1.39(2) . ?
C114 C113 1.39(2) . ?

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
C51 N10 C58 122.8(4) . . ?
C56 N10 C51 112.4(5) . . ?
C56 N10 C58 124.6(4) . . ?
C9 N2 C80 117.6(5) . . ?
C77 N12 C75 111.8(5) . . ?
C77 N12 C79 121.6(4) . . ?
C75 N12 C79 126.6(5) . . ?
C36 N7 C41 117.2(5) . . ?
C7 N3 C59 115.5(5) . . ?
C1 N1 C10 117.1(5) . . ?
C19 N4 C11 126.4(5) . . ?
C16 N4 C19 111.5(6) . . ?
C16 N4 C11 122.0(5) . . ?
C39 N8 C63 119.5(5) . . ?
C72 N11 C64 123.7(5) . . ?
C72 N11 C69 111.4(5) . . ?
C69 N11 C64 124.3(5) . . ?
C55 N9 C42 122.7(4) . . ?
C47 N9 C42 126.0(4) . . ?
C47 N9 C55 111.3(5) . . ?
C32 N6 C27 114.6(6) . . ?
C3 C4 C9 120.4(5) . . ?
C5 C4 C3 120.2(5) . . ?
C5 C4 C9 119.1(5) . . ?
O16 C129 O15 123.4(8) . . ?
O16 C129 C130 118.1(6) . . ?
O15 C129 C130 118.6(7) . . ?
N9 C42 C41 110.5(4) . . ?
N9 C42 C43 110.9(4) . . ?
C43 C42 C41 113.4(5) . . ?
C22 N5 C26 122.7(6) . . ?
C24 N5 C22 112.5(6) . . ?
C24 N5 C26 124.5(6) . . ?
O12 C77 N12 126.2(5) . . ?
O12 C77 C76 127.7(5) . . ?
N12 C77 C76 106.1(4) . . ?
C3 C2 C1 119.0(5) . . ?
C8 C2 C3 118.9(5) . . ?
C8 C2 C1 121.9(5) . . ?
N7 C36 C35 123.0(5) . . ?
C4 C3 C2 120.5(5) . . ?
C5 C6 C7 121.6(5) . . ?
C8 C6 C5 118.9(5) . . ?
C8 C6 C7 119.1(5) . . ?
C4 C5 C6 120.2(5) . . ?
C48 C49 C50 115.3(5) . . ?
N2 C80 C79 109.0(4) . . ?
N2 C80 C81 109.6(4) . . ?
C79 C80 C81 108.7(5) . . ?
O8 C51 N10 125.7(5) . . ?
O8 C51 C50 128.9(5) . . ?
N10 C51 C50 105.4(4) . . ?
C49 C48 C54 121.9(5) . . ?
C49 C48 C47 130.4(5) . . ?
C54 C48 C47 107.7(5) . . ?
C52 C53 C54 115.1(5) . . ?
O11 C75 N12 127.2(5) . . ?
O11 C75 C74 127.0(5) . . ?
N12 C75 C74 105.8(5) . . ?
C48 C54 C53 122.8(5) . . ?
C48 C54 C55 108.3(5) . . ?
C53 C54 C55 129.0(5) . . ?
C49 C50 C51 129.8(5) . . ?
C52 C50 C49 122.2(5) . . ?
C52 C50 C51 107.9(5) . . ?
C76 C74 C75 107.9(5) . . ?
C76 C74 C73 123.8(5) . . ?
C73 C74 C75 128.2(5) . . ?
C53 C52 C50 122.7(5) . . ?
C53 C52 C56 128.9(5) . . ?
C50 C52 C56 108.4(5) . . ?
N3 C7 C6 123.4(5) . . ?
C45 C46 C41 112.6(5) . . ?
C74 C76 C77 108.4(5) . . ?
C74 C76 C78 122.9(5) . . ?
C78 C76 C77 128.5(5) . . ?
C71 C70 C69 107.8(5) . . ?
C78 C70 C71 123.1(5) . . ?
C78 C70 C69 129.0(5) . . ?
N2 C9 C4 121.3(5) . . ?
O5 C55 N9 125.2(5) . . ?
O5 C55 C54 128.6(5) . . ?
N9 C55 C54 106.2(4) . . ?
O7 C56 N10 126.5(5) . . ?
O7 C56 C52 127.8(5) . . ?
N10 C56 C52 105.8(4) . . ?
N10 C58 C59 112.7(4) . . ?
N10 C58 C57 112.0(4) . . ?
C59 C58 C57 109.6(4) . . ?
O6 C47 N9 125.8(5) . . ?
O6 C47 C48 127.7(5) . . ?
N9 C47 C48 106.5(4) . . ?
C37 C35 C36 119.0(5) . . ?
C37 C35 C34 118.7(5) . . ?
C34 C35 C36 122.1(5) . . ?
N1 C1 C2 122.2(5) . . ?
N7 C41 C42 108.9(4) . . ?
N7 C41 C46 107.9(4) . . ?
C46 C41 C42 109.0(5) . . ?
N12 C79 C80 110.9(4) . . ?
N12 C79 C84 111.5(5) . . ?
C80 C79 C84 111.8(5) . . ?
N11 C64 C63 110.7(5) . . ?
N11 C64 C65 110.3(5) . . ?
C65 C64 C63 113.7(5) . . ?
N3 C59 C58 111.8(4) . . ?
N3 C59 C60 106.2(5) . . ?
C58 C59 C60 110.0(5) . . ?
C6 C8 C2 121.2(5) . . ?
O9 C72 N11 125.6(6) . . ?
O9 C72 C71 128.2(6) . . ?
N11 C72 C71 106.1(5) . . ?
C66 C67 C68 111.2(5) . . ?
C35 C37 C38 121.3(5) . . ?
C33 C34 C35 121.6(6) . . ?
C70 C71 C72 108.2(5) . . ?
C70 C71 C73 122.5(5) . . ?
C73 C71 C72 128.9(5) . . ?
C74 C73 C71 113.6(5) . . ?
O13 C85 C86 117.2(8) . . ?
O14 C85 O13 124.0(9) . . ?
O14 C85 C86 118.7(8) . . ?
C42 C43 C44 110.8(5) . . ?
C34 C33 C32 117.9(5) . . ?
C34 C33 C40 119.1(5) . . ?
C40 C33 C32 122.9(5) . . ?
N8 C39 C38 119.5(5) . . ?
C82 C81 C80 112.0(5) . . ?
C45 C44 C43 110.8(5) . . ?
O1 C19 N4 125.9(7) . . ?
O1 C19 C18 128.1(6) . . ?
N4 C19 C18 106.0(5) . . ?
O2 C16 N4 126.4(7) . . ?
O2 C16 C17 127.2(6) . . ?
N4 C16 C17 106.4(6) . . ?
N6 C32 C33 123.1(6) . . ?
C67 C68 C63 112.2(5) . . ?
N8 C63 C64 107.6(4) . . ?
N8 C63 C68 107.6(5) . . ?
C64 C63 C68 109.5(5) . . ?
C37 C38 C39 120.6(5) . . ?
C40 C38 C37 118.8(5) . . ?
C40 C38 C39 120.5(5) . . ?
N4 C11 C10 111.4(5) . . ?
N4 C11 C12 110.9(5) . . ?
C10 C11 C12 112.6(5) . . ?
O10 C69 N11 126.4(6) . . ?
O10 C69 C70 127.2(5) . . ?
N11 C69 C70 106.4(4) . . ?
C62 C57 C58 110.5(5) . . ?
C76 C78 C70 114.0(5) . . ?
C57 C62 C61 110.8(5) . . ?
C79 C84 C83 109.5(5) . . ?
C82 C83 C84 110.5(5) . . ?
C64 C65 C66 110.9(5) . . ?
C44 C45 C46 110.4(5) . . ?
O3 C22 N5 126.5(7) . . ?
O3 C22 C21 127.9(6) . . ?
N5 C22 C21 105.6(6) . . ?
C17 C18 C19 107.2(6) . . ?
C17 C18 C20 122.8(6) . . ?
C20 C18 C19 129.9(6) . . ?
C67 C66 C65 110.0(5) . . ?
O4 C24 N5 126.9(7) . . ?
O4 C24 C23 126.2(7) . . ?
N5 C24 C23 107.0(6) . . ?
N1 C10 C11 109.3(5) . . ?
N1 C10 C15 107.4(5) . . ?
C11 C10 C15 109.9(6) . . ?
C131 C130 C129 118.6(6) . . ?
C131 C130 C135 122.2(8) . . ?
C135 C130 C129 119.2(7) . . ?
C38 C40 C33 120.4(5) . . ?
N6 C27 C26 109.9(5) . . ?
N6 C27 C0AA 108.1(6) . . ?
C0AA C27 C26 111.1(6) . . ?
C83 C82 C81 111.5(5) . . ?
C18 C17 C16 108.8(6) . . ?
C18 C17 C25 122.5(7) . . ?
C25 C17 C16 128.7(6) . . ?
C25 C23 C24 129.1(6) . . ?
C25 C23 C21 123.3(6) . . ?
C21 C23 C24 107.6(6) . . ?
C61 C60 C59 112.2(5) . . ?
C18 C20 C21 115.6(6) . . ?
O19 C122 O20 121.5(12) . . ?
O19 C122 C123 120.0(11) . . ?
O20 C122 C123 118.5(9) . . ?
N5 C26 C27 111.4(5) . . ?
N5 C26 C31 110.3(6) . . ?
C31 C26 C27 111.4(5) . . ?
C13 C12 C11 111.1(5) . . ?
C23 C25 C17 114.6(6) . . ?
C130 C131 C132 118.2(7) . . ?
C62 C61 C60 110.6(5) . . ?
C130 C135 C134 118.7(7) . . ?
C23 C21 C22 107.3(6) . . ?
C20 C21 C22 131.6(6) . . ?
C20 C21 C23 121.1(7) . . ?
C14 C15 C10 112.7(6) . . ?
C133 C132 C131 120.3(8) . . ?
C133 C134 C135 119.8(7) . . ?
C132 C133 C134 120.8(8) . . ?
C31 C30 C29 109.9(7) . . ?
C12 C13 C14 111.2(7) . . ?
C27 C0AA C29 111.3(7) . . ?
C30 C31 C26 112.1(6) . . ?
C30 C29 C0AA 108.5(7) . . ?
C125 C124 C123 120.5(10) . . ?
C15 C14 C13 108.6(7) . . ?
C124 C123 C122 119.5(8) . . ?
C124 C123 C128 122.9(11) . . ?
C128 C123 C122 117.6(10) . . ?
C87 C86 C85 117.6(8) . . ?
C87 C86 C91 121.9(9) . . ?
C91 C86 C85 120.4(8) . . ?
O136 C28 O136 146.3(17) . 2_655 ?
C124 C125 C126 118.3(12) . . ?
C100 C101 C102 124.8(13) . . ?
C90 C89 C88 120.3(11) . . ?
C86 C87 C88 118.8(10) . . ?
C127 C126 C125 118.3(12) . . ?
O21 C99 C100 118.7(19) . . ?
O22 C99 C100 118(2) . . ?
O22 C99 O21 123(2) . . ?
C127 C128 C123 117.5(12) . . ?
C86 C91 C90 119.2(10) . . ?
C101 C102 C103 119.0(13) . . ?
C94 C95 C96 121.7(16) . . ?
C101 C100 C99 118.8(15) . . ?
C101 C100 C105 116.9(15) . . ?
C105 C100 C99 124.2(17) . . ?
C105 C104 C103 123.0(16) . . ?
C102 C103 C104 117.3(14) . . ?
C89 C90 C91 120.0(10) . . ?
C104 C105 C100 118.6(17) . . ?
C128 C127 C126 122.2(11) . . ?
C95 C94 C93 118.3(15) . . ?
C89 C88 C87 119.2(11) . . ?
O18 C92 C93 124(2) . . ?
O18 C92 O17 123(2) . . ?
O17 C92 C93 112(2) . . ?
C95 C96 C97 119.4(18) . . ?
C92 C93 C94 117.1(16) . . ?
C98 C93 C94 119.7(17) . . ?
C98 C93 C92 123.2(17) . . ?
C98 C97 C96 119(2) . . ?
C97 C98 C93 121(2) . . ?
C108 C109 C110 119.1(14) . . ?
C117 C109 C113 116.2(15) . . ?
O26 C106 C107 118.1(13) . . ?
O26 C106 O25 121.2(15) . . ?
O25 C106 C107 120.7(13) . . ?
C108 C107 C106 119.4(13) . . ?
C112 C107 C106 117.7(13) . . ?
C112 C107 C108 122.9(15) . . ?
C109 C108 C107 118.7(15) . . ?
C109 C110 C111 121.8(19) . . ?
C107 C112 C111 117.9(18) . . ?
C112 C111 C110 119(2) . . ?
O24 C119 C116 116.6(15) . . ?
O23 C119 O24 122(2) . . ?
O23 C119 C116 121.2(17) . . ?
C121 C121 O27 136(4) 2_656 . ?
C116 C117 C109 118.3(16) . . ?
C117 C116 C119 117.1(14) . . ?
C115 C116 C119 114.3(15) . . ?
C115 C116 C117 128.6(18) . . ?
C116 C115 C114 112.5(19) . . ?
C113 C114 C115 122(2) . . ?
C114 C113 C109 122(2) . . ?

_olex2_date_sample_data_collection 2019-08-16
_olex2_date_sample_submission    2019-07-08
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a mylar loop in perfluoroether oil'
_olex2_submission_original_sample_id HH_PlcyCage138RR_130K
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_hh_plcycage99_130k_0m
_audit_block_doi                 10.5517/ccdc.csd.cc2665qb
_database_code_depnum_ccdc_archive 'CCDC 2031731'
loop_
_citation_id
_citation_doi
_citation_year
1 10.26434/chemrxiv.12957314.v1 2020
loop_
_audit_author_name
_audit_author_address
'Prescimone A.'
;University of Basel
Switzerland
;
_audit_update_record             
;
2020-09-13 deposited with the CCDC.	2021-02-11 downloaded from the CCDC.
;
_audit_creation_date             2019-08-14
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
loop_
_audit_author_email
alessandro.prescimone@unibas.ch
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C84 H78 N12 O12, 5(C6 H5 N O2), C0.6 H1.5 O0.3, 0.9(C H4 O)'
_chemical_formula_sum            'C115.50 H108.10 N17 O23.20'
_chemical_formula_weight         2105.48
_chemical_absolute_configuration ad
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 1 2 1'
_space_group_name_Hall           'C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   31.8864(19)
_cell_length_b                   17.2148(10)
_cell_length_c                   20.9689(12)
_cell_angle_alpha                90
_cell_angle_beta                 102.403(3)
_cell_angle_gamma                90
_cell_volume                     11241.6(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    130
_cell_measurement_theta_max      70.319
_cell_measurement_theta_min      3.918
_shelx_estimated_absorpt_T_max   0.965
_shelx_estimated_absorpt_T_min   0.839
_exptl_absorpt_coefficient_mu    0.728
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.6898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0756 before and 0.0462 after correction.
The Ratio of minimum to maximum transmission is 0.9157.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             4423
_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of methanol and nitro-benzene  by solvent layering'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            74017
_diffrn_reflns_point_group_measured_fraction_full 0.927
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.336
_diffrn_reflns_theta_min         2.838
_diffrn_ambient_temperature      130
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.778
_reflns_Friedel_fraction_full    0.852
_reflns_Friedel_fraction_max     0.814
_reflns_number_gt                18073
_reflns_number_total             19234
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.318
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 
;
 Flack x determined using 7307 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.14(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1472
_refine_ls_number_reflns         19234
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0713
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1665P)²+7.3061P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2088
_refine_ls_wR_factor_ref         0.2145
_refine_special_details          
'there is a lot of solvent molecules in the structure. Many of them are not fully occupied and had to be restrained to be chemically reasonable.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C120-C115 \\sim C116-C115 \\sim C116-C117 \\sim C118-C117 \\sim C118-C119
\\sim C120-C119
 with sigma of 0.02
 C95-C94 \\sim C95-C96 \\sim C93-C94 \\sim C92-C93 \\sim C91-C92 \\sim C91-C96
 with sigma of 0.02
 C126-C125 \\sim C125-C124 \\sim C123-C124 \\sim C123-C122 \\sim C121-C122
\\sim C126-C121
 with sigma of 0.02
 C102-C97 \\sim C102-C101 \\sim C100-C99 \\sim C98-C97 \\sim C98-C99 \\sim
C100-C101 \\sim C100-C99
 with sigma of 0.02
3. Restrained planarity
 C120, C115, C116, C117, C118, C119, N18
 with sigma of 0.1
 C93, C92, C91, C96, C95, C94, N14, O16, O15
 with sigma of 0.1
 C121, C126, C125, C124, C123, C122
 with sigma of 0.1
 N15, C97, C98, C99, C100, C101, C102
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O15) = Uanis(O16) = Uanis(N14)
Uanis(C128) = Uanis(O29)
Uanis(C97) = Uanis(C98) = Uanis(C99) = Uanis(C100) = Uanis(C101) = Uanis(C102)
Uanis(C92) = Uanis(C93) = Uanis(C94) = Uanis(C95) = Uanis(C96) = Uanis(C91)
Uanis(O17) = Uanis(N15) = Uanis(O18)
Uanis(O16) = Uanis(N14) = Uanis(O15)
5. Others
 Fixed Sof: C122(0.5) H122(0.5) C124(0.5) H124(0.5) C121(0.5) C123(0.5)
 H123(0.5) N19(0.5) C125(0.5) H125(0.5) C126(0.5) H126(0.5) O22(0.5) O21(0.5)
 C93(0.5) H93(0.5) C95(0.5) H95(0.5) C92(0.5) H92(0.5) C91(0.5) O16(0.5)
 C94(0.5) H94(0.5) N14(0.5) C96(0.5) H96(0.5) O15(0.5) O28(0.3) H28(0.6)
 C129(0.6) H12C(0.3) H12D(0.3) H12E(0.3) C117(0.5) H117(0.5) C116(0.5)
 H116(0.5) C118(0.5) H118(0.5) N15(0.5) C115(0.5) O17(0.5) O18(0.5) C120(0.5)
 H120(0.5) C119(0.5) H119(0.5) O24(0.5) N18(0.5) O23(0.5) C97(0.5) C98(0.5)
 H98(0.5) C102(0.5) H102(0.5) C99(0.5) H99(0.5) C101(0.5) H101(0.5) C100(0.5)
 H100(0.5) O27(0.5) H27A(0.5) C127(0.5) H12F(0.5) H12G(0.5) H12H(0.5) O29(0.4)
 H29(0.4) C128(0.4) H12I(0.4) H12J(0.4) H12K(0.4)
6.a Riding coordinates:
 O28(H28), C129(H12C,H12D,H12E), O29(H29), C128(H12I,H12J,H12K)
6.b Ternary CH refined with riding coordinates:
 C57(H57), C27(H27), C42(H42), C11(H11), C58(H58), C41(H41), C26(H26),
 C10(H10), C79(H79), C63(H63), C80(H80), C64(H64)
6.c Secondary CH2 refined with riding coordinates:
 C59(H59A,H59B), C62(H62A,H62B), C29(H29A,H29B), C28(H28A,H28B), C14(H14A,
 H14B), C61(H61A,H61B), C30(H30A,H30B), C43(H43A,H43B), C44(H44A,H44B),
 C15(H15A,H15B), C45(H45A,H45B), C13(H13A,H13B), C12(H12A,H12B), C60(H60A,H60B),
  C31(H31A,H31B), C81(H81A,H81B), C46(H46A,H46B), C84(H84A,H84B), C66(H66A,
 H66B), C83(H83A,H83B), C65(H65A,H65B), C67(H67A,H67B), C82(H82A,H82B),
 C68(H68A,H68B)
6.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C34(H34), C49(H49), C53(H53), C39(H39), C36(H36), C40(H40), C1(H1),
 C32(H32), C8(H8), C37(H37), C3(H3), C20(H20), C6(H6), C9(H9), C25(H25),
 C110(H110), C114(H114), C112(H112), C113(H113), C78(H78), C73(H73), C111(H111),
  C104(H104), C105(H105), C122(H122), C86(H86), C106(H106), C88(H88),
 C108(H108), C90(H90), C124(H124), C123(H123), C125(H125), C89(H89), C126(H126),
  C107(H107), C87(H87), C93(H93), C95(H95), C92(H92), C94(H94), C96(H96),
 C117(H117), C116(H116), C118(H118), C120(H120), C119(H119), C98(H98),
 C102(H102), C99(H99), C101(H101), C100(H100)
6.e Idealised Me refined as rotating group:
 C127(H12F,H12G,H12H)
6.f Idealised tetrahedral OH refined as rotating group:
 O27(H27A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
O5 O 0.44083(11) 0.31925(19) 1.04023(16) 0.0366(7) Uani 1 1 d . . . . .
O4 O 0.65239(12) 0.31591(19) 0.90122(14) 0.0362(7) Uani 1 1 d . . . . .
O7 O 0.45289(11) 0.67044(19) 1.05605(16) 0.0356(7) Uani 1 1 d . . . . .
O3 O 0.67755(13) 0.3091(2) 0.69398(16) 0.0397(8) Uani 1 1 d . . . . .
O8 O 0.32860(11) 0.68729(19) 0.89876(16) 0.0364(7) Uani 1 1 d . . . . .
O6 O 0.32030(11) 0.3416(2) 0.87759(17) 0.0393(8) Uani 1 1 d . . . . .
O2 O 0.66914(12) 0.6538(2) 0.68313(15) 0.0373(7) Uani 1 1 d . . . . .
O1 O 0.63557(14) 0.6598(2) 0.88458(17) 0.0446(9) Uani 1 1 d . . . . .
N9 N 0.38129(12) 0.3096(2) 0.95521(16) 0.0266(7) Uani 1 1 d . . . . .
O10 O 0.41522(15) 0.6751(2) 0.4278(2) 0.0516(10) Uani 1 1 d . . . . .
N2 N 0.42922(13) 0.7988(2) 0.89192(17) 0.0299(8) Uani 1 1 d . . . . .
O12 O 0.43881(15) 0.3249(3) 0.4132(2) 0.0547(10) Uani 1 1 d . . . . .
N5 N 0.66684(12) 0.2908(2) 0.79879(17) 0.0286(7) Uani 1 1 d . . . . .
N6 N 0.59878(12) 0.1812(2) 0.78559(17) 0.0283(7) Uani 1 1 d . . . . .
N7 N 0.41790(12) 0.2131(2) 0.86361(17) 0.0298(8) Uani 1 1 d . . . . .
O11 O 0.31789(14) 0.2928(3) 0.4947(2) 0.0565(11) Uani 1 1 d . . . . .
N11 N 0.38029(14) 0.2873(3) 0.45556(18) 0.0367(9) Uani 1 1 d . . . . .
N10 N 0.39123(12) 0.7002(2) 0.97798(17) 0.0268(7) Uani 1 1 d . . . . .
N1 N 0.58657(13) 0.7975(2) 0.75409(18) 0.0321(8) Uani 1 1 d . . . . .
N4 N 0.65302(13) 0.6786(2) 0.78422(18) 0.0321(8) Uani 1 1 d . . . . .
N8 N 0.42970(13) 0.1965(3) 0.56408(18) 0.0357(9) Uani 1 1 d . . . . .
O26 O 0.73302(15) 0.5907(3) 0.9007(2) 0.0610(11) Uani 1 1 d . . . . .
O9 O 0.29577(15) 0.6332(3) 0.5102(2) 0.0598(11) Uani 1 1 d . . . . .
N17 N 0.73001(15) 0.5553(3) 0.9506(2) 0.0481(11) Uani 1 1 d . . . . .
O25 O 0.71748(17) 0.5842(3) 0.9967(2) 0.0664(13) Uani 1 1 d . . . . .
N3 N 0.39236(15) 0.7768(3) 0.58219(19) 0.0424(10) Uani 1 1 d . . . . .
C47 C 0.41276(15) 0.3488(3) 1.0005(2) 0.0288(9) Uani 1 1 d . . . . .
N12 N 0.35431(15) 0.6752(3) 0.47052(19) 0.0407(10) Uani 1 1 d . . . . .
C57 C 0.39159(14) 0.7861(2) 0.9811(2) 0.0277(8) Uani 1 1 d . . . . .
H57 H 0.3659 0.8050 0.9486 0.033 Uiso 1 1 calc R . . . .
C24 C 0.66933(15) 0.3343(3) 0.7437(2) 0.0295(9) Uani 1 1 d . . . . .
C33 C 0.52564(15) 0.2218(3) 0.7737(2) 0.0321(9) Uani 1 1 d . . . . .
C22 C 0.65597(15) 0.3367(3) 0.8474(2) 0.0303(9) Uani 1 1 d . . . . .
C48 C 0.40304(14) 0.4340(3) 0.9892(2) 0.0266(8) Uani 1 1 d . . . . .
C51 C 0.36993(14) 0.5755(3) 0.9470(2) 0.0281(8) Uani 1 1 d . . . . .
C5 C 0.46417(15) 0.7855(3) 0.8752(2) 0.0307(9) Uani 1 1 d . . . . .
H5 H 0.4897 0.7829 0.9082 0.037 Uiso 1 1 calc R . . . .
C35 C 0.44969(15) 0.2290(3) 0.7702(2) 0.0339(9) Uani 1 1 d . . . . .
C55 C 0.35165(14) 0.3600(3) 0.9176(2) 0.0296(9) Uani 1 1 d . . . . .
C50 C 0.40692(14) 0.5699(3) 0.99625(19) 0.0256(8) Uani 1 1 d . . . . .
C52 C 0.35902(14) 0.6591(3) 0.9358(2) 0.0279(8) Uani 1 1 d . . . . .
C34 C 0.49236(15) 0.2275(3) 0.8056(2) 0.0327(9) Uani 1 1 d . . . . .
H34 H 0.4983 0.2305 0.8519 0.039 Uiso 1 1 calc R . . . .
C27 C 0.63977(14) 0.1635(3) 0.8273(2) 0.0279(8) Uani 1 1 d . . . . .
H27 H 0.6399 0.1801 0.8731 0.033 Uiso 1 1 calc R . . . .
C42 C 0.37823(14) 0.2242(2) 0.95285(19) 0.0269(8) Uani 1 1 d . . . . .
H42 H 0.4041 0.2031 0.9837 0.032 Uiso 1 1 calc R . . . .
C49 C 0.42465(13) 0.4993(3) 1.01885(19) 0.0267(8) Uani 1 1 d . . . . .
H49 H 0.4499 0.4955 1.0523 0.032 Uiso 1 1 calc R . . . .
C11 C 0.66132(16) 0.7628(3) 0.7887(2) 0.0313(9) Uani 1 1 d . . . . .
H11 H 0.6574 0.7801 0.8325 0.038 Uiso 1 1 calc R . . . .
C75 C 0.40673(18) 0.3410(3) 0.4336(2) 0.0394(11) Uani 1 1 d . . . . .
C4 C 0.46716(16) 0.7737(3) 0.8068(2) 0.0330(9) Uani 1 1 d . . . . .
C21 C 0.65129(14) 0.4175(3) 0.8212(2) 0.0284(8) Uani 1 1 d . . . . .
C53 C 0.34841(15) 0.5104(3) 0.9162(2) 0.0308(9) Uani 1 1 d . . . . .
H53 H 0.3235 0.5142 0.8822 0.037 Uiso 1 1 calc R . . . .
C54 C 0.36643(14) 0.4400(3) 0.9394(2) 0.0282(9) Uani 1 1 d . . . . .
C39 C 0.46694(16) 0.2115(3) 0.5983(2) 0.0372(10) Uani 1 1 d . . . . .
H39 H 0.4903 0.2159 0.5770 0.045 Uiso 1 1 calc R . . . .
C56 C 0.42118(14) 0.6506(3) 1.0159(2) 0.0270(8) Uani 1 1 d . . . . .
C58 C 0.43163(15) 0.8187(3) 0.9605(2) 0.0287(9) Uani 1 1 d . . . . .
H58 H 0.4582 0.7963 0.9886 0.034 Uiso 1 1 calc R . . . .
C23 C 0.66046(14) 0.4158(3) 0.7592(2) 0.0282(8) Uani 1 1 d . . . . .
C36 C 0.41350(15) 0.2245(3) 0.8027(2) 0.0351(10) Uani 1 1 d . . . . .
H36 H 0.3853 0.2305 0.7770 0.042 Uiso 1 1 calc R . . . .
C40 C 0.51727(15) 0.2208(3) 0.7056(2) 0.0331(9) Uani 1 1 d . . . . .
H40 H 0.5404 0.2192 0.6837 0.040 Uiso 1 1 calc R . . . .
C59 C 0.43195(18) 0.9076(3) 0.9667(2) 0.0364(10) Uani 1 1 d . . . . .
H59A H 0.4589 0.9280 0.9569 0.044 Uiso 1 1 calc R . . . .
H59B H 0.4077 0.9292 0.9339 0.044 Uiso 1 1 calc R . . . .
C17 C 0.65539(15) 0.5505(3) 0.7538(2) 0.0306(9) Uani 1 1 d . . . . .
C62 C 0.38692(16) 0.8145(3) 1.0483(2) 0.0313(9) Uani 1 1 d . . . . .
H62A H 0.3594 0.7954 1.0572 0.038 Uiso 1 1 calc R . . . .
H62B H 0.4106 0.7930 1.0822 0.038 Uiso 1 1 calc R . . . .
C38 C 0.47511(15) 0.2222(3) 0.6695(2) 0.0344(10) Uani 1 1 d . . . . .
C41 C 0.37857(15) 0.1921(3) 0.8846(2) 0.0291(9) Uani 1 1 d . . . . .
H41 H 0.3531 0.2121 0.8524 0.035 Uiso 1 1 calc R . . . .
C19 C 0.64299(16) 0.6345(3) 0.8350(2) 0.0328(10) Uani 1 1 d . . . . .
C26 C 0.67491(15) 0.2065(3) 0.8022(2) 0.0298(9) Uani 1 1 d . . . . .
H26 H 0.6736 0.1881 0.7566 0.036 Uiso 1 1 calc R . . . .
C1 C 0.55458(17) 0.7766(3) 0.7104(2) 0.0358(10) Uani 1 1 d . . . . .
H1 H 0.5582 0.7647 0.6677 0.043 Uiso 1 1 calc R . . . .
C32 C 0.56982(15) 0.2078(3) 0.8119(2) 0.0297(9) Uani 1 1 d . . . . .
H32 H 0.5764 0.2193 0.8572 0.036 Uiso 1 1 calc R . . . .
C7 C 0.43402(16) 0.7628(3) 0.6918(2) 0.0345(10) Uani 1 1 d . . . . .
C18 C 0.64527(15) 0.5516(3) 0.8151(2) 0.0299(9) Uani 1 1 d . . . . .
C29 C 0.69310(18) 0.0549(3) 0.8634(2) 0.0392(11) Uani 1 1 d . . . . .
H29A H 0.6953 0.0661 0.9103 0.047 Uiso 1 1 calc R . . . .
H29B H 0.6979 -0.0014 0.8588 0.047 Uiso 1 1 calc R . . . .
C2 C 0.51166(16) 0.7710(3) 0.7263(2) 0.0328(9) Uani 1 1 d . . . . .
C28 C 0.64838(16) 0.0760(3) 0.8255(2) 0.0323(9) Uani 1 1 d . . . . .
H28A H 0.6268 0.0477 0.8443 0.039 Uiso 1 1 calc R . . . .
H28B H 0.6451 0.0591 0.7796 0.039 Uiso 1 1 calc R . . . .
C72 C 0.38757(17) 0.6408(3) 0.4461(2) 0.0396(11) Uani 1 1 d . . . . .
C10 C 0.62862(15) 0.8064(3) 0.7377(2) 0.0304(9) Uani 1 1 d . . . . .
H10 H 0.6281 0.7856 0.6930 0.036 Uiso 1 1 calc R . . . .
C77 C 0.34645(18) 0.3244(3) 0.4759(2) 0.0416(11) Uani 1 1 d . . . . .
N13 N 0.54378(18) 0.5114(4) 0.7271(3) 0.0593(13) Uani 1 1 d . . . . .
C109 C 0.74309(17) 0.4726(4) 0.9561(3) 0.0465(13) Uani 1 1 d . . . . .
C16 C 0.65989(15) 0.6316(3) 0.7330(2) 0.0298(9) Uani 1 1 d . . . . .
C79 C 0.38432(16) 0.2014(3) 0.4557(2) 0.0359(10) Uani 1 1 d . . . . .
H79 H 0.3613 0.1801 0.4764 0.043 Uiso 1 1 calc R . . . .
C8 C 0.39375(17) 0.7638(3) 0.6414(2) 0.0383(10) Uani 1 1 d . . . . .
H8 H 0.3675 0.7541 0.6546 0.046 Uiso 1 1 calc R . . . .
C14 C 0.68599(18) 0.9085(3) 0.7369(2) 0.0383(10) Uani 1 1 d . . . . .
H14A H 0.6904 0.8914 0.6937 0.046 Uiso 1 1 calc R . . . .
H14B H 0.6920 0.9649 0.7410 0.046 Uiso 1 1 calc R . . . .
C61 C 0.38799(19) 0.9031(3) 1.0518(2) 0.0393(11) Uani 1 1 d . . . . .
H61A H 0.3626 0.9244 1.0212 0.047 Uiso 1 1 calc R . . . .
H61B H 0.3866 0.9199 1.0965 0.047 Uiso 1 1 calc R . . . .
C37 C 0.44163(15) 0.2262(3) 0.7029(2) 0.0365(10) Uani 1 1 d . . . . .
H37 H 0.4128 0.2269 0.6788 0.044 Uiso 1 1 calc R . . . .
C3 C 0.50734(15) 0.7760(3) 0.7917(2) 0.0329(9) Uani 1 1 d . . . . .
H3 H 0.5322 0.7809 0.8257 0.040 Uiso 1 1 calc R . . . .
C20 C 0.64253(15) 0.4847(3) 0.8512(2) 0.0311(9) Uani 1 1 d . . . . .
H20 H 0.6353 0.4854 0.8928 0.037 Uiso 1 1 calc R . . . .
C30 C 0.72755(17) 0.0999(3) 0.8392(3) 0.0420(12) Uani 1 1 d . . . . .
H30A H 0.7276 0.0843 0.7938 0.050 Uiso 1 1 calc R . . . .
H30B H 0.7560 0.0874 0.8668 0.050 Uiso 1 1 calc R . . . .
C43 C 0.33854(16) 0.1946(3) 0.9753(2) 0.0333(9) Uani 1 1 d . . . . .
H43A H 0.3383 0.2156 1.0191 0.040 Uiso 1 1 calc R . . . .
H43B H 0.3123 0.2130 0.9447 0.040 Uiso 1 1 calc R . . . .
C44 C 0.33863(18) 0.1063(3) 0.9776(2) 0.0399(11) Uani 1 1 d . . . . .
H44A H 0.3643 0.0882 1.0096 0.048 Uiso 1 1 calc R . . . .
H44B H 0.3128 0.0880 0.9922 0.048 Uiso 1 1 calc R . . . .
C15 C 0.63935(17) 0.8936(3) 0.7410(2) 0.0350(10) Uani 1 1 d . . . . .
H15A H 0.6200 0.9208 0.7046 0.042 Uiso 1 1 calc R . . . .
H15B H 0.6343 0.9152 0.7825 0.042 Uiso 1 1 calc R . . . .
C45 C 0.33898(18) 0.0723(3) 0.9113(3) 0.0400(11) Uani 1 1 d . . . . .
H45A H 0.3120 0.0860 0.8802 0.048 Uiso 1 1 calc R . . . .
H45B H 0.3407 0.0149 0.9146 0.048 Uiso 1 1 calc R . . . .
C6 C 0.43060(15) 0.7664(3) 0.7570(2) 0.0332(9) Uani 1 1 d . . . . .
H6 H 0.4031 0.7638 0.7675 0.040 Uiso 1 1 calc R . . . .
C9 C 0.47478(17) 0.7641(3) 0.6769(2) 0.0368(10) Uani 1 1 d . . . . .
H9 H 0.4773 0.7603 0.6327 0.044 Uiso 1 1 calc R . . . .
C25 C 0.66277(16) 0.4824(3) 0.7232(2) 0.0310(9) Uani 1 1 d . . . . .
H25 H 0.6689 0.4813 0.6808 0.037 Uiso 1 1 calc R . . . .
C69 C 0.32711(18) 0.6205(4) 0.4875(2) 0.0442(12) Uani 1 1 d . . . . .
C110 C 0.74062(17) 0.4327(4) 1.0120(3) 0.0473(13) Uani 1 1 d . . . . .
H110 H 0.7302 0.4572 1.0461 0.057 Uiso 1 1 calc R . . . .
C13 C 0.71664(18) 0.8661(3) 0.7895(3) 0.0425(11) Uani 1 1 d . . . . .
H13A H 0.7137 0.8857 0.8328 0.051 Uiso 1 1 calc R . . . .
H13B H 0.7464 0.8760 0.7850 0.051 Uiso 1 1 calc R . . . .
C12 C 0.70787(16) 0.7793(3) 0.7856(2) 0.0375(10) Uani 1 1 d . . . . .
H12A H 0.7273 0.7527 0.8223 0.045 Uiso 1 1 calc R . . . .
H12B H 0.7136 0.7586 0.7443 0.045 Uiso 1 1 calc R . . . .
C70 C 0.34401(18) 0.5431(3) 0.4744(2) 0.0410(11) Uani 1 1 d . . . . .
C60 C 0.4283(2) 0.9348(3) 1.0347(3) 0.0415(11) Uani 1 1 d . . . . .
H60A H 0.4537 0.9169 1.0673 0.050 Uiso 1 1 calc R . . . .
H60B H 0.4278 0.9923 1.0358 0.050 Uiso 1 1 calc R . . . .
C31 C 0.71959(15) 0.1876(3) 0.8416(3) 0.0366(10) Uani 1 1 d . . . . .
H31A H 0.7221 0.2043 0.8875 0.044 Uiso 1 1 calc R . . . .
H31B H 0.7414 0.2160 0.8235 0.044 Uiso 1 1 calc R . . . .
C63 C 0.34888(18) 0.7880(4) 0.5423(2) 0.0437(12) Uani 1 1 d . . . . .
H63 H 0.3278 0.7581 0.5616 0.052 Uiso 1 1 calc R . . . .
C74 C 0.38935(17) 0.4197(3) 0.4431(2) 0.0391(11) Uani 1 1 d . . . . .
C76 C 0.35268(17) 0.4089(3) 0.4683(2) 0.0405(11) Uani 1 1 d . . . . .
C81 C 0.4306(2) 0.0856(4) 0.4940(3) 0.0547(15) Uani 1 1 d . . . . .
H81A H 0.4085 0.0620 0.5147 0.066 Uiso 1 1 calc R . . . .
H81B H 0.4591 0.0692 0.5191 0.066 Uiso 1 1 calc R . . . .
C114 C 0.75810(19) 0.4391(4) 0.9054(3) 0.0506(14) Uani 1 1 d . . . . .
H114 H 0.7590 0.4677 0.8670 0.061 Uiso 1 1 calc R . . . .
C46 C 0.37735(17) 0.1033(3) 0.8862(3) 0.0376(10) Uani 1 1 d . . . . .
H46A H 0.3760 0.0831 0.8417 0.045 Uiso 1 1 calc R . . . .
H46B H 0.4042 0.0839 0.9147 0.045 Uiso 1 1 calc R . . . .
C71 C 0.38084(17) 0.5550(3) 0.4486(2) 0.0371(10) Uani 1 1 d . . . . .
C80 C 0.42715(17) 0.1745(3) 0.4967(2) 0.0389(11) Uani 1 1 d . . . . .
H80 H 0.4512 0.1990 0.4802 0.047 Uiso 1 1 calc R . . . .
O13 O 0.5579(2) 0.4506(5) 0.7085(4) 0.0925(19) Uani 1 1 d . . . . .
C112 C 0.76989(19) 0.3211(4) 0.9681(3) 0.0520(14) Uani 1 1 d . . . . .
H112 H 0.7797 0.2689 0.9726 0.062 Uiso 1 1 calc R . . . .
N16 N 0.2640(2) 0.0261(5) 0.6997(3) 0.079(2) Uani 1 1 d . . . . .
O14 O 0.5511(2) 0.5753(4) 0.7094(4) 0.096(2) Uani 1 1 d . . . . .
C113 C 0.7717(2) 0.3626(4) 0.9121(3) 0.0546(15) Uani 1 1 d . . . . .
H113 H 0.7824 0.3384 0.8781 0.066 Uiso 1 1 calc R . . . .
C64 C 0.34732(19) 0.7596(3) 0.4721(2) 0.0411(11) Uani 1 1 d . . . . .
H64 H 0.3711 0.7857 0.4562 0.049 Uiso 1 1 calc R . . . .
C78 C 0.32896(18) 0.4698(4) 0.4849(3) 0.0460(12) Uani 1 1 d . . . . .
H78 H 0.3041 0.4620 0.5023 0.055 Uiso 1 1 calc R . . . .
C73 C 0.40458(18) 0.4933(3) 0.4324(2) 0.0416(11) Uani 1 1 d . . . . .
H73 H 0.4295 0.5008 0.4152 0.050 Uiso 1 1 calc R . . . .
C111 C 0.75382(19) 0.3555(4) 1.0173(3) 0.0511(14) Uani 1 1 d . . . . .
H111 H 0.7518 0.3263 1.0549 0.061 Uiso 1 1 calc R . . . .
O19 O 0.2526(3) -0.0239(5) 0.6575(4) 0.107(2) Uani 1 1 d . . . . .
C84 C 0.3759(2) 0.1704(3) 0.3855(2) 0.0442(12) Uani 1 1 d . . . . .
H84A H 0.3467 0.1858 0.3622 0.053 Uiso 1 1 calc R . . . .
H84B H 0.3968 0.1936 0.3622 0.053 Uiso 1 1 calc R . . . .
C66 C 0.2955(3) 0.8682(4) 0.4279(3) 0.0619(18) Uani 1 1 d . . . . .
H66A H 0.2675 0.8798 0.3985 0.074 Uiso 1 1 calc R . . . .
H66B H 0.3180 0.8978 0.4124 0.074 Uiso 1 1 calc R . . . .
C83 C 0.3798(2) 0.0821(4) 0.3851(3) 0.0524(14) Uani 1 1 d . . . . .
H83A H 0.3754 0.0634 0.3395 0.063 Uiso 1 1 calc R . . . .
H83B H 0.3573 0.0588 0.4050 0.063 Uiso 1 1 calc R . . . .
O20 O 0.2617(2) 0.0153(6) 0.7561(3) 0.115(3) Uani 1 1 d . . . . .
C65 C 0.3048(2) 0.7819(4) 0.4257(2) 0.0521(15) Uani 1 1 d . . . . .
H65A H 0.3061 0.7672 0.3805 0.062 Uiso 1 1 calc R . . . .
H65B H 0.2810 0.7524 0.4378 0.062 Uiso 1 1 calc R . . . .
C67 C 0.2944(3) 0.8937(5) 0.4976(3) 0.066(2) Uani 1 1 d . . . . .
H67A H 0.2713 0.8658 0.5129 0.080 Uiso 1 1 calc R . . . .
H67B H 0.2886 0.9501 0.4985 0.080 Uiso 1 1 calc R . . . .
C104 C 0.2846(2) 0.1606(6) 0.7243(3) 0.067(2) Uani 1 1 d . . . . .
H104 H 0.2784 0.1542 0.7663 0.080 Uiso 1 1 calc R . . . .
C82 C 0.4244(3) 0.0560(4) 0.4235(3) 0.0603(17) Uani 1 1 d . . . . .
H82A H 0.4265 -0.0014 0.4232 0.072 Uiso 1 1 calc R . . . .
H82B H 0.4471 0.0775 0.4029 0.072 Uiso 1 1 calc R . . . .
C68 C 0.3386(2) 0.8749(4) 0.5428(3) 0.0608(17) Uani 1 1 d . . . . .
H68A H 0.3613 0.9046 0.5280 0.073 Uiso 1 1 calc R . . . .
H68B H 0.3383 0.8913 0.5879 0.073 Uiso 1 1 calc R . . . .
C103 C 0.2796(2) 0.0994(5) 0.6810(3) 0.0606(18) Uani 1 1 d . . . . .
C85 C 0.5151(2) 0.5030(4) 0.7739(3) 0.0576(15) Uani 1 1 d . . . . .
C105 C 0.2984(2) 0.2296(6) 0.7064(5) 0.081(2) Uani 1 1 d . . . . .
H105 H 0.3012 0.2731 0.7350 0.097 Uiso 1 1 calc R . . . .
C122 C 0.2526(4) 0.7134(6) 0.6211(5) 0.043(2) Uiso 0.5 1 d D U . . .
H122 H 0.2336 0.7105 0.5795 0.051 Uiso 0.5 1 calc R . . . .
C86 C 0.5013(3) 0.5688(4) 0.7968(5) 0.075(2) Uani 1 1 d . . . . .
H86 H 0.5109 0.6181 0.7853 0.091 Uiso 1 1 calc R . . . .
C106 C 0.3088(3) 0.2360(7) 0.6433(6) 0.094(3) Uani 1 1 d . . . . .
H106 H 0.3200 0.2832 0.6306 0.113 Uiso 1 1 calc R . . . .
C88 C 0.4618(3) 0.4912(5) 0.8583(4) 0.075(2) Uani 1 1 d . . . . .
H88 H 0.4417 0.4863 0.8856 0.090 Uiso 1 1 calc R . . . .
C108 C 0.2886(3) 0.1051(7) 0.6192(4) 0.083(3) Uani 1 1 d . . . . .
H108 H 0.2853 0.0617 0.5905 0.099 Uiso 1 1 calc R . . . .
C90 C 0.5057(3) 0.4319(4) 0.7955(5) 0.077(2) Uani 1 1 d . . . . .
H90 H 0.5170 0.3862 0.7800 0.092 Uiso 1 1 calc R . . . .
C124 C 0.2888(4) 0.7933(7) 0.7098(5) 0.048(2) Uiso 0.5 1 d D U . . .
H124 H 0.2962 0.8424 0.7298 0.057 Uiso 0.5 1 calc R . . . .
C121 C 0.2683(4) 0.6457(7) 0.6505(6) 0.054(3) Uiso 0.5 1 d D U . . .
C123 C 0.2626(3) 0.7862(6) 0.6483(4) 0.040(2) Uiso 0.5 1 d D U . . .
H123 H 0.2514 0.8314 0.6246 0.047 Uiso 0.5 1 calc R . . . .
N19 N 0.2572(5) 0.5757(9) 0.6177(12) 0.099(6) Uani 0.5 1 d . . . . .
C125 C 0.3038(4) 0.7229(7) 0.7407(6) 0.059(3) Uiso 0.5 1 d D U . . .
H125 H 0.3214 0.7256 0.7834 0.070 Uiso 0.5 1 calc R . . . .
C89 C 0.4799(4) 0.4265(5) 0.8396(4) 0.083(2) Uani 1 1 d . . . . .
H89 H 0.4747 0.3774 0.8571 0.099 Uiso 1 1 calc R . . . .
C126 C 0.2946(5) 0.6505(9) 0.7136(7) 0.071(4) Uiso 0.5 1 d D U . . .
H126 H 0.3057 0.6049 0.7367 0.085 Uiso 0.5 1 calc R . . . .
C107 C 0.3024(4) 0.1742(7) 0.6013(5) 0.090(3) Uani 1 1 d . . . . .
H107 H 0.3079 0.1801 0.5588 0.108 Uiso 1 1 calc R . . . .
O22 O 0.2259(7) 0.5733(8) 0.5757(12) 0.133(8) Uani 0.5 1 d . . . . .
C87 C 0.4715(4) 0.5628(6) 0.8392(5) 0.099(3) Uani 1 1 d . . . . .
H87 H 0.4590 0.6079 0.8534 0.118 Uiso 1 1 calc R . . . .
O21 O 0.2789(6) 0.5177(9) 0.6250(11) 0.124(6) Uani 0.5 1 d . . . . .
C93 C 0.4295(5) 0.5648(8) 0.6232(7) 0.083(2) Uani 0.5 1 d D . . . .
H93 H 0.4326 0.6160 0.6080 0.100 Uiso 0.5 1 calc R . . . .
C95 C 0.4415(6) 0.4290(7) 0.6150(7) 0.083(2) Uani 0.5 1 d D . . . .
H95 H 0.4531 0.3873 0.5946 0.100 Uiso 0.5 1 calc R . . . .
C92 C 0.4062(5) 0.5519(7) 0.6659(7) 0.083(2) Uani 0.5 1 d D . . . .
H92 H 0.3936 0.5940 0.6844 0.100 Uiso 0.5 1 calc R . . . .
C91 C 0.4000(6) 0.4771(7) 0.6841(7) 0.083(2) Uani 0.5 1 d D . . . .
O16 O 0.3660(6) 0.5138(11) 0.7633(9) 0.116(4) Uani 0.5 1 d . . . . .
C94 C 0.4495(6) 0.5040(7) 0.6003(7) 0.083(2) Uani 0.5 1 d D . . . .
H94 H 0.4695 0.5142 0.5736 0.100 Uiso 0.5 1 calc R . . . .
N14 N 0.3746(7) 0.4618(14) 0.7335(12) 0.116(4) Uani 0.5 1 d . . . . .
C96 C 0.4173(6) 0.4150(8) 0.6583(7) 0.083(2) Uani 0.5 1 d D . . . .
H96 H 0.4123 0.3634 0.6709 0.100 Uiso 0.5 1 calc R . . . .
O15 O 0.3684(5) 0.3913(10) 0.7439(9) 0.116(4) Uani 0.5 1 d . . . . .
O28 O 0.5000 0.1336(7) 1.0000 0.063(3) Uani 0.6 2 d S T P . .
H28 H 0.5124 0.1754 1.0003 0.095 Uiso 0.6 1 d R . . . .
C129 C 0.4882(3) 0.1103(6) 0.9408(4) 0.049(2) Uani 0.6 1 d . . . . .
H12C H 0.4900 0.1522 0.9113 0.074 Uiso 0.3 1 d R . . . .
H12D H 0.5067 0.0687 0.9335 0.074 Uiso 0.3 1 d R . . . .
H12E H 0.4591 0.0920 0.9335 0.074 Uiso 0.3 1 d R . . . .
C117 C 0.5063(7) 1.0162(18) 0.7931(13) 0.079(6) Uani 0.5 1 d D . . A 1
H117 H 0.5268 1.0298 0.8314 0.094 Uiso 0.5 1 calc R . . A 1
C116 C 0.4641(5) 0.9975(8) 0.7961(6) 0.057(3) Uani 0.5 1 d D . . A 1
H116 H 0.4549 0.9992 0.8363 0.069 Uiso 0.5 1 calc R . . A 1
C118 C 0.5176(6) 1.0143(10) 0.7325(8) 0.075(5) Uani 0.5 1 d D . . A 1
H118 H 0.5455 1.0310 0.7292 0.090 Uiso 0.5 1 calc R . . A 1
N15 N 0.4006(5) 0.0420(10) 0.6826(7) 0.089(2) Uani 0.5 1 d . . . B 2
C115 C 0.4364(4) 0.9768(5) 0.7395(5) 0.047(3) Uani 0.5 1 d D . . A 1
O17 O 0.3828(4) 0.0818(9) 0.7183(6) 0.089(2) Uani 0.5 1 d . . . B 2
O18 O 0.3829(4) 0.0254(9) 0.6267(6) 0.089(2) Uani 0.5 1 d . . . B 2
C120 C 0.4464(5) 0.9711(8) 0.6790(6) 0.062(3) Uani 0.5 1 d D . . A 1
H120 H 0.4258 0.9563 0.6411 0.074 Uiso 0.5 1 calc R . . A 1
C119 C 0.4893(6) 0.9887(14) 0.6769(8) 0.085(6) Uani 0.5 1 d D . . A 1
H119 H 0.4988 0.9831 0.6372 0.102 Uiso 0.5 1 calc R . . A 1
O24 O 0.3842(5) 0.9529(9) 0.7970(8) 0.085(4) Uani 0.5 1 d . . . A 1
N18 N 0.3906(4) 0.9598(6) 0.7426(5) 0.055(3) Uani 0.5 1 d . . . A 1
O23 O 0.3656(5) 0.9509(12) 0.6948(6) 0.112(6) Uani 0.5 1 d . . . A 1
C97 C 0.4452(5) 0.0199(8) 0.7088(7) 0.0735(19) Uani 0.5 1 d D . . B 2
C98 C 0.4677(7) -0.0165(12) 0.6691(11) 0.0735(19) Uani 0.5 1 d D . . B 2
H98 H 0.4546 -0.0287 0.6251 0.088 Uiso 0.5 1 calc R . . B 2
C102 C 0.4635(5) 0.0364(11) 0.7728(9) 0.0735(19) Uani 0.5 1 d D . . B 2
H102 H 0.4469 0.0595 0.8004 0.088 Uiso 0.5 1 calc R . . B 2
C99 C 0.5095(6) -0.0350(11) 0.6939(9) 0.0735(19) Uani 0.5 1 d D . . B 2
H99 H 0.5259 -0.0604 0.6673 0.088 Uiso 0.5 1 calc R . . B 2
C101 C 0.5057(8) 0.019(2) 0.7961(16) 0.0735(19) Uani 0.5 1 d D . . B 2
H101 H 0.5194 0.0325 0.8396 0.088 Uiso 0.5 1 calc R . . B 2
C100 C 0.5276(6) -0.0170(12) 0.7565(9) 0.0735(19) Uani 0.5 1 d D . . B 2
H100 H 0.5568 -0.0304 0.7732 0.088 Uiso 0.5 1 calc R . . B 2
O27 O 0.3508(3) 0.8611(7) 0.8218(5) 0.069(3) Uani 0.5 1 d . . . C 2
H27A H 0.3723 0.8355 0.8409 0.104 Uiso 0.5 1 calc GR . . C 2
C127 C 0.3645(7) 0.9231(10) 0.7841(8) 0.064(4) Uani 0.5 1 d . . . C 2
H12F H 0.3668 0.9031 0.7412 0.097 Uiso 0.5 1 calc GR . . C 2
H12G H 0.3926 0.9426 0.8071 0.097 Uiso 0.5 1 calc GR . . C 2
H12H H 0.3435 0.9654 0.7784 0.097 Uiso 0.5 1 calc GR . . C 2
O29 O 0.4547(6) 0.8772(11) 0.5303(8) 0.091(4) Uani 0.4 1 d . . . . .
H29 H 0.4304 0.8593 0.5184 0.137 Uiso 0.4 1 d R . . . .
C128 C 0.4840(8) 0.8372(16) 0.4971(13) 0.091(4) Uani 0.4 1 d . . . . .
H12I H 0.4743 0.8408 0.4505 0.137 Uiso 0.4 1 d R . . . .
H12J H 0.5118 0.8608 0.5099 0.137 Uiso 0.4 1 d R . . . .
H12K H 0.4857 0.7836 0.5099 0.137 Uiso 0.4 1 d R . . . .


_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
O5 C47 1.198(6) . ?
O4 C22 1.212(6) . ?
O7 C56 1.218(6) . ?
O3 C24 1.210(6) . ?
O8 C52 1.206(6) . ?
O6 C55 1.201(6) . ?
O2 C16 1.207(6) . ?
O1 C19 1.197(6) . ?
N9 C47 1.399(6) . ?
N9 C55 1.396(6) . ?
N9 C42 1.472(5) . ?
O10 C72 1.191(7) . ?
N2 C5 1.259(6) . ?
N2 C58 1.465(5) . ?
O12 C75 1.223(7) . ?
N5 C24 1.393(6) . ?
N5 C22 1.392(6) . ?
N5 C26 1.473(6) . ?
N6 C27 1.440(6) . ?
N6 C32 1.259(6) . ?
N7 C36 1.270(6) . ?
N7 C41 1.461(6) . ?
O11 C77 1.198(7) . ?
N11 C75 1.394(7) . ?
N11 C77 1.397(7) . ?
N11 C79 1.483(7) . ?
N10 C57 1.481(5) . ?
N10 C52 1.395(6) . ?
N10 C56 1.395(6) . ?
N1 C1 1.267(7) . ?
N1 C10 1.462(6) . ?
N4 C11 1.471(6) . ?
N4 C19 1.399(6) . ?
N4 C16 1.400(6) . ?
N8 C39 1.275(7) . ?
N8 C80 1.449(6) . ?
O26 N17 1.231(7) . ?
O9 C69 1.215(7) . ?
N17 O25 1.229(7) . ?
N17 C109 1.480(8) . ?
N3 C8 1.252(7) . ?
N3 C63 1.470(7) . ?
C47 C48 1.507(6) . ?
N12 C72 1.404(7) . ?
N12 C69 1.378(8) . ?
N12 C64 1.472(7) . ?
C57 C58 1.539(6) . ?
C57 C62 1.529(6) . ?
C24 C23 1.482(6) . ?
C33 C34 1.374(7) . ?
C33 C40 1.396(6) . ?
C33 C32 1.483(6) . ?
C22 C21 1.491(6) . ?
C48 C49 1.392(6) . ?
C48 C54 1.394(6) . ?
C51 C50 1.394(6) . ?
C51 C52 1.488(6) . ?
C51 C53 1.397(7) . ?
C5 C4 1.471(6) . ?
C35 C34 1.403(7) . ?
C35 C36 1.463(6) . ?
C35 C37 1.380(6) . ?
C55 C54 1.494(6) . ?
C50 C49 1.380(6) . ?
C50 C56 1.493(6) . ?
C27 C26 1.527(6) . ?
C27 C28 1.534(6) . ?
C42 C41 1.536(5) . ?
C42 C43 1.529(6) . ?
C11 C10 1.522(6) . ?
C11 C12 1.526(7) . ?
C75 C74 1.494(8) . ?
C4 C3 1.385(7) . ?
C4 C6 1.394(7) . ?
C21 C23 1.392(6) . ?
C21 C20 1.373(7) . ?
C53 C54 1.384(6) . ?
C39 C38 1.470(6) . ?
C58 C59 1.535(6) . ?
C23 C25 1.383(6) . ?
C40 C38 1.394(7) . ?
C59 C60 1.530(7) . ?
C17 C18 1.392(6) . ?
C17 C16 1.478(6) . ?
C17 C25 1.382(7) . ?
C62 C61 1.528(6) . ?
C38 C37 1.399(7) . ?
C41 C46 1.530(6) . ?
C19 C18 1.493(6) . ?
C26 C31 1.521(6) . ?
C1 C2 1.479(7) . ?
C7 C8 1.478(7) . ?
C7 C6 1.396(6) . ?
C7 C9 1.400(7) . ?
C18 C20 1.391(7) . ?
C29 C28 1.520(7) . ?
C29 C30 1.517(8) . ?
C2 C3 1.411(6) . ?
C2 C9 1.394(7) . ?
C72 C71 1.495(8) . ?
C10 C15 1.538(6) . ?
C77 C76 1.483(8) . ?
N13 O13 1.235(9) . ?
N13 O14 1.201(9) . ?
N13 C85 1.484(9) . ?
C109 C110 1.377(9) . ?
C109 C114 1.382(8) . ?
C79 C80 1.521(7) . ?
C79 C84 1.534(7) . ?
C14 C15 1.530(7) . ?
C14 C13 1.497(8) . ?
C61 C60 1.510(8) . ?
C30 C31 1.534(7) . ?
C43 C44 1.521(7) . ?
C44 C45 1.510(7) . ?
C45 C46 1.529(7) . ?
C69 C70 1.485(8) . ?
C110 C111 1.392(10) . ?
C13 C12 1.520(7) . ?
C70 C71 1.409(7) . ?
C70 C78 1.384(9) . ?
C63 C64 1.542(6) . ?
C63 C68 1.531(9) . ?
C74 C76 1.395(7) . ?
C74 C73 1.391(8) . ?
C76 C78 1.380(8) . ?
C81 C80 1.536(8) . ?
C81 C82 1.536(8) . ?
C114 C113 1.384(10) . ?
C71 C73 1.388(8) . ?
C112 C113 1.386(10) . ?
C112 C111 1.380(9) . ?
N16 O19 1.233(11) . ?
N16 O20 1.215(9) . ?
N16 C103 1.440(12) . ?
C64 C65 1.538(7) . ?
C84 C83 1.526(8) . ?
C66 C65 1.517(9) . ?
C66 C67 1.533(8) . ?
C83 C82 1.543(9) . ?
C67 C68 1.553(10) . ?
C104 C103 1.377(12) . ?
C104 C105 1.348(14) . ?
C103 C108 1.391(10) . ?
C85 C86 1.341(11) . ?
C85 C90 1.363(11) . ?
C105 C106 1.437(15) . ?
C122 C121 1.362(13) . ?
C122 C123 1.386(12) . ?
C86 C87 1.437(13) . ?
C106 C107 1.366(17) . ?
C88 C89 1.351(13) . ?
C88 C87 1.352(14) . ?
C108 C107 1.350(15) . ?
C90 C89 1.366(12) . ?
C124 C123 1.384(13) . ?
C124 C125 1.409(14) . ?
C121 N19 1.39(2) . ?
C121 C126 1.409(15) . ?
N19 O22 1.18(3) . ?
N19 O21 1.21(2) . ?
C125 C126 1.376(15) . ?
C93 C92 1.300(17) . ?
C93 C94 1.365(15) . ?
C95 C94 1.364(16) . ?
C95 C96 1.335(18) . ?
C92 C91 1.370(16) . ?
C91 N14 1.47(3) . ?
C91 C96 1.366(15) . ?
O16 N14 1.16(3) . ?
N14 O15 1.26(3) . ?
O28 C129 1.281(10) 2_657 ?
O28 C129 1.281(10) . ?
C117 C116 1.400(19) . ?
C117 C118 1.39(2) . ?
C116 C115 1.367(14) . ?
C118 C119 1.384(17) . ?
N15 O17 1.24(2) . ?
N15 O18 1.220(19) . ?
N15 C97 1.46(2) . ?
C115 C120 1.377(14) . ?
C115 N18 1.504(18) . ?
C120 C119 1.409(16) . ?
O24 N18 1.206(17) . ?
N18 O23 1.150(16) . ?
C97 C98 1.363(17) . ?
C97 C102 1.374(17) . ?
C98 C99 1.360(18) . ?
C102 C101 1.36(2) . ?
C99 C100 1.352(18) . ?
C101 C100 1.35(2) . ?
O27 C127 1.45(2) . ?
O29 C128 1.45(3) . ?
C128 C128 1.00(5) 2_656 ?

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
C47 N9 C42 122.5(4) . . ?
C55 N9 C47 112.5(4) . . ?
C55 N9 C42 124.7(4) . . ?
C5 N2 C58 117.0(4) . . ?
C24 N5 C26 122.0(4) . . ?
C22 N5 C24 111.7(4) . . ?
C22 N5 C26 126.4(4) . . ?
C32 N6 C27 117.8(4) . . ?
C36 N7 C41 115.2(4) . . ?
C75 N11 C77 111.0(4) . . ?
C75 N11 C79 127.1(4) . . ?
C77 N11 C79 121.8(4) . . ?
C52 N10 C57 122.1(4) . . ?
C56 N10 C57 126.0(4) . . ?
C56 N10 C52 111.9(4) . . ?
C1 N1 C10 119.8(4) . . ?
C19 N4 C11 123.6(4) . . ?
C19 N4 C16 111.7(4) . . ?
C16 N4 C11 124.2(4) . . ?
C39 N8 C80 116.9(4) . . ?
O26 N17 C109 118.1(5) . . ?
O25 N17 O26 124.5(6) . . ?
O25 N17 C109 117.5(5) . . ?
C8 N3 C63 114.6(5) . . ?
O5 C47 N9 125.9(4) . . ?
O5 C47 C48 128.4(4) . . ?
N9 C47 C48 105.7(4) . . ?
C72 N12 C64 123.7(5) . . ?
C69 N12 C72 111.9(5) . . ?
C69 N12 C64 124.2(5) . . ?
N10 C57 C58 110.5(4) . . ?
N10 C57 C62 111.0(3) . . ?
C62 C57 C58 113.1(4) . . ?
O3 C24 N5 125.7(4) . . ?
O3 C24 C23 128.0(4) . . ?
N5 C24 C23 106.3(4) . . ?
C34 C33 C40 120.0(4) . . ?
C34 C33 C32 119.5(4) . . ?
C40 C33 C32 120.1(4) . . ?
O4 C22 N5 127.0(4) . . ?
O4 C22 C21 126.7(4) . . ?
N5 C22 C21 106.3(4) . . ?
C49 C48 C47 130.5(4) . . ?
C49 C48 C54 122.0(4) . . ?
C54 C48 C47 107.5(4) . . ?
C50 C51 C52 108.4(4) . . ?
C50 C51 C53 122.7(4) . . ?
C53 C51 C52 128.9(4) . . ?
N2 C5 C4 122.9(4) . . ?
C34 C35 C36 121.7(4) . . ?
C37 C35 C34 119.1(4) . . ?
C37 C35 C36 118.8(4) . . ?
O6 C55 N9 126.3(4) . . ?
O6 C55 C54 128.1(4) . . ?
N9 C55 C54 105.6(4) . . ?
C51 C50 C56 107.4(4) . . ?
C49 C50 C51 122.3(4) . . ?
C49 C50 C56 130.3(4) . . ?
O8 C52 N10 125.8(4) . . ?
O8 C52 C51 128.3(4) . . ?
N10 C52 C51 105.9(4) . . ?
C33 C34 C35 120.5(4) . . ?
N6 C27 C26 109.0(4) . . ?
N6 C27 C28 109.7(4) . . ?
C26 C27 C28 108.6(4) . . ?
N9 C42 C41 112.1(3) . . ?
N9 C42 C43 112.0(4) . . ?
C43 C42 C41 109.8(4) . . ?
C50 C49 C48 115.5(4) . . ?
N4 C11 C10 110.8(4) . . ?
N4 C11 C12 110.1(4) . . ?
C10 C11 C12 113.9(4) . . ?
O12 C75 N11 125.2(5) . . ?
O12 C75 C74 127.9(5) . . ?
N11 C75 C74 106.9(4) . . ?
C3 C4 C5 118.5(4) . . ?
C3 C4 C6 119.8(4) . . ?
C6 C4 C5 121.6(4) . . ?
C23 C21 C22 107.5(4) . . ?
C20 C21 C22 129.1(4) . . ?
C20 C21 C23 123.3(4) . . ?
C54 C53 C51 114.5(4) . . ?
C48 C54 C55 108.7(4) . . ?
C53 C54 C48 123.0(4) . . ?
C53 C54 C55 128.3(4) . . ?
N8 C39 C38 122.5(4) . . ?
O7 C56 N10 126.0(4) . . ?
O7 C56 C50 127.6(4) . . ?
N10 C56 C50 106.4(4) . . ?
N2 C58 C57 108.6(4) . . ?
N2 C58 C59 108.3(3) . . ?
C59 C58 C57 109.3(4) . . ?
C21 C23 C24 108.2(4) . . ?
C25 C23 C24 129.0(4) . . ?
C25 C23 C21 122.6(4) . . ?
N7 C36 C35 123.3(4) . . ?
C38 C40 C33 120.4(4) . . ?
C60 C59 C58 112.5(4) . . ?
C18 C17 C16 108.4(4) . . ?
C25 C17 C18 122.5(4) . . ?
C25 C17 C16 128.9(4) . . ?
C61 C62 C57 111.0(4) . . ?
C40 C38 C39 119.3(4) . . ?
C40 C38 C37 118.7(4) . . ?
C37 C38 C39 121.8(4) . . ?
N7 C41 C42 111.7(4) . . ?
N7 C41 C46 106.4(4) . . ?
C46 C41 C42 109.5(4) . . ?
O1 C19 N4 125.8(4) . . ?
O1 C19 C18 128.3(4) . . ?
N4 C19 C18 105.9(4) . . ?
N5 C26 C27 111.1(4) . . ?
N5 C26 C31 111.7(4) . . ?
C31 C26 C27 112.4(4) . . ?
N1 C1 C2 119.8(4) . . ?
N6 C32 C33 121.6(4) . . ?
C6 C7 C8 117.5(4) . . ?
C6 C7 C9 119.2(4) . . ?
C9 C7 C8 123.1(4) . . ?
C17 C18 C19 107.8(4) . . ?
C20 C18 C17 123.1(4) . . ?
C20 C18 C19 128.8(4) . . ?
C30 C29 C28 111.7(4) . . ?
C3 C2 C1 120.2(4) . . ?
C9 C2 C1 120.8(4) . . ?
C9 C2 C3 118.9(4) . . ?
C29 C28 C27 112.0(4) . . ?
O10 C72 N12 125.3(5) . . ?
O10 C72 C71 128.6(5) . . ?
N12 C72 C71 106.2(5) . . ?
N1 C10 C11 107.9(4) . . ?
N1 C10 C15 107.4(4) . . ?
C11 C10 C15 109.7(4) . . ?
O11 C77 N11 125.8(5) . . ?
O11 C77 C76 127.6(5) . . ?
N11 C77 C76 106.6(5) . . ?
O13 N13 C85 116.4(6) . . ?
O14 N13 O13 124.8(7) . . ?
O14 N13 C85 118.8(7) . . ?
C110 C109 N17 118.6(5) . . ?
C110 C109 C114 122.7(6) . . ?
C114 C109 N17 118.7(6) . . ?
O2 C16 N4 126.1(4) . . ?
O2 C16 C17 127.6(4) . . ?
N4 C16 C17 106.2(4) . . ?
N11 C79 C80 111.8(4) . . ?
N11 C79 C84 110.3(4) . . ?
C80 C79 C84 112.8(4) . . ?
N3 C8 C7 123.5(5) . . ?
C13 C14 C15 111.4(4) . . ?
C60 C61 C62 111.2(4) . . ?
C35 C37 C38 121.3(4) . . ?
C4 C3 C2 120.7(4) . . ?
C21 C20 C18 113.9(4) . . ?
C29 C30 C31 110.8(4) . . ?
C44 C43 C42 110.3(4) . . ?
C45 C44 C43 111.0(4) . . ?
C14 C15 C10 111.8(4) . . ?
C44 C45 C46 110.2(4) . . ?
C4 C6 C7 120.6(4) . . ?
C2 C9 C7 120.8(4) . . ?
C17 C25 C23 114.5(4) . . ?
O9 C69 N12 126.5(6) . . ?
O9 C69 C70 126.6(6) . . ?
N12 C69 C70 106.9(5) . . ?
C109 C110 C111 118.2(5) . . ?
C14 C13 C12 110.9(4) . . ?
C13 C12 C11 110.5(4) . . ?
C71 C70 C69 107.8(5) . . ?
C78 C70 C69 129.5(5) . . ?
C78 C70 C71 122.7(5) . . ?
C61 C60 C59 110.5(4) . . ?
C26 C31 C30 109.5(4) . . ?
N3 C63 C64 109.5(4) . . ?
N3 C63 C68 107.7(5) . . ?
C68 C63 C64 110.6(5) . . ?
C76 C74 C75 107.1(5) . . ?
C73 C74 C75 130.7(5) . . ?
C73 C74 C76 122.2(5) . . ?
C74 C76 C77 108.3(5) . . ?
C78 C76 C77 128.7(5) . . ?
C78 C76 C74 122.9(6) . . ?
C80 C81 C82 111.8(5) . . ?
C109 C114 C113 118.1(6) . . ?
C45 C46 C41 112.5(4) . . ?
C70 C71 C72 107.2(5) . . ?
C73 C71 C72 131.1(5) . . ?
C73 C71 C70 121.7(5) . . ?
N8 C80 C79 109.1(4) . . ?
N8 C80 C81 107.9(4) . . ?
C79 C80 C81 110.2(5) . . ?
C111 C112 C113 120.2(6) . . ?
O19 N16 C103 118.8(7) . . ?
O20 N16 O19 121.4(10) . . ?
O20 N16 C103 119.7(9) . . ?
C114 C113 C112 120.5(6) . . ?
N12 C64 C63 111.2(4) . . ?
N12 C64 C65 110.4(5) . . ?
C65 C64 C63 111.6(4) . . ?
C76 C78 C70 115.1(5) . . ?
C71 C73 C74 115.4(5) . . ?
C112 C111 C110 120.3(6) . . ?
C83 C84 C79 110.7(4) . . ?
C65 C66 C67 110.8(5) . . ?
C84 C83 C82 110.8(5) . . ?
C66 C65 C64 112.1(5) . . ?
C66 C67 C68 108.5(6) . . ?
C105 C104 C103 119.4(7) . . ?
C81 C82 C83 108.5(5) . . ?
C63 C68 C67 111.6(6) . . ?
C104 C103 N16 119.2(6) . . ?
C104 C103 C108 122.8(8) . . ?
C108 C103 N16 117.9(8) . . ?
C86 C85 N13 116.8(7) . . ?
C86 C85 C90 121.8(7) . . ?
C90 C85 N13 121.2(7) . . ?
C104 C105 C106 118.5(10) . . ?
C121 C122 C123 124.0(10) . . ?
C85 C86 C87 118.2(8) . . ?
C107 C106 C105 120.2(9) . . ?
C89 C88 C87 121.8(8) . . ?
C107 C108 C103 117.8(10) . . ?
C85 C90 C89 119.6(8) . . ?
C123 C124 C125 115.5(11) . . ?
C122 C121 N19 119.2(12) . . ?
C122 C121 C126 117.5(12) . . ?
N19 C121 C126 123.4(13) . . ?
C124 C123 C122 120.2(10) . . ?
O22 N19 C121 118.8(15) . . ?
O22 N19 O21 116(2) . . ?
O21 N19 C121 125(2) . . ?
C126 C125 C124 124.6(12) . . ?
C88 C89 C90 119.8(8) . . ?
C125 C126 C121 118.2(14) . . ?
C108 C107 C106 121.3(9) . . ?
C88 C87 C86 118.3(9) . . ?
C92 C93 C94 119.4(16) . . ?
C96 C95 C94 119.3(15) . . ?
C93 C92 C91 119.3(15) . . ?
C92 C91 N14 119.9(16) . . ?
C96 C91 C92 122.1(17) . . ?
C96 C91 N14 118.0(17) . . ?
C95 C94 C93 121.5(18) . . ?
O16 N14 C91 118.1(19) . . ?
O16 N14 O15 126(3) . . ?
O15 N14 C91 115(2) . . ?
C95 C96 C91 117.9(16) . . ?
C129 O28 C129 143.5(14) 2_657 . ?
C118 C117 C116 118(2) . . ?
C115 C116 C117 117.9(16) . . ?
C119 C118 C117 122(2) . . ?
O17 N15 C97 116.9(14) . . ?
O18 N15 O17 122.2(16) . . ?
O18 N15 C97 120.7(15) . . ?
C116 C115 C120 125.8(13) . . ?
C116 C115 N18 117.6(11) . . ?
C120 C115 N18 116.5(10) . . ?
C115 C120 C119 115.5(13) . . ?
C118 C119 C120 120.3(17) . . ?
O24 N18 C115 115.1(12) . . ?
O23 N18 C115 119.0(12) . . ?
O23 N18 O24 125.7(15) . . ?
C98 C97 N15 119.3(15) . . ?
C98 C97 C102 121.6(17) . . ?
C102 C97 N15 119.1(14) . . ?
C99 C98 C97 118.3(19) . . ?
C101 C102 C97 119(2) . . ?
C100 C99 C98 119.8(18) . . ?
C100 C101 C102 119(3) . . ?
C101 C100 C99 122(2) . . ?
C128 C128 O29 133(3) 2_656 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O27 H27A N2 0.84 2.00 2.825(11) 166.8 .
C128 H12J O29 0.96 1.52 2.26(3) 129.7 2_656

_olex2_date_sample_data_collection 2019-08-12
_olex2_date_sample_submission    2019-07-08
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a mylar loop in perfluoroether oil'
_olex2_submission_original_sample_id HH_PlcyCage99_130K
_olex2_submission_special_instructions 'No special instructions were received'
