# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_res42_lavaggi_6
_database_code_depnum_ccdc_archive 'CCDC 2117238'
loop_
_audit_author_name
_audit_author_address
'Giovanni Pierri'
;University of Salerno
Italy
;
_audit_update_record             
;
2022-03-16 deposited with the CCDC.	2022-03-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_res42_lavaggi_6     
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: This is due to the  weak diffracting power of the sample
;
_vrf_PLAT242_res42_lavaggi_6     
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         O8 Check
RESPONSE: The atom belongs to a side chain
;
_vrf_PLAT340_res42_lavaggi_6     
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01107 Ang.
RESPONSE: This is due to the  weak diffracting power of the sample
;
# Added during the CSD deposition process: Wednesday 16 March 2022 11:39 AM
# end Validation Reply Form

_audit_creation_date             2021-11-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H92 N12 O20'
_chemical_formula_sum            'C60 H92 N12 O20'
_chemical_formula_weight         1301.45
_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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.9939(4)
_cell_length_b                   23.5910(9)
_cell_length_c                   14.8973(6)
_cell_angle_alpha                90
_cell_angle_beta                 93.357(3)
_cell_angle_gamma                90
_cell_volume                     3506.3(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4405
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      59.05
_cell_measurement_theta_min      3.75
_shelx_estimated_absorpt_T_max   0.919
_shelx_estimated_absorpt_T_min   0.684
_exptl_absorpt_coefficient_mu    0.776
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.6479
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1209 before and 0.0699 after correction.
The Ratio of minimum to maximum transmission is 0.8620.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0849
_diffrn_reflns_av_unetI/netI     0.0801
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17538
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        59.080
_diffrn_reflns_theta_max         59.080
_diffrn_reflns_theta_min         3.747
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2488
_reflns_number_total             4907
_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       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.169
_refine_diff_density_rms         0.036
_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     458
_refine_ls_number_reflns         4907
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1796
_refine_ls_R_factor_gt           0.0923
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0687P)²+3.0005P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1870
_refine_ls_wR_factor_ref         0.2268
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(O7B)=Sof(H14C)=Sof(H14D)=Sof(C15B)=Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(1)
 Sof(O7A)=Sof(H14A)=Sof(H14B)=Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(1)
 Sof(O9B)=Sof(H23C)=Sof(H23D)=Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(2)
 Sof(O9A)=Sof(H23A)=Sof(H23B)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(2)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C9(H9A,H9B), C11(H11A,
 H11B), C13(H13A,H13B), C14(H14C,H14D), C14(H14A,H14B), C16(H16A,H16B),
 C17(H17A,H17B), C19(H19A,H19B), C22(H22A,H22B), C23(H23C,H23D), C23(H23A,H23B),
  C25(H25A,H25B), C28(H28A,H28B), C29(H29A,H29B)
3.b Me refined with riding coordinates:
 C24B(H24D,H24E,H24F)
3.c Idealised Me refined as rotating group:
 C15A(H15A,H15B,H15C), C15B(H15D,H15E,H15F), C18(H18A,H18B,H18C), C24A(H24A,
 H24B,H24C), C30(H30A,H30B,H30C)
3.d :
 C21(H21), C27(H27)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
O1 O 1.1936(4) -0.00347(16) 0.7656(3) 0.1091(14) Uani 1 1 d . . . . .
O2 O 1.2557(4) 0.13747(18) 0.6215(3) 0.1211(15) Uani 1 1 d . . . . .
O3 O 0.9996(4) 0.29289(17) 0.6364(3) 0.1100(14) Uani 1 1 d . . . . .
O4 O 0.7874(5) 0.18909(19) 0.7702(3) 0.1177(15) Uani 1 1 d . . . . .
O5 O 0.7611(4) 0.06536(16) 0.5807(3) 0.1038(13) Uani 1 1 d . . . . .
O6 O 0.8017(3) 0.12760(16) 0.4024(3) 0.0915(12) Uani 1 1 d . . . . .
O7A O 0.8680(12) -0.0419(5) 0.7534(9) 0.132(5) Uani 0.595(14) 1 d . . P A 1
O7B O 0.7894(14) -0.0910(9) 0.7295(10) 0.150(7) Uani 0.405(14) 1 d . . P A 2
O8 O 0.9950(10) 0.0746(3) 0.9199(5) 0.216(3) Uani 1 1 d . . . . .
O9A O 0.577(4) 0.3467(12) 0.5882(14) 0.196(10) Uani 0.53(3) 1 d . . P B 1
O9B O 0.5326(18) 0.3276(9) 0.642(3) 0.168(10) Uani 0.47(3) 1 d . . P B 2
O10 O 0.5013(4) 0.1882(2) 0.4482(3) 0.1060(13) Uani 1 1 d . . . . .
N1 N 1.0766(4) -0.04812(17) 0.6105(3) 0.0827(13) Uani 1 1 d . . . . .
N2 N 1.1068(4) 0.0844(2) 0.7429(3) 0.0894(14) Uani 1 1 d . . . . .
N3 N 1.0887(4) 0.1939(2) 0.5642(3) 0.0855(13) Uani 1 1 d . . . . .
N4 N 0.7849(5) 0.2643(2) 0.6348(3) 0.0985(15) Uani 1 1 d . . . . .
N5 N 0.6389(5) 0.1281(3) 0.7021(4) 0.1010(15) Uani 1 1 d . . . . .
N6 N 0.5940(4) 0.06949(18) 0.4748(4) 0.0826(13) Uani 1 1 d . . . . .
C1 C 1.0691(5) 0.0127(2) 0.6255(4) 0.0861(16) Uani 1 1 d . . . . .
H1A H 0.975961 0.024454 0.619742 0.103 Uiso 1 1 calc R U . . .
H1B H 1.116151 0.032138 0.579374 0.103 Uiso 1 1 calc R U . . .
C2 C 1.1290(5) 0.0307(3) 0.7175(4) 0.0878(17) Uani 1 1 d . . . . .
C3 C 1.0417(5) 0.1252(2) 0.6825(4) 0.0903(17) Uani 1 1 d . . . . .
H3A H 1.001531 0.154629 0.717590 0.108 Uiso 1 1 calc R U . . .
H3B H 0.970265 0.106480 0.646964 0.108 Uiso 1 1 calc R U . . .
C4 C 1.1387(6) 0.1529(2) 0.6185(4) 0.0873(17) Uani 1 1 d . . . . .
C5 C 0.9481(5) 0.2085(2) 0.5561(4) 0.0830(16) Uani 1 1 d . . . . .
H5A H 0.895892 0.175877 0.572885 0.100 Uiso 1 1 calc R U . . .
H5B H 0.923122 0.217296 0.493747 0.100 Uiso 1 1 calc R U . . .
C6 C 0.9133(7) 0.2585(2) 0.6142(4) 0.0842(16) Uani 1 1 d . . . . .
C7 C 0.6895(6) 0.2176(3) 0.6277(4) 0.0950(18) Uani 1 1 d . . . . .
H7A H 0.701029 0.197091 0.572270 0.114 Uiso 1 1 calc R U . . .
H7B H 0.599069 0.232731 0.625190 0.114 Uiso 1 1 calc R U . . .
C8 C 0.7076(7) 0.1770(3) 0.7068(5) 0.0943(19) Uani 1 1 d . . . . .
C9 C 0.5612(5) 0.1103(3) 0.6223(4) 0.0935(18) Uani 1 1 d . . . . .
H9A H 0.520154 0.143290 0.593131 0.112 Uiso 1 1 calc R U . . .
H9B H 0.489934 0.085288 0.639310 0.112 Uiso 1 1 calc R U . . .
C10 C 0.6464(6) 0.0800(2) 0.5569(5) 0.0829(16) Uani 1 1 d . . . . .
C11 C 0.6819(5) 0.0409(2) 0.4147(4) 0.0932(18) Uani 1 1 d . . . . .
H11A H 0.633897 0.034496 0.357107 0.112 Uiso 1 1 calc R U . . .
H11B H 0.707778 0.004324 0.439805 0.112 Uiso 1 1 calc R U . . .
C12 C 0.8078(5) 0.0760(3) 0.4006(4) 0.0797(15) Uani 1 1 d . . . . .
C13 C 0.9550(5) -0.0804(3) 0.6259(5) 0.1008(19) Uani 1 1 d . . . . .
H13A H 0.966206 -0.118803 0.604113 0.121 Uiso 1 1 calc R U . . .
H13B H 0.880428 -0.063576 0.590858 0.121 Uiso 1 1 calc R U . . .
C14 C 0.9211(8) -0.0830(4) 0.7214(6) 0.126(2) Uani 1 1 d . . . . .
H14C H 0.970538 -0.113696 0.751126 0.151 Uiso 0.405(14) 1 calc R U P A 2
H14D H 0.948324 -0.047869 0.751052 0.151 Uiso 0.405(14) 1 calc R U P A 2
H14A H 0.862411 -0.115240 0.728115 0.151 Uiso 0.595(14) 1 calc R U P A 1
H14B H 1.003143 -0.090558 0.757378 0.151 Uiso 0.595(14) 1 calc R U P A 1
C15A C 0.857(2) -0.0441(8) 0.8440(13) 0.199(10) Uani 0.595(14) 1 d . . P A 1
H15A H 0.933780 -0.062940 0.871719 0.299 Uiso 0.595(14) 1 calc R U P A 1
H15B H 0.777234 -0.064608 0.856874 0.299 Uiso 0.595(14) 1 calc R U P A 1
H15C H 0.851677 -0.006284 0.867416 0.299 Uiso 0.595(14) 1 calc R U P A 1
C15B C 0.748(2) -0.0981(12) 0.8169(16) 0.159(10) Uani 0.405(14) 1 d . . P A 2
H15D H 0.742827 -0.137811 0.830202 0.239 Uiso 0.405(14) 1 calc R U P A 2
H15E H 0.661747 -0.080993 0.821588 0.239 Uiso 0.405(14) 1 calc R U P A 2
H15F H 0.811772 -0.080371 0.858758 0.239 Uiso 0.405(14) 1 calc R U P A 2
C16 C 1.1680(7) 0.1062(3) 0.8278(6) 0.127(2) Uani 1 1 d . . . . .
H16A H 1.218970 0.140115 0.816059 0.152 Uiso 1 1 calc R U . . .
H16B H 1.229569 0.078110 0.853965 0.152 Uiso 1 1 calc R U . . .
C17 C 1.0588(13) 0.1204(4) 0.8964(6) 0.187(4) Uani 1 1 d . . . . .
H17A H 1.101628 0.137973 0.949565 0.225 Uiso 1 1 calc R U . . .
H17B H 0.995086 0.147304 0.869292 0.225 Uiso 1 1 calc R U . . .
C18 C 0.9066(15) 0.0911(8) 0.9845(10) 0.375(13) Uani 1 1 d . . . . .
H18A H 0.946769 0.083818 1.043507 0.562 Uiso 1 1 calc R U . . .
H18B H 0.824790 0.069970 0.976107 0.562 Uiso 1 1 calc R U . . .
H18C H 0.887740 0.130856 0.978239 0.562 Uiso 1 1 calc R U . . .
C19 C 1.1825(6) 0.2274(3) 0.5137(5) 0.1021(19) Uani 1 1 d . . . . .
H19A H 1.183445 0.266038 0.535973 0.123 Uiso 1 1 calc R U . . .
H19B H 1.271974 0.212003 0.524555 0.123 Uiso 1 1 calc R U . . .
C20 C 1.1501(7) 0.2282(3) 0.4191(7) 0.108(2) Uani 1 1 d . . . . .
C21 C 1.1216(9) 0.2294(3) 0.3416(7) 0.140(3) Uani 1 1 d . . . . .
H21 H 1.099090 0.230305 0.280113 0.168 Uiso 1 1 calc R U . . .
C22 C 0.7499(7) 0.3121(3) 0.6917(5) 0.129(2) Uani 1 1 d . . . . .
H22A H 0.700037 0.297749 0.740865 0.154 Uiso 1 1 calc R U . . .
H22B H 0.831866 0.328939 0.717555 0.154 Uiso 1 1 calc R U . . .
C23 C 0.6721(15) 0.3552(5) 0.6457(9) 0.178(6) Uani 1 1 d . . . . .
H23C H 0.702429 0.362158 0.585994 0.214 Uiso 0.47(3) 1 calc R U P B 2
H23D H 0.673665 0.390419 0.679353 0.214 Uiso 0.47(3) 1 calc R U P B 2
H23A H 0.635471 0.378335 0.692166 0.214 Uiso 0.53(3) 1 calc R U P B 1
H23B H 0.735675 0.378991 0.616420 0.214 Uiso 0.53(3) 1 calc R U P B 1
C24A C 0.503(3) 0.3823(10) 0.5298(18) 0.267(16) Uani 0.53(3) 1 d . . P B 1
H24A H 0.490037 0.418121 0.558569 0.401 Uiso 0.53(3) 1 calc R U P B 1
H24B H 0.417587 0.365335 0.514105 0.401 Uiso 0.53(3) 1 calc R U P B 1
H24C H 0.550581 0.388035 0.476332 0.401 Uiso 0.53(3) 1 calc R U P B 1
C24B C 0.412(3) 0.3581(13) 0.622(3) 0.27(2) Uani 0.47(3) 1 d . . P B 2
H24D H 0.337347 0.332754 0.623227 0.399 Uiso 0.47(3) 1 calc R U P B 2
H24E H 0.403580 0.387376 0.666133 0.399 Uiso 0.47(3) 1 calc R U P B 2
H24F H 0.414652 0.374885 0.563478 0.399 Uiso 0.47(3) 1 calc R U P B 2
C25 C 0.6767(7) 0.0850(4) 0.7713(5) 0.137(3) Uani 1 1 d . . . . .
H25A H 0.737265 0.057897 0.746147 0.164 Uiso 1 1 calc R U . . .
H25B H 0.724741 0.103497 0.821621 0.164 Uiso 1 1 calc R U . . .
C26 C 0.5693(9) 0.0562(4) 0.8025(7) 0.155(3) Uani 1 1 d . . . . .
C27 C 0.4878(11) 0.0270(5) 0.8225(8) 0.205(5) Uani 1 1 d . . . . .
H27 H 0.420105 0.002800 0.839116 0.246 Uiso 1 1 calc R U . . .
C28 C 0.4632(5) 0.0893(3) 0.4383(4) 0.0958(18) Uani 1 1 d . . . . .
H28A H 0.404677 0.094444 0.487395 0.115 Uiso 1 1 calc R U . . .
H28B H 0.423743 0.060512 0.398618 0.115 Uiso 1 1 calc R U . . .
C29 C 0.4707(6) 0.1440(3) 0.3874(5) 0.1027(19) Uani 1 1 d . . . . .
H29A H 0.539301 0.141347 0.344187 0.123 Uiso 1 1 calc R U . . .
H29B H 0.385537 0.151388 0.354938 0.123 Uiso 1 1 calc R U . . .
C30 C 0.5347(8) 0.2391(3) 0.4054(5) 0.150(3) Uani 1 1 d . . . . .
H30A H 0.619282 0.234688 0.378727 0.225 Uiso 1 1 calc R U . . .
H30B H 0.541078 0.269156 0.448809 0.225 Uiso 1 1 calc R U . . .
H30C H 0.466627 0.248027 0.359466 0.225 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
O1 C2 1.235(6) . ?
O2 C4 1.223(6) . ?
O3 C6 1.216(6) . ?
O4 C8 1.233(7) . ?
O5 C10 1.228(6) . ?
O6 C12 1.218(6) . ?
O7A C14 1.215(10) . ?
O7A C15A 1.363(16) . ?
O7B C14 1.342(15) . ?
O7B C15B 1.40(2) . ?
O8 C17 1.313(9) . ?
O8 C18 1.398(13) . ?
O9A C23 1.26(3) . ?
O9A C24A 1.39(3) . ?
O9B C23 1.54(2) . ?
O9B C24B 1.42(3) . ?
O10 C29 1.403(7) . ?
O10 C30 1.409(7) . ?
N1 C1 1.456(6) . ?
N1 C12 1.348(6) 3_756 ?
N1 C13 1.464(6) . ?
N2 C2 1.345(6) . ?
N2 C3 1.446(6) . ?
N2 C16 1.465(7) . ?
N3 C4 1.339(7) . ?
N3 C5 1.445(6) . ?
N3 C19 1.467(7) . ?
N4 C6 1.344(7) . ?
N4 C7 1.457(7) . ?
N4 C22 1.464(7) . ?
N5 C8 1.342(7) . ?
N5 C9 1.444(7) . ?
N5 C25 1.481(8) . ?
N6 C10 1.325(7) . ?
N6 C11 1.456(6) . ?
N6 C28 1.463(6) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.523(7) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.543(8) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.515(7) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.522(8) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.512(8) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.531(7) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.483(9) . ?
C14 H14C 0.9700 . ?
C14 H14D 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15A H15A 0.9600 . ?
C15A H15B 0.9600 . ?
C15A H15C 0.9600 . ?
C15B H15D 0.9600 . ?
C15B H15E 0.9600 . ?
C15B H15F 0.9600 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.576(11) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.427(9) . ?
C20 C21 1.174(9) . ?
C21 H21 0.9300 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.431(12) . ?
C23 H23C 0.9700 . ?
C23 H23D 0.9700 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24A H24A 0.9600 . ?
C24A H24B 0.9600 . ?
C24A H24C 0.9600 . ?
C24B H24D 0.9600 . ?
C24B H24E 0.9600 . ?
C24B H24F 0.9600 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.374(10) . ?
C26 C27 1.120(10) . ?
C27 H27 0.9300 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C29 1.499(8) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?

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
C14 O7A C15A 114.9(11) . . ?
C14 O7B C15B 116.4(14) . . ?
C17 O8 C18 106.9(12) . . ?
C23 O9A C24A 133(3) . . ?
C24B O9B C23 123(2) . . ?
C29 O10 C30 113.0(5) . . ?
C1 N1 C13 116.1(4) . . ?
C12 N1 C1 123.6(4) 3_756 . ?
C12 N1 C13 119.3(5) 3_756 . ?
C2 N2 C3 121.9(5) . . ?
C2 N2 C16 120.3(5) . . ?
C3 N2 C16 117.0(5) . . ?
C4 N3 C5 123.3(5) . . ?
C4 N3 C19 118.2(5) . . ?
C5 N3 C19 118.5(5) . . ?
C6 N4 C7 122.4(5) . . ?
C6 N4 C22 118.4(5) . . ?
C7 N4 C22 116.5(5) . . ?
C8 N5 C9 122.8(6) . . ?
C8 N5 C25 116.4(6) . . ?
C9 N5 C25 118.5(6) . . ?
C10 N6 C11 115.7(5) . . ?
C10 N6 C28 125.4(5) . . ?
C11 N6 C28 118.5(5) . . ?
N1 C1 H1A 109.0 . . ?
N1 C1 H1B 109.0 . . ?
N1 C1 C2 113.0(5) . . ?
H1A C1 H1B 107.8 . . ?
C2 C1 H1A 109.0 . . ?
C2 C1 H1B 109.0 . . ?
O1 C2 N2 122.8(6) . . ?
O1 C2 C1 120.4(5) . . ?
N2 C2 C1 116.9(5) . . ?
N2 C3 H3A 109.0 . . ?
N2 C3 H3B 109.0 . . ?
N2 C3 C4 113.0(5) . . ?
H3A C3 H3B 107.8 . . ?
C4 C3 H3A 109.0 . . ?
C4 C3 H3B 109.0 . . ?
O2 C4 N3 124.0(6) . . ?
O2 C4 C3 119.0(6) . . ?
N3 C4 C3 117.0(5) . . ?
N3 C5 H5A 109.0 . . ?
N3 C5 H5B 109.0 . . ?
N3 C5 C6 113.0(4) . . ?
H5A C5 H5B 107.8 . . ?
C6 C5 H5A 109.0 . . ?
C6 C5 H5B 109.0 . . ?
O3 C6 N4 122.7(5) . . ?
O3 C6 C5 119.5(6) . . ?
N4 C6 C5 117.7(5) . . ?
N4 C7 H7A 109.2 . . ?
N4 C7 H7B 109.2 . . ?
N4 C7 C8 111.9(5) . . ?
H7A C7 H7B 107.9 . . ?
C8 C7 H7A 109.2 . . ?
C8 C7 H7B 109.2 . . ?
O4 C8 N5 123.0(7) . . ?
O4 C8 C7 119.3(7) . . ?
N5 C8 C7 117.6(6) . . ?
N5 C9 H9A 109.3 . . ?
N5 C9 H9B 109.3 . . ?
N5 C9 C10 111.8(5) . . ?
H9A C9 H9B 107.9 . . ?
C10 C9 H9A 109.3 . . ?
C10 C9 H9B 109.3 . . ?
O5 C10 N6 121.7(6) . . ?
O5 C10 C9 119.9(6) . . ?
N6 C10 C9 118.4(5) . . ?
N6 C11 H11A 109.4 . . ?
N6 C11 H11B 109.4 . . ?
N6 C11 C12 111.3(4) . . ?
H11A C11 H11B 108.0 . . ?
C12 C11 H11A 109.4 . . ?
C12 C11 H11B 109.4 . . ?
O6 C12 N1 122.4(5) . 3_756 ?
O6 C12 C11 119.6(5) . . ?
N1 C12 C11 118.0(5) 3_756 . ?
N1 C13 H13A 108.7 . . ?
N1 C13 H13B 108.7 . . ?
N1 C13 C14 114.2(5) . . ?
H13A C13 H13B 107.6 . . ?
C14 C13 H13A 108.7 . . ?
C14 C13 H13B 108.7 . . ?
O7A C14 C13 118.3(10) . . ?
O7A C14 H14A 107.7 . . ?
O7A C14 H14B 107.7 . . ?
O7B C14 C13 111.9(9) . . ?
O7B C14 H14C 109.2 . . ?
O7B C14 H14D 109.2 . . ?
C13 C14 H14C 109.2 . . ?
C13 C14 H14D 109.2 . . ?
C13 C14 H14A 107.7 . . ?
C13 C14 H14B 107.7 . . ?
H14C C14 H14D 107.9 . . ?
H14A C14 H14B 107.1 . . ?
O7A C15A H15A 109.5 . . ?
O7A C15A H15B 109.5 . . ?
O7A C15A H15C 109.5 . . ?
H15A C15A H15B 109.5 . . ?
H15A C15A H15C 109.5 . . ?
H15B C15A H15C 109.5 . . ?
O7B C15B H15D 109.5 . . ?
O7B C15B H15E 109.5 . . ?
O7B C15B H15F 109.5 . . ?
H15D C15B H15E 109.5 . . ?
H15D C15B H15F 109.5 . . ?
H15E C15B H15F 109.5 . . ?
N2 C16 H16A 109.3 . . ?
N2 C16 H16B 109.3 . . ?
N2 C16 C17 111.4(6) . . ?
H16A C16 H16B 108.0 . . ?
C17 C16 H16A 109.3 . . ?
C17 C16 H16B 109.3 . . ?
O8 C17 C16 111.3(9) . . ?
O8 C17 H17A 109.4 . . ?
O8 C17 H17B 109.4 . . ?
C16 C17 H17A 109.4 . . ?
C16 C17 H17B 109.4 . . ?
H17A C17 H17B 108.0 . . ?
O8 C18 H18A 109.5 . . ?
O8 C18 H18B 109.5 . . ?
O8 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 H19A 108.9 . . ?
N3 C19 H19B 108.9 . . ?
H19A C19 H19B 107.7 . . ?
C20 C19 N3 113.5(6) . . ?
C20 C19 H19A 108.9 . . ?
C20 C19 H19B 108.9 . . ?
C21 C20 C19 178.9(9) . . ?
C20 C21 H21 180.0 . . ?
N4 C22 H22A 108.7 . . ?
N4 C22 H22B 108.7 . . ?
H22A C22 H22B 107.6 . . ?
C23 C22 N4 114.2(7) . . ?
C23 C22 H22A 108.7 . . ?
C23 C22 H22B 108.7 . . ?
O9A C23 C22 125.4(17) . . ?
O9A C23 H23A 106.0 . . ?
O9A C23 H23B 106.0 . . ?
O9B C23 H23C 111.7 . . ?
O9B C23 H23D 111.7 . . ?
C22 C23 O9B 100.5(16) . . ?
C22 C23 H23C 111.7 . . ?
C22 C23 H23D 111.7 . . ?
C22 C23 H23A 106.0 . . ?
C22 C23 H23B 106.0 . . ?
H23C C23 H23D 109.4 . . ?
H23A C23 H23B 106.3 . . ?
O9A C24A H24A 109.5 . . ?
O9A C24A H24B 109.5 . . ?
O9A C24A H24C 109.5 . . ?
H24A C24A H24B 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
O9B C24B H24D 109.5 . . ?
O9B C24B H24E 109.5 . . ?
O9B C24B H24F 109.5 . . ?
H24D C24B H24E 109.5 . . ?
H24D C24B H24F 109.5 . . ?
H24E C24B H24F 109.5 . . ?
N5 C25 H25A 108.8 . . ?
N5 C25 H25B 108.8 . . ?
H25A C25 H25B 107.7 . . ?
C26 C25 N5 113.7(7) . . ?
C26 C25 H25A 108.8 . . ?
C26 C25 H25B 108.8 . . ?
C27 C26 C25 171.3(13) . . ?
C26 C27 H27 180.0 . . ?
N6 C28 H28A 108.9 . . ?
N6 C28 H28B 108.9 . . ?
N6 C28 C29 113.2(4) . . ?
H28A C28 H28B 107.8 . . ?
C29 C28 H28A 108.9 . . ?
C29 C28 H28B 108.9 . . ?
O10 C29 C28 109.1(5) . . ?
O10 C29 H29A 109.9 . . ?
O10 C29 H29B 109.9 . . ?
C28 C29 H29A 109.9 . . ?
C28 C29 H29B 109.9 . . ?
H29A C29 H29B 108.3 . . ?
O10 C30 H30A 109.5 . . ?
O10 C30 H30B 109.5 . . ?
O10 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 O1 10.1(8) . . . . ?
N1 C1 C2 N2 -169.3(5) . . . . ?
N1 C13 C14 O7A 78.3(11) . . . . ?
N1 C13 C14 O7B 154.2(12) . . . . ?
N2 C3 C4 O2 2.5(7) . . . . ?
N2 C3 C4 N3 -175.8(5) . . . . ?
N2 C16 C17 O8 64.3(11) . . . . ?
N3 C5 C6 O3 24.7(8) . . . . ?
N3 C5 C6 N4 -159.0(5) . . . . ?
N4 C7 C8 O4 6.5(7) . . . . ?
N4 C7 C8 N5 -170.8(5) . . . . ?
N4 C22 C23 O9A 41(3) . . . . ?
N4 C22 C23 O9B 78.7(17) . . . . ?
N5 C9 C10 O5 11.4(7) . . . . ?
N5 C9 C10 N6 -169.1(5) . . . . ?
N6 C11 C12 O6 -31.8(7) . . . . ?
N6 C11 C12 N1 146.1(5) . . . 3_756 ?
N6 C28 C29 O10 -70.7(6) . . . . ?
C1 N1 C13 C14 -68.2(8) . . . . ?
C2 N2 C3 C4 -82.6(6) . . . . ?
C2 N2 C16 C17 -114.4(7) . . . . ?
C3 N2 C2 O1 174.1(5) . . . . ?
C3 N2 C2 C1 -6.5(8) . . . . ?
C3 N2 C16 C17 75.6(8) . . . . ?
C4 N3 C5 C6 96.9(6) . . . . ?
C4 N3 C19 C20 125.7(6) . . . . ?
C5 N3 C4 O2 174.7(5) . . . . ?
C5 N3 C4 C3 -7.1(7) . . . . ?
C5 N3 C19 C20 -57.0(7) . . . . ?
C6 N4 C7 C8 78.2(7) . . . . ?
C6 N4 C22 C23 109.5(9) . . . . ?
C7 N4 C6 O3 -164.9(6) . . . . ?
C7 N4 C6 C5 18.9(8) . . . . ?
C7 N4 C22 C23 -89.0(10) . . . . ?
C8 N5 C9 C10 85.1(7) . . . . ?
C8 N5 C25 C26 140.8(7) . . . . ?
C9 N5 C8 O4 -170.5(5) . . . . ?
C9 N5 C8 C7 6.7(8) . . . . ?
C9 N5 C25 C26 -56.0(9) . . . . ?
C10 N6 C11 C12 -60.2(6) . . . . ?
C10 N6 C28 C29 93.8(7) . . . . ?
C11 N6 C10 O5 -1.4(8) . . . . ?
C11 N6 C10 C9 179.1(4) . . . . ?
C11 N6 C28 C29 -79.2(6) . . . . ?
C12 N1 C1 C2 -69.8(7) 3_756 . . . ?
C12 N1 C13 C14 100.4(7) 3_756 . . . ?
C13 N1 C1 C2 98.2(6) . . . . ?
C15A O7A C14 C13 -171.2(13) . . . . ?
C15B O7B C14 C13 175.5(16) . . . . ?
C16 N2 C2 O1 4.6(9) . . . . ?
C16 N2 C2 C1 -176.0(5) . . . . ?
C16 N2 C3 C4 87.3(6) . . . . ?
C18 O8 C17 C16 176.5(9) . . . . ?
C19 N3 C4 O2 -8.1(8) . . . . ?
C19 N3 C4 C3 170.1(5) . . . . ?
C19 N3 C5 C6 -80.2(6) . . . . ?
C22 N4 C6 O3 -4.5(9) . . . . ?
C22 N4 C6 C5 179.3(6) . . . . ?
C22 N4 C7 C8 -82.5(6) . . . . ?
C24A O9A C23 C22 -171(2) . . . . ?
C24B O9B C23 C22 164(2) . . . . ?
C25 N5 C8 O4 -8.1(9) . . . . ?
C25 N5 C8 C7 169.1(5) . . . . ?
C25 N5 C9 C10 -77.0(6) . . . . ?
C28 N6 C10 O5 -174.6(5) . . . . ?
C28 N6 C10 C9 5.9(8) . . . . ?
C28 N6 C11 C12 113.5(5) . . . . ?
C30 O10 C29 C28 168.9(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: chloroform/diethyl ether'
####################################################################### 
# 
# 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_res84_tol_squeeze
_database_code_depnum_ccdc_archive 'CCDC 2117235'
loop_
_audit_author_name
_audit_author_address
'Giovanni Pierri'
;University of Salerno
Italy
;
_audit_update_record             
;
2022-03-16 deposited with the CCDC.	2022-03-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_res84_tol_squeeze   
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.939 Why?
RESPONSE: This is due to the  weak diffracting power of the sample
;
# Added during the CSD deposition process: Wednesday 16 March 2022 11:45 AM
# end Validation Reply Form

_audit_creation_date             2022-02-23
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H60 N12 O12, [+ solvents]'
_chemical_formula_sum            'C60 H60 N12 O12'
_chemical_formula_weight         1141.20
_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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.1468(17)
_cell_length_b                   19.626(4)
_cell_length_c                   18.398(5)
_cell_angle_alpha                90
_cell_angle_beta                 98.846(17)
_cell_angle_gamma                90
_cell_volume                     3620.3(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4298
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      74.03
_cell_measurement_theta_min      4.69
_shelx_estimated_absorpt_T_max   0.913
_shelx_estimated_absorpt_T_min   0.732
_exptl_absorpt_coefficient_mu    0.616
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.5944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1022 before and 0.0556 after correction.
The Ratio of minimum to maximum transmission is 0.7885.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.047
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0776
_diffrn_reflns_Laue_measured_fraction_full 0.939
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11770
_diffrn_reflns_point_group_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.694
_diffrn_reflns_theta_min         4.506
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4433
_reflns_number_total             6577
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         0.222
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       0.0029(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         6577
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0660
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0908P)²+0.6687P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1796
_refine_ls_wR_factor_ref         0.1969
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Others
 Sof(H16C)=Sof(H16D)=Sof(C17B)=Sof(C18B)=Sof(H18B)=1-FVAR(1)
 Sof(H16A)=Sof(H16B)=Sof(C17A)=Sof(C18A)=Sof(H18A)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C9(H9A,H9B), C11(H11A,
 H11B), C13(H13A,H13B), C16(H16C,H16D), C16(H16A,H16B), C19(H19A,H19B),
 C22(H22A,H22B), C25(H25A,H25B), C28(H28A,H28B)
3.b :
 C15(H15), C18A(H18A), C21(H21), C24(H24), C27(H27), C30(H30), C18B(H18B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
O1 O 0.5704(2) 0.40479(11) 0.29279(11) 0.0722(6) Uani 1 1 d . . . . .
O2 O 0.2180(2) 0.47605(11) 0.30932(13) 0.0770(6) Uani 1 1 d . . . . .
O3 O 0.10079(18) 0.66329(11) 0.20514(11) 0.0712(6) Uani 1 1 d . . . . .
O4 O 0.48056(19) 0.72411(12) 0.22353(10) 0.0772(7) Uani 1 1 d . . . . .
O5 O 0.52602(17) 0.65450(10) 0.41235(10) 0.0612(5) Uani 1 1 d . . . . .
O6 O 0.29460(16) 0.66038(10) 0.51494(10) 0.0635(5) Uani 1 1 d . . . . .
N1 N 0.64312(18) 0.44105(12) 0.43441(11) 0.0520(6) Uani 1 1 d . . . . .
N2 N 0.4475(2) 0.49785(12) 0.25884(11) 0.0536(6) Uani 1 1 d . . . . .
N3 N 0.17231(18) 0.58617(12) 0.32889(11) 0.0513(5) Uani 1 1 d . . . . .
N4 N 0.2333(2) 0.75117(12) 0.24580(11) 0.0549(6) Uani 1 1 d . . . . .
N5 N 0.5857(2) 0.76115(13) 0.33287(11) 0.0625(6) Uani 1 1 d . . . . .
N6 N 0.5473(2) 0.70867(12) 0.52036(11) 0.0553(6) Uani 1 1 d . . . . .
C1 C 0.5451(2) 0.48319(14) 0.38832(13) 0.0507(6) Uani 1 1 d . . . . .
H1A H 0.576016 0.530005 0.389848 0.061 Uiso 1 1 calc R U . . .
H1B H 0.461371 0.482071 0.407641 0.061 Uiso 1 1 calc R U . . .
C2 C 0.5222(2) 0.45846(15) 0.30908(14) 0.0525(6) Uani 1 1 d . . . . .
C3 C 0.3753(2) 0.55676(14) 0.27912(14) 0.0513(6) Uani 1 1 d . . . . .
H3A H 0.353544 0.586340 0.236727 0.062 Uiso 1 1 calc R U . . .
H3B H 0.431395 0.582145 0.317213 0.062 Uiso 1 1 calc R U . . .
C4 C 0.2473(2) 0.53572(15) 0.30696(14) 0.0517(6) Uani 1 1 d . . . . .
C5 C 0.2130(2) 0.65657(14) 0.32849(14) 0.0518(6) Uani 1 1 d . . . . .
H5A H 0.308715 0.659138 0.343905 0.062 Uiso 1 1 calc R U . . .
H5B H 0.170656 0.681515 0.364118 0.062 Uiso 1 1 calc R U . . .
C6 C 0.1785(2) 0.69067(14) 0.25403(13) 0.0498(6) Uani 1 1 d . . . . .
C7 C 0.3424(2) 0.77857(14) 0.29891(14) 0.0516(6) Uani 1 1 d . . . . .
H7A H 0.330480 0.765308 0.348265 0.062 Uiso 1 1 calc R U . . .
H7B H 0.341723 0.827934 0.296391 0.062 Uiso 1 1 calc R U . . .
C8 C 0.4753(3) 0.75181(15) 0.28248(13) 0.0564(7) Uani 1 1 d . . . . .
C9 C 0.5767(3) 0.77316(15) 0.41000(13) 0.0584(7) Uani 1 1 d . . . . .
H9A H 0.506217 0.805746 0.413753 0.070 Uiso 1 1 calc R U . . .
H9B H 0.659990 0.792376 0.434411 0.070 Uiso 1 1 calc R U . . .
C10 C 0.5481(2) 0.70745(14) 0.44771(13) 0.0480(6) Uani 1 1 d . . . . .
C11 C 0.5281(2) 0.64484(17) 0.55641(15) 0.0631(8) Uani 1 1 d . . . . .
H11A H 0.558148 0.649686 0.608806 0.076 Uiso 1 1 calc R U . . .
H11B H 0.582434 0.610035 0.538070 0.076 Uiso 1 1 calc R U . . .
C12 C 0.3833(2) 0.62200(15) 0.54393(13) 0.0499(6) Uani 1 1 d . . . . .
C13 C 0.7824(2) 0.46204(16) 0.43689(16) 0.0596(7) Uani 1 1 d . . . . .
H13A H 0.840273 0.427182 0.461871 0.072 Uiso 1 1 calc R U . . .
H13B H 0.801803 0.465812 0.387032 0.072 Uiso 1 1 calc R U . . .
C14 C 0.8114(2) 0.52621(17) 0.47413(16) 0.0601(7) Uani 1 1 d . . . . .
C15 C 0.8366(3) 0.5775(2) 0.5036(2) 0.0888(11) Uani 1 1 d . . . . .
H15 H 0.856997 0.618873 0.527432 0.107 Uiso 1 1 calc R U . . .
C16 C 0.4083(3) 0.4687(2) 0.18549(16) 0.0795(10) Uani 1 1 d . . . . .
H16C H 0.315705 0.479023 0.167037 0.095 Uiso 0.31(4) 1 calc R U P A 2
H16D H 0.419665 0.419604 0.186747 0.095 Uiso 0.31(4) 1 calc R U P A 2
H16A H 0.382942 0.421626 0.191643 0.095 Uiso 0.69(4) 1 calc R U P A 1
H16B H 0.329061 0.492543 0.162408 0.095 Uiso 0.69(4) 1 calc R U P A 1
C17A C 0.499(2) 0.4696(15) 0.1373(9) 0.123(6) Uani 0.69(4) 1 d . . P A 1
C18A C 0.5788(16) 0.470(2) 0.0972(8) 0.219(12) Uani 0.69(4) 1 d . . P A 1
H18A H 0.641862 0.471155 0.065454 0.262 Uiso 0.69(4) 1 calc R U P A 1
C19 C 0.0488(2) 0.56831(17) 0.35662(16) 0.0663(8) Uani 1 1 d . . . . .
H19A H 0.060310 0.524047 0.380183 0.080 Uiso 1 1 calc R U . . .
H19B H 0.034146 0.601227 0.393893 0.080 Uiso 1 1 calc R U . . .
C20 C -0.0695(3) 0.56613(18) 0.30093(19) 0.0754(9) Uani 1 1 d . . . . .
C21 C -0.1673(3) 0.5619(3) 0.2602(2) 0.1136(15) Uani 1 1 d . . . . .
H21 H -0.246339 0.558549 0.227279 0.136 Uiso 1 1 calc R U . . .
C22 C 0.1999(3) 0.78646(16) 0.17639(16) 0.0644(8) Uani 1 1 d . . . . .
H22A H 0.277263 0.811494 0.165920 0.077 Uiso 1 1 calc R U . . .
H22B H 0.176149 0.753406 0.137379 0.077 Uiso 1 1 calc R U . . .
C23 C 0.0900(3) 0.83318(17) 0.17763(18) 0.0747(9) Uani 1 1 d . . . . .
C24 C 0.0023(4) 0.8696(2) 0.1817(3) 0.1204(17) Uani 1 1 d . . . . .
H24 H -0.068436 0.898965 0.184900 0.144 Uiso 1 1 calc R U . . .
C25 C 0.7087(3) 0.7294(2) 0.31589(18) 0.0914(12) Uani 1 1 d . . . . .
H25A H 0.705675 0.681146 0.326824 0.110 Uiso 1 1 calc R U . . .
H25B H 0.710023 0.733872 0.263504 0.110 Uiso 1 1 calc R U . . .
C26 C 0.8274(4) 0.7560(3) 0.3534(3) 0.141(2) Uani 1 1 d . . . . .
C27 C 0.9280(6) 0.7747(5) 0.3842(6) 0.282(6) Uani 1 1 d . . . . .
H27 H 1.009399 0.789865 0.409184 0.339 Uiso 1 1 calc R U . . .
C28 C 0.5659(3) 0.77078(16) 0.56440(14) 0.0611(8) Uani 1 1 d . . . . .
H28A H 0.533212 0.809298 0.533816 0.073 Uiso 1 1 calc R U . . .
H28B H 0.513103 0.767684 0.603986 0.073 Uiso 1 1 calc R U . . .
C29 C 0.7043(3) 0.78289(18) 0.59562(17) 0.0741(9) Uani 1 1 d . . . . .
C30 C 0.8139(4) 0.7933(2) 0.6220(2) 0.1119(15) Uani 1 1 d . . . . .
H30 H 0.901701 0.801721 0.643039 0.134 Uiso 1 1 calc R U . . .
C17B C 0.498(4) 0.501(2) 0.1382(11) 0.098(11) Uani 0.31(4) 1 d . . P A 2
C18B C 0.561(4) 0.528(3) 0.0970(17) 0.165(14) Uani 0.31(4) 1 d . . P A 2
H18B H 0.609746 0.549711 0.064894 0.198 Uiso 0.31(4) 1 calc R U 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
O1 C2 1.218(3) . ?
O2 C4 1.210(3) . ?
O3 C6 1.225(3) . ?
O4 C8 1.222(3) . ?
O5 C10 1.228(3) . ?
O6 C12 1.231(3) . ?
N1 C1 1.461(3) . ?
N1 C12 1.340(3) 3_666 ?
N1 C13 1.466(3) . ?
N2 C2 1.346(3) . ?
N2 C3 1.448(3) . ?
N2 C16 1.464(3) . ?
N3 C4 1.348(3) . ?
N3 C5 1.442(3) . ?
N3 C19 1.467(3) . ?
N4 C6 1.330(3) . ?
N4 C7 1.462(3) . ?
N4 C22 1.446(3) . ?
N5 C8 1.352(3) . ?
N5 C9 1.455(3) . ?
N5 C25 1.470(4) . ?
N6 C10 1.338(3) . ?
N6 C11 1.445(4) . ?
N6 C28 1.460(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.520(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.525(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.516(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.520(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.514(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.519(3) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.442(4) . ?
C14 C15 1.154(4) . ?
C15 H15 0.9300 . ?
C16 H16C 0.9700 . ?
C16 H16D 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17A 1.37(2) . ?
C16 C17B 1.49(3) . ?
C17A C18A 1.18(2) . ?
C18A H18A 0.9300 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.454(4) . ?
C20 C21 1.151(5) . ?
C21 H21 0.9300 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.446(4) . ?
C23 C24 1.153(5) . ?
C24 H24 0.9300 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.394(5) . ?
C26 C27 1.149(7) . ?
C27 H27 0.9300 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C29 1.453(4) . ?
C29 C30 1.161(4) . ?
C30 H30 0.9300 . ?
C17B C18B 1.19(4) . ?
C18B H18B 0.9300 . ?

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
C1 N1 C13 115.2(2) . . ?
C12 N1 C1 123.1(2) 3_666 . ?
C12 N1 C13 119.1(2) 3_666 . ?
C2 N2 C3 122.4(2) . . ?
C2 N2 C16 116.9(2) . . ?
C3 N2 C16 118.3(2) . . ?
C4 N3 C5 121.8(2) . . ?
C4 N3 C19 118.7(2) . . ?
C5 N3 C19 119.4(2) . . ?
C6 N4 C7 122.6(2) . . ?
C6 N4 C22 118.9(2) . . ?
C22 N4 C7 117.7(2) . . ?
C8 N5 C9 121.4(2) . . ?
C8 N5 C25 115.9(2) . . ?
C9 N5 C25 117.3(2) . . ?
C10 N6 C11 117.7(2) . . ?
C10 N6 C28 123.3(2) . . ?
C11 N6 C28 119.0(2) . . ?
N1 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
N1 C1 C2 111.5(2) . . ?
H1A C1 H1B 108.0 . . ?
C2 C1 H1A 109.3 . . ?
C2 C1 H1B 109.3 . . ?
O1 C2 N2 122.2(2) . . ?
O1 C2 C1 120.3(2) . . ?
N2 C2 C1 117.5(2) . . ?
N2 C3 H3A 109.4 . . ?
N2 C3 H3B 109.4 . . ?
N2 C3 C4 111.2(2) . . ?
H3A C3 H3B 108.0 . . ?
C4 C3 H3A 109.4 . . ?
C4 C3 H3B 109.4 . . ?
O2 C4 N3 123.2(2) . . ?
O2 C4 C3 120.0(3) . . ?
N3 C4 C3 116.8(2) . . ?
N3 C5 H5A 108.8 . . ?
N3 C5 H5B 108.8 . . ?
N3 C5 C6 113.6(2) . . ?
H5A C5 H5B 107.7 . . ?
C6 C5 H5A 108.8 . . ?
C6 C5 H5B 108.8 . . ?
O3 C6 N4 122.8(2) . . ?
O3 C6 C5 120.2(2) . . ?
N4 C6 C5 117.0(2) . . ?
N4 C7 H7A 109.6 . . ?
N4 C7 H7B 109.6 . . ?
N4 C7 C8 110.1(2) . . ?
H7A C7 H7B 108.2 . . ?
C8 C7 H7A 109.6 . . ?
C8 C7 H7B 109.6 . . ?
O4 C8 N5 121.6(2) . . ?
O4 C8 C7 119.4(2) . . ?
N5 C8 C7 118.9(2) . . ?
N5 C9 H9A 109.5 . . ?
N5 C9 H9B 109.5 . . ?
N5 C9 C10 110.7(2) . . ?
H9A C9 H9B 108.1 . . ?
C10 C9 H9A 109.5 . . ?
C10 C9 H9B 109.5 . . ?
O5 C10 N6 121.0(2) . . ?
O5 C10 C9 120.7(2) . . ?
N6 C10 C9 118.3(2) . . ?
N6 C11 H11A 109.1 . . ?
N6 C11 H11B 109.1 . . ?
N6 C11 C12 112.4(2) . . ?
H11A C11 H11B 107.8 . . ?
C12 C11 H11A 109.1 . . ?
C12 C11 H11B 109.1 . . ?
O6 C12 N1 121.8(2) . 3_666 ?
O6 C12 C11 120.7(3) . . ?
N1 C12 C11 117.4(2) 3_666 . ?
N1 C13 H13A 109.1 . . ?
N1 C13 H13B 109.1 . . ?
H13A C13 H13B 107.8 . . ?
C14 C13 N1 112.7(2) . . ?
C14 C13 H13A 109.1 . . ?
C14 C13 H13B 109.1 . . ?
C15 C14 C13 178.9(3) . . ?
C14 C15 H15 180.0 . . ?
N2 C16 H16C 110.6 . . ?
N2 C16 H16D 110.6 . . ?
N2 C16 H16A 107.7 . . ?
N2 C16 H16B 107.7 . . ?
N2 C16 C17B 105.6(12) . . ?
H16C C16 H16D 108.7 . . ?
H16A C16 H16B 107.1 . . ?
C17A C16 N2 118.4(8) . . ?
C17A C16 H16A 107.7 . . ?
C17A C16 H16B 107.7 . . ?
C17B C16 H16C 110.6 . . ?
C17B C16 H16D 110.6 . . ?
C18A C17A C16 178.7(18) . . ?
C17A C18A H18A 180.0 . . ?
N3 C19 H19A 108.6 . . ?
N3 C19 H19B 108.6 . . ?
H19A C19 H19B 107.5 . . ?
C20 C19 N3 114.8(2) . . ?
C20 C19 H19A 108.6 . . ?
C20 C19 H19B 108.6 . . ?
C21 C20 C19 175.4(4) . . ?
C20 C21 H21 180.0 . . ?
N4 C22 H22A 109.3 . . ?
N4 C22 H22B 109.3 . . ?
H22A C22 H22B 108.0 . . ?
C23 C22 N4 111.5(2) . . ?
C23 C22 H22A 109.3 . . ?
C23 C22 H22B 109.3 . . ?
C24 C23 C22 177.1(4) . . ?
C23 C24 H24 180.0 . . ?
N5 C25 H25A 108.4 . . ?
N5 C25 H25B 108.4 . . ?
H25A C25 H25B 107.4 . . ?
C26 C25 N5 115.7(3) . . ?
C26 C25 H25A 108.4 . . ?
C26 C25 H25B 108.4 . . ?
C27 C26 C25 176.6(7) . . ?
C26 C27 H27 180.0 . . ?
N6 C28 H28A 109.0 . . ?
N6 C28 H28B 109.0 . . ?
H28A C28 H28B 107.8 . . ?
C29 C28 N6 113.0(2) . . ?
C29 C28 H28A 109.0 . . ?
C29 C28 H28B 109.0 . . ?
C30 C29 C28 178.4(4) . . ?
C29 C30 H30 180.0 . . ?
C18B C17B C16 175(3) . . ?
C17B C18B H18B 180.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 O1 8.6(4) . . . . ?
N1 C1 C2 N2 -171.6(2) . . . . ?
N2 C3 C4 O2 -0.4(3) . . . . ?
N2 C3 C4 N3 178.8(2) . . . . ?
N3 C5 C6 O3 13.4(3) . . . . ?
N3 C5 C6 N4 -168.2(2) . . . . ?
N4 C7 C8 O4 13.8(4) . . . . ?
N4 C7 C8 N5 -168.1(2) . . . . ?
N5 C9 C10 O5 -5.4(3) . . . . ?
N5 C9 C10 N6 174.8(2) . . . . ?
N6 C11 C12 O6 -9.5(4) . . . . ?
N6 C11 C12 N1 170.4(2) . . . 3_666 ?
C1 N1 C13 C14 68.1(3) . . . . ?
C2 N2 C3 C4 -78.2(3) . . . . ?
C2 N2 C16 C17A -80.6(14) . . . . ?
C2 N2 C16 C17B -103(2) . . . . ?
C3 N2 C2 O1 171.4(2) . . . . ?
C3 N2 C2 C1 -8.4(4) . . . . ?
C3 N2 C16 C17A 116.6(13) . . . . ?
C3 N2 C16 C17B 94(2) . . . . ?
C4 N3 C5 C6 83.0(3) . . . . ?
C4 N3 C19 C20 -90.6(3) . . . . ?
C5 N3 C4 O2 177.1(2) . . . . ?
C5 N3 C4 C3 -2.0(3) . . . . ?
C5 N3 C19 C20 91.8(3) . . . . ?
C6 N4 C7 C8 84.8(3) . . . . ?
C6 N4 C22 C23 93.6(3) . . . . ?
C7 N4 C6 O3 -169.3(2) . . . . ?
C7 N4 C6 C5 12.4(3) . . . . ?
C7 N4 C22 C23 -96.4(3) . . . . ?
C8 N5 C9 C10 76.8(3) . . . . ?
C8 N5 C25 C26 160.1(4) . . . . ?
C9 N5 C8 O4 -159.9(3) . . . . ?
C9 N5 C8 C7 22.1(4) . . . . ?
C9 N5 C25 C26 -45.4(5) . . . . ?
C10 N6 C11 C12 -77.4(3) . . . . ?
C10 N6 C28 C29 -92.1(3) . . . . ?
C11 N6 C10 O5 4.0(3) . . . . ?
C11 N6 C10 C9 -176.2(2) . . . . ?
C11 N6 C28 C29 87.2(3) . . . . ?
C12 N1 C1 C2 -73.8(3) 3_666 . . . ?
C12 N1 C13 C14 -129.5(3) 3_666 . . . ?
C13 N1 C1 C2 87.8(3) . . . . ?
C16 N2 C2 O1 9.4(4) . . . . ?
C16 N2 C2 C1 -170.4(2) . . . . ?
C16 N2 C3 C4 83.6(3) . . . . ?
C19 N3 C4 O2 -0.4(4) . . . . ?
C19 N3 C4 C3 -179.6(2) . . . . ?
C19 N3 C5 C6 -99.5(3) . . . . ?
C22 N4 C6 O3 0.1(4) . . . . ?
C22 N4 C6 C5 -178.1(2) . . . . ?
C22 N4 C7 C8 -84.8(3) . . . . ?
C25 N5 C8 O4 -6.5(4) . . . . ?
C25 N5 C8 C7 175.5(3) . . . . ?
C25 N5 C9 C10 -76.3(3) . . . . ?
C28 N6 C10 O5 -176.6(2) . . . . ?
C28 N6 C10 C9 3.2(3) . . . . ?
C28 N6 C11 C12 103.2(3) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 132 electrons were 
found in a volume of 740Å³ in 1 void per unit cell. 
This is consistent with the presence of 
1[C5H12O2] per Formula Unit 
which account for 116 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.500 370.5 65.5 '1 C5H12O2'
2 0.000 0.500 0.000 370.5 65.5 '1 C5H12O2'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol/toluene'
####################################################################### 
# 
# 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_res55_a4__28_squeeze_h_water
_database_code_depnum_ccdc_archive 'CCDC 2117236'
loop_
_audit_author_name
_audit_author_address
'Giovanni Pierri'
;University of Salerno
Italy
;
_audit_update_record             
;
2022-03-25 deposited with the CCDC.	2022-03-28 downloaded from the CCDC.
;
_audit_creation_date             2022-03-25
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H92 N12 O20, 0.556(H2 O), 2[C3H8O]'
_chemical_formula_sum            'C66 H109.11 N12 O22.56'
_chemical_formula_weight         1431.72
_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.5603(5)
_cell_length_b                   13.0290(5)
_cell_length_c                   14.4868(6)
_cell_angle_alpha                105.2750(10)
_cell_angle_beta                 108.615(2)
_cell_angle_gamma                99.629(2)
_cell_volume                     1917.90(14)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      72.92
_cell_measurement_theta_min      3.66
_shelx_estimated_absorpt_T_max   0.947
_shelx_estimated_absorpt_T_min   0.656
_exptl_absorpt_coefficient_mu    0.779
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.4442
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1448 before and 0.0653 after correction.
The Ratio of minimum to maximum transmission is 0.5893.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             770
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23947
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.310
_diffrn_reflns_theta_min         3.658
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5414
_reflns_number_total             7207
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.034
_refine_ls_extinction_coef       0.0047(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         7207
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0521
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0804P)²+0.2685P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1440
_refine_ls_wR_factor_ref         0.1561
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O1W-H1WA = O1W-H1WB
 0.85 with sigma of 0.02
 H1WA-H1WB
 1.34 with sigma of 0.04
3. Others
 Sof(H19C)=Sof(H19D)=Sof(C20B)=Sof(H20C)=Sof(H20D)=1-FVAR(1)
 Sof(H19A)=Sof(H19B)=Sof(C20A)=Sof(H20A)=Sof(H20B)=FVAR(1)
 Sof(O7B)=Sof(H16C)=Sof(H16D)=Sof(C17B)=Sof(H17C)=Sof(H17D)=Sof(C18B)=
 Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(2)
 Sof(O7A)=Sof(H16A)=Sof(H16B)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(C18A)=
 Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(2)
 Sof(O1W)=Sof(H1WA)=Sof(H1WB)=FVAR(3)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C9(H9A,H9B), C11(H11A,
 H11B), C13(H13A,H13B), C16(H16A,H16B), C16(H16C,H16D), C17A(H17A,H17B),
 C17B(H17C,H17D), C19A(H19A,H19B), C19A(H19C,H19D), C20A(H20A,H20B), C20B(H20C,
 H20D), C22(H22A,H22B), C25(H25A,H25B), C26(H26A,H26B), C28(H28A,H28B),
 C29(H29A,H29B)
4.b Idealised Me refined as rotating group:
 C18A(H18A,H18B,H18C), C18B(H18D,H18E,H18F), C21(H21A,H21B,H21C), C27(H27A,
 H27B,H27C), C30(H30A,H30B,H30C)
4.c :
 C15(H15), C24(H24)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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
O1 O 0.52969(14) 0.27114(12) 0.73014(11) 0.0704(4) Uani 1 1 d . . . . .
O2 O 0.37812(15) 0.11949(14) 0.90439(13) 0.0800(5) Uani 1 1 d . . . . .
O3 O -0.03080(17) 0.02649(11) 0.82114(14) 0.0859(5) Uani 1 1 d . . . . .
O4 O -0.06940(17) 0.19553(11) 0.63552(11) 0.0797(4) Uani 1 1 d . . . . .
O5 O 0.18136(12) 0.43881(9) 0.84966(10) 0.0556(3) Uani 1 1 d . . . . .
O6 O 0.19472(12) 0.49689(11) 1.07314(10) 0.0612(3) Uani 1 1 d . . . . .
O7A O 0.2200(5) 0.1430(4) 0.5243(3) 0.0877(14) Uani 0.510(7) 1 d . . P A 1
O7B O 0.1426(4) 0.1119(4) 0.5496(3) 0.0806(15) Uani 0.490(7) 1 d . . P A 2
O8 O 0.18156(19) 0.23169(15) 1.14036(13) 0.0908(5) Uani 1 1 d . . . . .
O9 O 0.1316(2) 0.40880(18) 0.51901(14) 0.1037(6) Uani 1 1 d . . . . .
O10 O 0.12634(18) 0.73073(13) 0.79541(12) 0.0857(5) Uani 1 1 d . . . . .
N1 N 0.59173(13) 0.46624(11) 0.88066(11) 0.0514(3) Uani 1 1 d . . . . .
N2 N 0.34801(14) 0.19756(12) 0.74453(12) 0.0543(4) Uani 1 1 d . . . . .
N3 N 0.21090(16) 0.16330(13) 0.93594(13) 0.0613(4) Uani 1 1 d . . . . .
N4 N -0.11782(15) 0.16377(13) 0.79574(12) 0.0608(4) Uani 1 1 d . . . . .
N5 N -0.04276(15) 0.38010(12) 0.68705(11) 0.0576(4) Uani 1 1 d . . . . .
N6 N 0.16574(13) 0.60412(11) 0.93158(11) 0.0493(3) Uani 1 1 d . . . . .
C1 C 0.47446(16) 0.38615(14) 0.85803(14) 0.0497(4) Uani 1 1 d . . . . .
H1A H 0.404041 0.417688 0.837685 0.060 Uiso 1 1 calc R U . . .
H1B H 0.477300 0.369492 0.920019 0.060 Uiso 1 1 calc R U . . .
C2 C 0.45238(16) 0.27904(14) 0.77131(14) 0.0511(4) Uani 1 1 d . . . . .
C3 C 0.25906(16) 0.20627(14) 0.79541(14) 0.0532(4) Uani 1 1 d . . . . .
H3A H 0.173899 0.166633 0.745070 0.064 Uiso 1 1 calc R U . . .
H3B H 0.261543 0.283443 0.822436 0.064 Uiso 1 1 calc R U . . .
C4 C 0.28843(18) 0.15949(15) 0.88392(15) 0.0559(4) Uani 1 1 d . . . . .
C5 C 0.10475(17) 0.21114(14) 0.91035(15) 0.0542(4) Uani 1 1 d . . . . .
H5A H 0.123463 0.265760 0.879006 0.065 Uiso 1 1 calc R U . . .
H5B H 0.094867 0.248794 0.973550 0.065 Uiso 1 1 calc R U . . .
C6 C -0.01909(19) 0.12476(15) 0.83657(15) 0.0576(4) Uani 1 1 d . . . . .
C7 C -0.10252(18) 0.27418(15) 0.79013(14) 0.0550(4) Uani 1 1 d . . . . .
H7A H -0.036079 0.326309 0.853510 0.066 Uiso 1 1 calc R U . . .
H7B H -0.180851 0.294798 0.783495 0.066 Uiso 1 1 calc R U . . .
C8 C -0.06811(17) 0.28000(15) 0.69746(14) 0.0563(4) Uani 1 1 d . . . . .
C9 C -0.01289(17) 0.48170(14) 0.77145(14) 0.0549(4) Uani 1 1 d . . . . .
H9A H -0.075261 0.475574 0.802778 0.066 Uiso 1 1 calc R U . . .
H9B H -0.017572 0.542343 0.744632 0.066 Uiso 1 1 calc R U . . .
C10 C 0.11986(16) 0.50707(13) 0.85405(13) 0.0467(4) Uani 1 1 d . . . . .
C11 C 0.29125(17) 0.62450(14) 1.00864(14) 0.0526(4) Uani 1 1 d . . . . .
H11A H 0.319106 0.700339 1.055429 0.063 Uiso 1 1 calc R U . . .
H11B H 0.350522 0.614951 0.974555 0.063 Uiso 1 1 calc R U . . .
C12 C 0.29217(16) 0.54654(13) 1.07028(12) 0.0471(4) Uani 1 1 d . . . . .
C13 C 0.5860(2) 0.53468(17) 0.81492(17) 0.0636(5) Uani 1 1 d . . . . .
H13A H 0.668968 0.585799 0.837865 0.076 Uiso 1 1 calc R U . . .
H13B H 0.564276 0.487679 0.744230 0.076 Uiso 1 1 calc R U . . .
C14 C 0.4929(2) 0.59708(18) 0.81732(18) 0.0696(5) Uani 1 1 d . . . . .
C15 C 0.4158(3) 0.6454(2) 0.8154(2) 0.0975(8) Uani 1 1 d . . . . .
H15 H 0.354651 0.683833 0.813907 0.117 Uiso 1 1 calc R U . . .
C16 C 0.3246(2) 0.09101(16) 0.66535(17) 0.0684(5) Uani 1 1 d . . . . .
H16A H 0.273604 0.033114 0.677898 0.082 Uiso 0.510(7) 1 calc R U P A 1
H16B H 0.404956 0.074810 0.671089 0.082 Uiso 0.510(7) 1 calc R U P A 1
H16C H 0.321738 0.032844 0.695476 0.082 Uiso 0.490(7) 1 calc R U P A 2
H16D H 0.393585 0.093387 0.640916 0.082 Uiso 0.490(7) 1 calc R U P A 2
C17A C 0.2552(7) 0.0902(8) 0.5538(6) 0.0775(17) Uani 0.510(7) 1 d . . P A 1
H17A H 0.312888 0.072550 0.519908 0.093 Uiso 0.510(7) 1 calc R U P A 1
H17B H 0.184080 0.024311 0.523908 0.093 Uiso 0.510(7) 1 calc R U P A 1
C17B C 0.2024(10) 0.0657(4) 0.5765(5) 0.0742(16) Uani 0.490(7) 1 d . . P A 2
H17C H 0.220518 0.030264 0.516848 0.089 Uiso 0.490(7) 1 calc R U P A 2
H17D H 0.146724 0.006864 0.584287 0.089 Uiso 0.490(7) 1 calc R U P A 2
C18A C 0.094(2) 0.1187(18) 0.4332(13) 0.128(5) Uani 0.510(7) 1 d . . P A 1
H18A H 0.026932 0.123353 0.458669 0.192 Uiso 0.510(7) 1 calc R U P A 1
H18B H 0.074585 0.045694 0.385051 0.192 Uiso 0.510(7) 1 calc R U P A 1
H18C H 0.100763 0.171930 0.398926 0.192 Uiso 0.510(7) 1 calc R U P A 1
C18B C 0.077(2) 0.1122(14) 0.4555(12) 0.116(5) Uani 0.490(7) 1 d . . P A 2
H18D H 0.002990 0.136691 0.456013 0.174 Uiso 0.490(7) 1 calc R U P A 2
H18E H 0.050860 0.038808 0.406319 0.174 Uiso 0.490(7) 1 calc R U P A 2
H18F H 0.128913 0.161480 0.436467 0.174 Uiso 0.490(7) 1 calc R U P A 2
C19A C 0.2222(3) 0.1041(2) 1.0109(2) 0.0961(9) Uani 1 1 d . . . . .
H19A H 0.141367 0.049404 0.986816 0.115 Uiso 0.586(11) 1 calc R U P B 1
H19B H 0.284375 0.063634 1.005872 0.115 Uiso 0.586(11) 1 calc R U P B 1
H19C H 0.190279 0.025502 0.971766 0.115 Uiso 0.414(11) 1 calc R U P B 2
H19D H 0.311869 0.118675 1.051044 0.115 Uiso 0.414(11) 1 calc R U P B 2
C20A C 0.2547(7) 0.1602(4) 1.1160(4) 0.0706(16) Uani 0.586(11) 1 d . . P B 1
H20A H 0.342935 0.203135 1.145226 0.085 Uiso 0.586(11) 1 calc R U P B 1
H20B H 0.248295 0.105678 1.149982 0.085 Uiso 0.586(11) 1 calc R U P B 1
C20B C 0.1645(11) 0.1258(5) 1.0775(6) 0.077(3) Uani 0.414(11) 1 d . . P B 2
H20C H 0.187855 0.083191 1.122871 0.092 Uiso 0.414(11) 1 calc R U P B 2
H20D H 0.074002 0.095147 1.037419 0.092 Uiso 0.414(11) 1 calc R U P B 2
C21 C 0.2027(3) 0.2640(3) 1.2438(2) 0.1123(10) Uani 1 1 d . . . . .
H21A H 0.286835 0.312635 1.282985 0.168 Uiso 1 1 calc R U . . .
H21B H 0.194231 0.200026 1.264701 0.168 Uiso 1 1 calc R U . . .
H21C H 0.141824 0.302014 1.255981 0.168 Uiso 1 1 calc R U . . .
C22 C -0.2410(2) 0.08255(19) 0.72858(18) 0.0762(6) Uani 1 1 d . . . . .
H22A H -0.282039 0.105951 0.671128 0.091 Uiso 1 1 calc R U . . .
H22B H -0.227301 0.011432 0.700461 0.091 Uiso 1 1 calc R U . . .
C23 C -0.3233(2) 0.07074(16) 0.78481(17) 0.0662(5) Uani 1 1 d . . . . .
C24 C -0.3911(3) 0.0624(2) 0.8290(2) 0.0936(8) Uani 1 1 d . . . . .
H24 H -0.445065 0.055810 0.864187 0.112 Uiso 1 1 calc R U . . .
C25 C -0.0159(2) 0.38807(18) 0.59668(16) 0.0708(6) Uani 1 1 d . . . . .
H25A H -0.042692 0.449623 0.579422 0.085 Uiso 1 1 calc R U . . .
H25B H -0.065897 0.321102 0.538307 0.085 Uiso 1 1 calc R U . . .
C26 C 0.1201(3) 0.4038(2) 0.61204(18) 0.0821(7) Uani 1 1 d . . . . .
H26A H 0.171572 0.471806 0.668650 0.099 Uiso 1 1 calc R U . . .
H26B H 0.148616 0.342613 0.628623 0.099 Uiso 1 1 calc R U . . .
C27 C 0.2568(4) 0.4221(4) 0.5251(3) 0.1475(16) Uani 1 1 d . . . . .
H27A H 0.288060 0.364465 0.545478 0.221 Uiso 1 1 calc R U . . .
H27B H 0.308902 0.492776 0.575357 0.221 Uiso 1 1 calc R U . . .
H27C H 0.259265 0.418269 0.458706 0.221 Uiso 1 1 calc R U . . .
C28 C 0.10187(19) 0.69198(14) 0.93971(14) 0.0559(4) Uani 1 1 d . . . . .
H28A H 0.114703 0.726140 1.011646 0.067 Uiso 1 1 calc R U . . .
H28B H 0.011389 0.659632 0.900656 0.067 Uiso 1 1 calc R U . . .
C29 C 0.1489(2) 0.77974(16) 0.90034(17) 0.0686(5) Uani 1 1 d . . . . .
H29A H 0.104955 0.836697 0.908539 0.082 Uiso 1 1 calc R U . . .
H29B H 0.239049 0.813880 0.939634 0.082 Uiso 1 1 calc R U . . .
C30 C 0.1536(4) 0.8093(3) 0.7483(3) 0.1229(11) Uani 1 1 d . . . . .
H30A H 0.136577 0.771630 0.676807 0.184 Uiso 1 1 calc R U . . .
H30B H 0.241439 0.850583 0.783189 0.184 Uiso 1 1 calc R U . . .
H30C H 0.101353 0.858940 0.752965 0.184 Uiso 1 1 calc R U . . .
O1W O 0.4486(7) 0.9283(6) 0.9391(6) 0.099(3) Uiso 0.278(6) 1 d D . P C -1
H1WA H 0.477(11) 0.958(9) 0.901(7) 0.148 Uiso 0.278(6) 1 d D U P C -1
H1WB H 0.493(14) 0.974(9) 1.000(4) 0.148 Uiso 0.278(6) 1 d D U P C -1


_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
O1 C2 1.226(2) . ?
O2 C4 1.225(2) . ?
O3 C6 1.216(2) . ?
O4 C8 1.217(2) . ?
O5 C10 1.2292(19) . ?
O6 C12 1.221(2) . ?
O7A C17A 0.980(8) . ?
O7A C18A 1.54(2) . ?
O7B C17B 1.041(8) . ?
O7B C18B 1.335(19) . ?
O8 C20A 1.410(5) . ?
O8 C20B 1.380(7) . ?
O8 C21 1.371(3) . ?
O9 C26 1.413(3) . ?
O9 C27 1.400(4) . ?
O10 C29 1.402(3) . ?
O10 C30 1.418(3) . ?
N1 C1 1.448(2) . ?
N1 C12 1.365(2) 2_667 ?
N1 C13 1.461(2) . ?
N2 C2 1.338(2) . ?
N2 C3 1.447(2) . ?
N2 C16 1.467(2) . ?
N3 C4 1.342(2) . ?
N3 C5 1.456(2) . ?
N3 C19A 1.474(3) . ?
N4 C6 1.354(3) . ?
N4 C7 1.447(2) . ?
N4 C22 1.471(3) . ?
N5 C8 1.347(2) . ?
N5 C9 1.446(2) . ?
N5 C25 1.463(3) . ?
N6 C10 1.338(2) . ?
N6 C11 1.450(2) . ?
N6 C28 1.462(2) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.531(2) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.528(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.519(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.533(3) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.532(2) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.518(2) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.457(3) . ?
C14 C15 1.172(3) . ?
C15 H15 0.9300 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 H16C 0.9700 . ?
C16 H16D 0.9700 . ?
C16 C17A 1.554(10) . ?
C16 C17B 1.490(9) . ?
C17A H17A 0.9700 . ?
C17A H17B 0.9700 . ?
C17B H17C 0.9700 . ?
C17B H17D 0.9700 . ?
C18A H18A 0.9600 . ?
C18A H18B 0.9600 . ?
C18A H18C 0.9600 . ?
C18B H18D 0.9600 . ?
C18B H18E 0.9600 . ?
C18B H18F 0.9600 . ?
C19A H19A 0.9700 . ?
C19A H19B 0.9700 . ?
C19A H19C 0.9700 . ?
C19A H19D 0.9700 . ?
C19A C20A 1.397(5) . ?
C19A C20B 1.337(7) . ?
C20A H20A 0.9700 . ?
C20A H20B 0.9700 . ?
C20B H20C 0.9700 . ?
C20B H20D 0.9700 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.451(3) . ?
C23 C24 1.168(3) . ?
C24 H24 0.9300 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.486(3) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C29 1.504(3) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
O1W H1WA 0.86(2) . ?
O1W H1WB 0.86(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
C17A O7A C18A 127.6(10) . . ?
C17B O7B C18B 133.6(9) . . ?
C21 O8 C20A 111.4(3) . . ?
C21 O8 C20B 126.0(3) . . ?
C27 O9 C26 112.1(2) . . ?
C29 O10 C30 112.8(2) . . ?
C1 N1 C13 116.42(14) . . ?
C12 N1 C1 122.20(14) 2_667 . ?
C12 N1 C13 116.93(14) 2_667 . ?
C2 N2 C3 122.83(14) . . ?
C2 N2 C16 119.94(15) . . ?
C3 N2 C16 117.09(15) . . ?
C4 N3 C5 121.66(15) . . ?
C4 N3 C19A 119.18(16) . . ?
C5 N3 C19A 118.61(17) . . ?
C6 N4 C7 123.32(15) . . ?
C6 N4 C22 117.65(17) . . ?
C7 N4 C22 116.74(17) . . ?
C8 N5 C9 122.20(15) . . ?
C8 N5 C25 118.57(16) . . ?
C9 N5 C25 117.73(16) . . ?
C10 N6 C11 116.62(13) . . ?
C10 N6 C28 124.58(14) . . ?
C11 N6 C28 118.68(14) . . ?
N1 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
N1 C1 C2 111.62(14) . . ?
H1A C1 H1B 108.0 . . ?
C2 C1 H1A 109.3 . . ?
C2 C1 H1B 109.3 . . ?
O1 C2 N2 123.11(16) . . ?
O1 C2 C1 119.55(16) . . ?
N2 C2 C1 117.34(15) . . ?
N2 C3 H3A 109.2 . . ?
N2 C3 H3B 109.2 . . ?
N2 C3 C4 112.24(14) . . ?
H3A C3 H3B 107.9 . . ?
C4 C3 H3A 109.2 . . ?
C4 C3 H3B 109.2 . . ?
O2 C4 N3 122.51(18) . . ?
O2 C4 C3 120.59(17) . . ?
N3 C4 C3 116.89(15) . . ?
N3 C5 H5A 109.1 . . ?
N3 C5 H5B 109.1 . . ?
N3 C5 C6 112.53(15) . . ?
H5A C5 H5B 107.8 . . ?
C6 C5 H5A 109.1 . . ?
C6 C5 H5B 109.1 . . ?
O3 C6 N4 122.04(19) . . ?
O3 C6 C5 121.52(18) . . ?
N4 C6 C5 116.23(15) . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
N4 C7 C8 110.79(15) . . ?
H7A C7 H7B 108.1 . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
O4 C8 N5 123.27(18) . . ?
O4 C8 C7 119.70(17) . . ?
N5 C8 C7 116.97(15) . . ?
N5 C9 H9A 109.3 . . ?
N5 C9 H9B 109.3 . . ?
N5 C9 C10 111.64(14) . . ?
H9A C9 H9B 108.0 . . ?
C10 C9 H9A 109.3 . . ?
C10 C9 H9B 109.3 . . ?
O5 C10 N6 121.14(15) . . ?
O5 C10 C9 120.50(15) . . ?
N6 C10 C9 118.35(14) . . ?
N6 C11 H11A 109.3 . . ?
N6 C11 H11B 109.3 . . ?
N6 C11 C12 111.52(14) . . ?
H11A C11 H11B 108.0 . . ?
C12 C11 H11A 109.3 . . ?
C12 C11 H11B 109.3 . . ?
O6 C12 N1 122.71(15) . 2_667 ?
O6 C12 C11 121.79(15) . . ?
N1 C12 C11 115.47(14) 2_667 . ?
N1 C13 H13A 109.2 . . ?
N1 C13 H13B 109.2 . . ?
H13A C13 H13B 107.9 . . ?
C14 C13 N1 112.17(17) . . ?
C14 C13 H13A 109.2 . . ?
C14 C13 H13B 109.2 . . ?
C15 C14 C13 177.6(3) . . ?
C14 C15 H15 180.0 . . ?
N2 C16 H16A 109.1 . . ?
N2 C16 H16B 109.1 . . ?
N2 C16 H16C 109.5 . . ?
N2 C16 H16D 109.5 . . ?
N2 C16 C17A 112.5(3) . . ?
N2 C16 C17B 110.8(3) . . ?
H16A C16 H16B 107.8 . . ?
H16C C16 H16D 108.1 . . ?
C17A C16 H16A 109.1 . . ?
C17A C16 H16B 109.1 . . ?
C17B C16 H16C 109.5 . . ?
C17B C16 H16D 109.5 . . ?
O7A C17A C16 134.9(5) . . ?
O7A C17A H17A 103.5 . . ?
O7A C17A H17B 103.5 . . ?
C16 C17A H17A 103.5 . . ?
C16 C17A H17B 103.5 . . ?
H17A C17A H17B 105.3 . . ?
O7B C17B C16 134.8(5) . . ?
O7B C17B H17C 103.5 . . ?
O7B C17B H17D 103.5 . . ?
C16 C17B H17C 103.5 . . ?
C16 C17B H17D 103.5 . . ?
H17C C17B H17D 105.3 . . ?
O7A C18A H18A 109.5 . . ?
O7A C18A H18B 109.5 . . ?
O7A C18A H18C 109.5 . . ?
H18A C18A H18B 109.5 . . ?
H18A C18A H18C 109.5 . . ?
H18B C18A H18C 109.5 . . ?
O7B C18B H18D 109.5 . . ?
O7B C18B H18E 109.5 . . ?
O7B C18B H18F 109.5 . . ?
H18D C18B H18E 109.5 . . ?
H18D C18B H18F 109.5 . . ?
H18E C18B H18F 109.5 . . ?
N3 C19A H19A 106.9 . . ?
N3 C19A H19B 106.9 . . ?
N3 C19A H19C 107.5 . . ?
N3 C19A H19D 107.5 . . ?
H19A C19A H19B 106.7 . . ?
H19C C19A H19D 107.0 . . ?
C20A C19A N3 121.6(3) . . ?
C20A C19A H19A 106.9 . . ?
C20A C19A H19B 106.9 . . ?
C20B C19A N3 119.1(3) . . ?
C20B C19A H19C 107.5 . . ?
C20B C19A H19D 107.5 . . ?
O8 C20A H20A 108.2 . . ?
O8 C20A H20B 108.2 . . ?
C19A C20A O8 116.2(4) . . ?
C19A C20A H20A 108.2 . . ?
C19A C20A H20B 108.2 . . ?
H20A C20A H20B 107.4 . . ?
O8 C20B H20C 106.7 . . ?
O8 C20B H20D 106.7 . . ?
C19A C20B O8 122.6(6) . . ?
C19A C20B H20C 106.7 . . ?
C19A C20B H20D 106.7 . . ?
H20C C20B H20D 106.6 . . ?
O8 C21 H21A 109.5 . . ?
O8 C21 H21B 109.5 . . ?
O8 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N4 C22 H22A 109.3 . . ?
N4 C22 H22B 109.3 . . ?
H22A C22 H22B 108.0 . . ?
C23 C22 N4 111.52(18) . . ?
C23 C22 H22A 109.3 . . ?
C23 C22 H22B 109.3 . . ?
C24 C23 C22 178.6(3) . . ?
C23 C24 H24 180.0 . . ?
N5 C25 H25A 108.8 . . ?
N5 C25 H25B 108.8 . . ?
N5 C25 C26 113.86(17) . . ?
H25A C25 H25B 107.7 . . ?
C26 C25 H25A 108.8 . . ?
C26 C25 H25B 108.8 . . ?
O9 C26 C25 107.7(2) . . ?
O9 C26 H26A 110.2 . . ?
O9 C26 H26B 110.2 . . ?
C25 C26 H26A 110.2 . . ?
C25 C26 H26B 110.2 . . ?
H26A C26 H26B 108.5 . . ?
O9 C27 H27A 109.5 . . ?
O9 C27 H27B 109.5 . . ?
O9 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N6 C28 H28A 109.0 . . ?
N6 C28 H28B 109.0 . . ?
N6 C28 C29 113.00(16) . . ?
H28A C28 H28B 107.8 . . ?
C29 C28 H28A 109.0 . . ?
C29 C28 H28B 109.0 . . ?
O10 C29 C28 108.85(16) . . ?
O10 C29 H29A 109.9 . . ?
O10 C29 H29B 109.9 . . ?
C28 C29 H29A 109.9 . . ?
C28 C29 H29B 109.9 . . ?
H29A C29 H29B 108.3 . . ?
O10 C30 H30A 109.5 . . ?
O10 C30 H30B 109.5 . . ?
O10 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
H1WA O1W H1WB 102(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 O1 -0.9(2) . . . . ?
N1 C1 C2 N2 178.78(15) . . . . ?
N2 C3 C4 O2 -0.6(3) . . . . ?
N2 C3 C4 N3 -179.76(15) . . . . ?
N2 C16 C17A O7A -3.5(16) . . . . ?
N2 C16 C17B O7B 17.6(14) . . . . ?
N3 C5 C6 O3 15.4(3) . . . . ?
N3 C5 C6 N4 -169.69(15) . . . . ?
N3 C19A C20A O8 52.2(7) . . . . ?
N3 C19A C20B O8 -52.8(11) . . . . ?
N4 C7 C8 O4 7.0(2) . . . . ?
N4 C7 C8 N5 -175.70(16) . . . . ?
N5 C9 C10 O5 -7.9(2) . . . . ?
N5 C9 C10 N6 173.28(15) . . . . ?
N5 C25 C26 O9 179.35(18) . . . . ?
N6 C11 C12 O6 -18.7(2) . . . . ?
N6 C11 C12 N1 159.53(14) . . . 2_667 ?
N6 C28 C29 O10 60.6(2) . . . . ?
C1 N1 C13 C14 57.8(2) . . . . ?
C2 N2 C3 C4 -93.3(2) . . . . ?
C2 N2 C16 C17A -86.2(5) . . . . ?
C2 N2 C16 C17B -120.5(4) . . . . ?
C3 N2 C2 O1 178.19(17) . . . . ?
C3 N2 C2 C1 -1.5(2) . . . . ?
C3 N2 C16 C17A 97.9(4) . . . . ?
C3 N2 C16 C17B 63.6(4) . . . . ?
C4 N3 C5 C6 94.7(2) . . . . ?
C4 N3 C19A C20A 118.0(4) . . . . ?
C4 N3 C19A C20B 166.4(6) . . . . ?
C5 N3 C4 O2 -179.96(18) . . . . ?
C5 N3 C4 C3 -0.8(3) . . . . ?
C5 N3 C19A C20A -70.3(5) . . . . ?
C5 N3 C19A C20B -22.0(7) . . . . ?
C6 N4 C7 C8 80.5(2) . . . . ?
C6 N4 C22 C23 98.1(2) . . . . ?
C7 N4 C6 O3 -163.97(18) . . . . ?
C7 N4 C6 C5 21.1(3) . . . . ?
C7 N4 C22 C23 -98.5(2) . . . . ?
C8 N5 C9 C10 72.3(2) . . . . ?
C8 N5 C25 C26 -87.9(2) . . . . ?
C9 N5 C8 O4 -165.41(19) . . . . ?
C9 N5 C8 C7 17.4(3) . . . . ?
C9 N5 C25 C26 78.4(2) . . . . ?
C10 N6 C11 C12 -66.5(2) . . . . ?
C10 N6 C28 C29 -96.9(2) . . . . ?
C11 N6 C10 O5 0.7(2) . . . . ?
C11 N6 C10 C9 179.46(15) . . . . ?
C11 N6 C28 C29 79.0(2) . . . . ?
C12 N1 C1 C2 -71.7(2) 2_667 . . . ?
C12 N1 C13 C14 -145.28(17) 2_667 . . . ?
C13 N1 C1 C2 83.87(18) . . . . ?
C16 N2 C2 O1 2.6(3) . . . . ?
C16 N2 C2 C1 -177.14(16) . . . . ?
C16 N2 C3 C4 82.5(2) . . . . ?
C18A O7A C17A C16 -138.3(11) . . . . ?
C18B O7B C17B C16 139.5(15) . . . . ?
C19A N3 C4 O2 -8.6(3) . . . . ?
C19A N3 C4 C3 170.5(2) . . . . ?
C19A N3 C5 C6 -76.7(2) . . . . ?
C21 O8 C20A C19A 167.2(4) . . . . ?
C21 O8 C20B C19A -134.9(6) . . . . ?
C22 N4 C6 O3 -1.7(3) . . . . ?
C22 N4 C6 C5 -176.68(17) . . . . ?
C22 N4 C7 C8 -81.9(2) . . . . ?
C25 N5 C8 O4 0.3(3) . . . . ?
C25 N5 C8 C7 -176.91(16) . . . . ?
C25 N5 C9 C10 -93.45(19) . . . . ?
C27 O9 C26 C25 -179.2(3) . . . . ?
C28 N6 C10 O5 176.64(16) . . . . ?
C28 N6 C10 C9 -4.5(2) . . . . ?
C28 N6 C11 C12 117.27(16) . . . . ?
C30 O10 C29 C28 172.9(2) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 65 electrons were 
found in a volume of 321Å³ in 1 void per unit cell. 
This is consistent with the presence of 
2[C3H8O] per Formula Unit 
which account for 68 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 -0.921 0.500 320.6 65.0 '2 C3H8O'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: isopropyl alcohol'
####################################################################### 
# 
# 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_res59_e5_cap3_sir_90_squeeze
_database_code_depnum_ccdc_archive 'CCDC 2117237'
loop_
_audit_author_name
_audit_author_address
'Giovanni Pierri'
;University of Salerno
Italy
;
_audit_update_record             
;
2022-03-16 deposited with the CCDC.	2022-03-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT230_res59_e5_cap3_sir_90_squeeze 
;
PROBLEM: Hirshfeld Test Diff for    C16      --C17      .       11.0 s.u.
RESPONSE: The atoms belong to a side chain
;
# Added during the CSD deposition process: Wednesday 16 March 2022 11:42 AM
# end Validation Reply Form

_audit_creation_date             2022-02-28
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H92 N12 O20, 2[C4H8O2]'
_chemical_formula_sum            'C68 H108 N12 O24'
_chemical_formula_weight         1477.66
_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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.7433(3)
_cell_length_b                   24.2497(7)
_cell_length_c                   13.9071(4)
_cell_angle_alpha                90
_cell_angle_beta                 100.5630(10)
_cell_angle_gamma                90
_cell_volume                     3893.23(19)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    296.00
_cell_measurement_theta_max      74.60
_cell_measurement_theta_min      3.71
_shelx_estimated_absorpt_T_max   0.932
_shelx_estimated_absorpt_T_min   0.756
_exptl_absorpt_coefficient_mu    0.799
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.5327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0959 before and 0.0665 after correction.
The Ratio of minimum to maximum transmission is 0.7067.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            45155
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.598
_diffrn_reflns_theta_min         3.711
_diffrn_ambient_temperature      296.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4919
_reflns_number_total             7289
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       0.0019(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         7289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0557
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0841P)²+0.7139P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1535
_refine_ls_wR_factor_ref         0.1688
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Others
 Sof(H14C)=Sof(H14D)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(O7B)=1-FVAR(1)
 Sof(O7A)=Sof(H14A)=Sof(H14B)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C9(H9A,H9B), C11(H11A,
 H11B), C13(H13A,H13B), C14(H14A,H14B), C14(H14C,H14D), C16(H16A,H16B),
 C17(H17A,H17B), C19(H19A,H19B), C22(H22A,H22B), C25(H25A,H25B), C26(H26A,H26B),
  C28(H28A,H28B), C29(H29A,H29B)
3.b Idealised Me refined as rotating group:
 C15(H15D,H15E,H15F), C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C27(H27A,H27B,
 H27C), C30(H30A,H30B,H30C)
3.c :
 C21(H21), C24(H24)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
O1 O -0.13141(15) 0.46170(7) 0.27679(13) 0.0772(5) Uani 1 1 d . . . . .
O2 O 0.04110(14) 0.33453(7) 0.16621(13) 0.0787(5) Uani 1 1 d . . . . .
O3 O 0.41955(19) 0.30115(8) 0.25641(16) 0.1009(6) Uani 1 1 d . . . . .
O4 O 0.45736(16) 0.44751(7) 0.38108(11) 0.0777(5) Uani 1 1 d . . . . .
O5 O 0.28899(13) 0.50852(6) 0.15069(10) 0.0604(4) Uani 1 1 d . . . . .
O6 O 0.32649(13) 0.47352(7) -0.05443(11) 0.0697(4) Uani 1 1 d . . . . .
O7A O 0.0486(3) 0.61003(11) 0.1470(5) 0.0947(15) Uani 0.845(15) 1 d . . P A 1
O8 O 0.19720(19) 0.44061(10) 0.46708(15) 0.1056(7) Uani 1 1 d . . . . .
O9 O 0.2877(2) 0.60591(11) 0.42804(16) 0.1181(8) Uani 1 1 d . . . . .
O10 O 0.41604(18) 0.67472(7) 0.13603(14) 0.0871(5) Uani 1 1 d . . . . .
N1 N -0.13426(15) 0.51995(7) 0.11298(13) 0.0591(5) Uani 1 1 d . . . . .
N2 N 0.04519(15) 0.42413(7) 0.28331(12) 0.0576(4) Uani 1 1 d . . . . .
N3 N 0.22410(16) 0.34297(8) 0.14249(15) 0.0648(5) Uani 1 1 d . . . . .
N4 N 0.52555(16) 0.37824(8) 0.25197(13) 0.0620(5) Uani 1 1 d . . . . .
N5 N 0.47288(15) 0.52528(7) 0.29557(12) 0.0572(4) Uani 1 1 d . . . . .
N6 N 0.34171(15) 0.56953(7) 0.04625(12) 0.0536(4) Uani 1 1 d . . . . .
C1 C -0.03454(18) 0.48472(9) 0.14569(15) 0.0569(5) Uani 1 1 d . . . . .
H1A H 0.035463 0.506836 0.155699 0.068 Uiso 1 1 calc R U . . .
H1B H -0.028769 0.457549 0.095617 0.068 Uiso 1 1 calc R U . . .
C2 C -0.04485(19) 0.45536(9) 0.24093(16) 0.0564(5) Uani 1 1 d . . . . .
C3 C 0.14574(17) 0.41308(9) 0.23965(15) 0.0554(5) Uani 1 1 d . . . . .
H3A H 0.213622 0.410087 0.290933 0.067 Uiso 1 1 calc R U . . .
H3B H 0.157784 0.443739 0.197858 0.067 Uiso 1 1 calc R U . . .
C4 C 0.13230(18) 0.36023(9) 0.17966(15) 0.0554(5) Uani 1 1 d . . . . .
C5 C 0.33180(18) 0.37397(9) 0.15364(16) 0.0596(5) Uani 1 1 d . . . . .
H5A H 0.318476 0.411133 0.174905 0.072 Uiso 1 1 calc R U . . .
H5B H 0.355755 0.376511 0.090639 0.072 Uiso 1 1 calc R U . . .
C6 C 0.4285(2) 0.34780(10) 0.22679(17) 0.0644(6) Uani 1 1 d . . . . .
C7 C 0.53017(18) 0.43658(9) 0.23282(15) 0.0572(5) Uani 1 1 d . . . . .
H7A H 0.485793 0.444411 0.168316 0.069 Uiso 1 1 calc R U . . .
H7B H 0.609851 0.447316 0.233349 0.069 Uiso 1 1 calc R U . . .
C8 C 0.48160(18) 0.47056(9) 0.30934(14) 0.0546(5) Uani 1 1 d . . . . .
C9 C 0.47501(19) 0.55065(9) 0.20113(15) 0.0573(5) Uani 1 1 d . . . . .
H9A H 0.537984 0.535048 0.173567 0.069 Uiso 1 1 calc R U . . .
H9B H 0.488944 0.589918 0.209885 0.069 Uiso 1 1 calc R U . . .
C10 C 0.36065(18) 0.54145(8) 0.13039(14) 0.0506(5) Uani 1 1 d . . . . .
C11 C 0.23402(19) 0.55734(9) -0.02075(15) 0.0548(5) Uani 1 1 d . . . . .
H11A H 0.221771 0.584574 -0.072701 0.066 Uiso 1 1 calc R U . . .
H11B H 0.169833 0.559750 0.014124 0.066 Uiso 1 1 calc R U . . .
C12 C 0.23637(18) 0.50017(9) -0.06499(14) 0.0527(5) Uani 1 1 d . . . . .
C13 C -0.1347(2) 0.57304(10) 0.16287(19) 0.0704(6) Uani 1 1 d . . . . .
H13A H -0.101490 0.567962 0.231469 0.085 Uiso 1 1 calc R U . . .
H13B H -0.214378 0.584772 0.158992 0.085 Uiso 1 1 calc R U . . .
C14 C -0.0703(3) 0.61753(12) 0.1231(3) 0.0932(9) Uani 1 1 d . . . . .
H14A H -0.093456 0.618545 0.052504 0.112 Uiso 0.845(15) 1 calc R U P A 1
H14B H -0.090343 0.652716 0.148708 0.112 Uiso 0.845(15) 1 calc R U P A 1
H14C H -0.128969 0.640515 0.084253 0.112 Uiso 0.155(15) 1 calc R U P A 2
H14D H -0.036114 0.639648 0.179119 0.112 Uiso 0.155(15) 1 calc R U P A 2
C15 C 0.1073(4) 0.65671(14) 0.1180(4) 0.1352(15) Uani 1 1 d . . . . .
H15D H 0.136425 0.671491 0.063157 0.203 Uiso 0.155(15) 1 calc R U P A 2
H15E H 0.168486 0.637769 0.160538 0.203 Uiso 0.155(15) 1 calc R U P A 2
H15F H 0.078874 0.686202 0.153074 0.203 Uiso 0.155(15) 1 calc R U P A 2
H15A H 0.080720 0.663589 0.049544 0.203 Uiso 0.845(15) 1 calc R U P A 1
H15B H 0.189162 0.649714 0.129719 0.203 Uiso 0.845(15) 1 calc R U P A 1
H15C H 0.091707 0.688330 0.154987 0.203 Uiso 0.845(15) 1 calc R U P A 1
C16 C 0.0388(2) 0.39627(11) 0.37537(17) 0.0713(6) Uani 1 1 d . . . . .
H16A H 0.083306 0.362397 0.379147 0.086 Uiso 1 1 calc R U . . .
H16B H -0.041189 0.386473 0.375886 0.086 Uiso 1 1 calc R U . . .
C17 C 0.0834(3) 0.43084(13) 0.4636(2) 0.0880(8) Uani 1 1 d . . . . .
H17A H 0.041421 0.465440 0.459760 0.106 Uiso 1 1 calc R U . . .
H17B H 0.072219 0.411676 0.522364 0.106 Uiso 1 1 calc R U . . .
C18 C 0.2504(3) 0.47224(18) 0.5519(2) 0.1257(13) Uani 1 1 d . . . . .
H18A H 0.329764 0.479728 0.548132 0.189 Uiso 1 1 calc R U . . .
H18B H 0.247287 0.451551 0.610235 0.189 Uiso 1 1 calc R U . . .
H18C H 0.209517 0.506398 0.553618 0.189 Uiso 1 1 calc R U . . .
C19 C 0.2184(3) 0.28926(11) 0.0934(2) 0.0881(8) Uani 1 1 d . . . . .
H19A H 0.261260 0.262467 0.137722 0.106 Uiso 1 1 calc R U . . .
H19B H 0.138314 0.277283 0.078453 0.106 Uiso 1 1 calc R U . . .
C20 C 0.2652(3) 0.29050(13) 0.0035(2) 0.0906(9) Uani 1 1 d . . . . .
C21 C 0.3038(3) 0.29012(18) -0.0672(3) 0.1282(14) Uani 1 1 d . . . . .
H21 H 0.334767 0.289821 -0.124113 0.154 Uiso 1 1 calc R U . . .
C22 C 0.6226(2) 0.35477(12) 0.3214(2) 0.0810(7) Uani 1 1 d . . . . .
H22A H 0.596244 0.322458 0.352164 0.097 Uiso 1 1 calc R U . . .
H22B H 0.649704 0.381573 0.372254 0.097 Uiso 1 1 calc R U . . .
C23 C 0.7187(2) 0.33926(10) 0.2725(2) 0.0731(7) Uani 1 1 d . . . . .
C24 C 0.7960(3) 0.32763(13) 0.2336(2) 0.0920(9) Uani 1 1 d . . . . .
H24 H 0.857262 0.318416 0.202739 0.110 Uiso 1 1 calc R U . . .
C25 C 0.4349(2) 0.56004(10) 0.36992(17) 0.0710(7) Uani 1 1 d . . . . .
H25A H 0.473509 0.595463 0.371344 0.085 Uiso 1 1 calc R U . . .
H25B H 0.458840 0.542939 0.433467 0.085 Uiso 1 1 calc R U . . .
C26 C 0.3069(3) 0.56937(13) 0.3532(2) 0.0890(8) Uani 1 1 d . . . . .
H26A H 0.280086 0.585577 0.289248 0.107 Uiso 1 1 calc R U . . .
H26B H 0.266196 0.534867 0.357125 0.107 Uiso 1 1 calc R U . . .
C27 C 0.1784(4) 0.6242(2) 0.4189(3) 0.1582(19) Uani 1 1 d . . . . .
H27A H 0.173439 0.650101 0.470132 0.237 Uiso 1 1 calc R U . . .
H27B H 0.127697 0.593639 0.423400 0.237 Uiso 1 1 calc R U . . .
H27C H 0.155975 0.641906 0.356557 0.237 Uiso 1 1 calc R U . . .
C28 C 0.4230(2) 0.60789(9) 0.01522(16) 0.0620(6) Uani 1 1 d . . . . .
H28A H 0.420909 0.603259 -0.054365 0.074 Uiso 1 1 calc R U . . .
H28B H 0.500688 0.598885 0.048803 0.074 Uiso 1 1 calc R U . . .
C29 C 0.3984(2) 0.66685(10) 0.03498(18) 0.0727(7) Uani 1 1 d . . . . .
H29A H 0.449378 0.690779 0.006397 0.087 Uiso 1 1 calc R U . . .
H29B H 0.318965 0.675798 0.006021 0.087 Uiso 1 1 calc R U . . .
C30 C 0.3996(4) 0.72982(13) 0.1641(3) 0.1224(13) Uani 1 1 d . . . . .
H30A H 0.407712 0.731816 0.233942 0.184 Uiso 1 1 calc R U . . .
H30B H 0.323509 0.741952 0.134254 0.184 Uiso 1 1 calc R U . . .
H30C H 0.456521 0.753085 0.143061 0.184 Uiso 1 1 calc R U . . .
O7B O 0.000(2) 0.6126(7) 0.078(3) 0.093(11) Uani 0.155(15) 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
O1 C2 1.221(2) . ?
O2 C4 1.224(2) . ?
O3 C6 1.215(3) . ?
O4 C8 1.222(2) . ?
O5 C10 1.230(2) . ?
O6 C12 1.226(2) . ?
O7A C14 1.387(5) . ?
O7A C15 1.422(4) . ?
O8 C17 1.349(3) . ?
O8 C18 1.450(4) . ?
O9 C26 1.416(3) . ?
O9 C27 1.342(4) . ?
O10 C29 1.396(3) . ?
O10 C30 1.415(3) . ?
N1 C1 1.453(3) . ?
N1 C12 1.352(3) 3_565 ?
N1 C13 1.463(3) . ?
N2 C2 1.345(3) . ?
N2 C3 1.448(3) . ?
N2 C16 1.462(3) . ?
N3 C4 1.345(3) . ?
N3 C5 1.455(3) . ?
N3 C19 1.466(3) . ?
N4 C6 1.349(3) . ?
N4 C7 1.442(3) . ?
N4 C22 1.467(3) . ?
N5 C8 1.342(3) . ?
N5 C9 1.455(3) . ?
N5 C25 1.466(3) . ?
N6 C10 1.337(3) . ?
N6 C11 1.457(3) . ?
N6 C28 1.454(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.528(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.522(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.518(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.536(3) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.529(3) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.519(3) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.481(4) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C14 H14D 0.9700 . ?
C14 O7B 1.128(13) . ?
C15 H15D 0.9600 . ?
C15 H15E 0.9600 . ?
C15 H15F 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C15 O7B 1.67(2) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.499(4) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.456(4) . ?
C20 C21 1.155(5) . ?
C21 H21 0.9300 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.469(4) . ?
C23 C24 1.173(4) . ?
C24 H24 0.9300 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.496(4) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C29 1.494(3) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?

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
C14 O7A C15 110.3(4) . . ?
C17 O8 C18 113.5(2) . . ?
C27 O9 C26 114.5(3) . . ?
C29 O10 C30 113.8(2) . . ?
C1 N1 C13 116.20(18) . . ?
C12 N1 C1 122.22(18) 3_565 . ?
C12 N1 C13 118.14(17) 3_565 . ?
C2 N2 C3 123.79(18) . . ?
C2 N2 C16 118.77(18) . . ?
C3 N2 C16 117.29(18) . . ?
C4 N3 C5 122.72(18) . . ?
C4 N3 C19 118.95(19) . . ?
C5 N3 C19 118.24(18) . . ?
C6 N4 C7 123.18(18) . . ?
C6 N4 C22 118.4(2) . . ?
C7 N4 C22 116.8(2) . . ?
C8 N5 C9 122.25(17) . . ?
C8 N5 C25 119.55(18) . . ?
C9 N5 C25 116.85(18) . . ?
C10 N6 C11 116.23(17) . . ?
C10 N6 C28 124.94(18) . . ?
C28 N6 C11 118.71(16) . . ?
N1 C1 H1A 109.4 . . ?
N1 C1 H1B 109.4 . . ?
N1 C1 C2 110.97(17) . . ?
H1A C1 H1B 108.0 . . ?
C2 C1 H1A 109.4 . . ?
C2 C1 H1B 109.4 . . ?
O1 C2 N2 122.5(2) . . ?
O1 C2 C1 120.0(2) . . ?
N2 C2 C1 117.47(18) . . ?
N2 C3 H3A 109.2 . . ?
N2 C3 H3B 109.2 . . ?
N2 C3 C4 112.04(17) . . ?
H3A C3 H3B 107.9 . . ?
C4 C3 H3A 109.2 . . ?
C4 C3 H3B 109.2 . . ?
O2 C4 N3 121.6(2) . . ?
O2 C4 C3 120.84(19) . . ?
N3 C4 C3 117.58(18) . . ?
N3 C5 H5A 109.1 . . ?
N3 C5 H5B 109.1 . . ?
N3 C5 C6 112.59(19) . . ?
H5A C5 H5B 107.8 . . ?
C6 C5 H5A 109.1 . . ?
C6 C5 H5B 109.1 . . ?
O3 C6 N4 122.9(2) . . ?
O3 C6 C5 121.1(2) . . ?
N4 C6 C5 116.0(2) . . ?
N4 C7 H7A 109.3 . . ?
N4 C7 H7B 109.3 . . ?
N4 C7 C8 111.52(18) . . ?
H7A C7 H7B 108.0 . . ?
C8 C7 H7A 109.3 . . ?
C8 C7 H7B 109.3 . . ?
O4 C8 N5 123.08(19) . . ?
O4 C8 C7 119.5(2) . . ?
N5 C8 C7 117.38(18) . . ?
N5 C9 H9A 109.4 . . ?
N5 C9 H9B 109.4 . . ?
N5 C9 C10 111.15(17) . . ?
H9A C9 H9B 108.0 . . ?
C10 C9 H9A 109.4 . . ?
C10 C9 H9B 109.4 . . ?
O5 C10 N6 121.38(18) . . ?
O5 C10 C9 120.29(18) . . ?
N6 C10 C9 118.32(18) . . ?
N6 C11 H11A 109.3 . . ?
N6 C11 H11B 109.3 . . ?
N6 C11 C12 111.48(17) . . ?
H11A C11 H11B 108.0 . . ?
C12 C11 H11A 109.3 . . ?
C12 C11 H11B 109.3 . . ?
O6 C12 N1 122.49(19) . 3_565 ?
O6 C12 C11 120.80(19) . . ?
N1 C12 C11 116.67(17) 3_565 . ?
N1 C13 H13A 108.6 . . ?
N1 C13 H13B 108.6 . . ?
N1 C13 C14 114.7(2) . . ?
H13A C13 H13B 107.6 . . ?
C14 C13 H13A 108.6 . . ?
C14 C13 H13B 108.6 . . ?
O7A C14 C13 112.1(3) . . ?
O7A C14 H14A 109.2 . . ?
O7A C14 H14B 109.2 . . ?
C13 C14 H14A 109.2 . . ?
C13 C14 H14B 109.2 . . ?
C13 C14 H14C 105.5 . . ?
C13 C14 H14D 105.5 . . ?
H14A C14 H14B 107.9 . . ?
H14C C14 H14D 106.1 . . ?
O7B C14 C13 127.2(8) . . ?
O7B C14 H14C 105.5 . . ?
O7B C14 H14D 105.5 . . ?
O7A C15 H15A 109.5 . . ?
O7A C15 H15B 109.5 . . ?
O7A C15 H15C 109.5 . . ?
H15D C15 H15E 109.5 . . ?
H15D C15 H15F 109.5 . . ?
H15E C15 H15F 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O7B C15 H15D 109.5 . . ?
O7B C15 H15E 109.5 . . ?
O7B C15 H15F 109.5 . . ?
N2 C16 H16A 109.0 . . ?
N2 C16 H16B 109.0 . . ?
N2 C16 C17 113.1(2) . . ?
H16A C16 H16B 107.8 . . ?
C17 C16 H16A 109.0 . . ?
C17 C16 H16B 109.0 . . ?
O8 C17 C16 108.9(2) . . ?
O8 C17 H17A 109.9 . . ?
O8 C17 H17B 109.9 . . ?
C16 C17 H17A 109.9 . . ?
C16 C17 H17B 109.9 . . ?
H17A C17 H17B 108.3 . . ?
O8 C18 H18A 109.5 . . ?
O8 C18 H18B 109.5 . . ?
O8 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 H19A 109.0 . . ?
N3 C19 H19B 109.0 . . ?
H19A C19 H19B 107.8 . . ?
C20 C19 N3 112.9(2) . . ?
C20 C19 H19A 109.0 . . ?
C20 C19 H19B 109.0 . . ?
C21 C20 C19 178.2(4) . . ?
C20 C21 H21 180.0 . . ?
N4 C22 H22A 109.4 . . ?
N4 C22 H22B 109.4 . . ?
N4 C22 C23 111.4(2) . . ?
H22A C22 H22B 108.0 . . ?
C23 C22 H22A 109.4 . . ?
C23 C22 H22B 109.4 . . ?
C24 C23 C22 179.1(3) . . ?
C23 C24 H24 180.0 . . ?
N5 C25 H25A 108.8 . . ?
N5 C25 H25B 108.8 . . ?
N5 C25 C26 113.9(2) . . ?
H25A C25 H25B 107.7 . . ?
C26 C25 H25A 108.8 . . ?
C26 C25 H25B 108.8 . . ?
O9 C26 C25 105.7(2) . . ?
O9 C26 H26A 110.6 . . ?
O9 C26 H26B 110.6 . . ?
C25 C26 H26A 110.6 . . ?
C25 C26 H26B 110.6 . . ?
H26A C26 H26B 108.7 . . ?
O9 C27 H27A 109.5 . . ?
O9 C27 H27B 109.5 . . ?
O9 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N6 C28 H28A 108.9 . . ?
N6 C28 H28B 108.9 . . ?
N6 C28 C29 113.41(18) . . ?
H28A C28 H28B 107.7 . . ?
C29 C28 H28A 108.9 . . ?
C29 C28 H28B 108.9 . . ?
O10 C29 C28 108.54(19) . . ?
O10 C29 H29A 110.0 . . ?
O10 C29 H29B 110.0 . . ?
C28 C29 H29A 110.0 . . ?
C28 C29 H29B 110.0 . . ?
H29A C29 H29B 108.4 . . ?
O10 C30 H30A 109.5 . . ?
O10 C30 H30B 109.5 . . ?
O10 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C14 O7B C15 109.4(18) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 O1 2.7(3) . . . . ?
N1 C1 C2 N2 -175.67(18) . . . . ?
N1 C13 C14 O7A -72.8(4) . . . . ?
N1 C13 C14 O7B -21(3) . . . . ?
N2 C3 C4 O2 5.5(3) . . . . ?
N2 C3 C4 N3 -174.30(19) . . . . ?
N2 C16 C17 O8 -63.7(3) . . . . ?
N3 C5 C6 O3 12.9(3) . . . . ?
N3 C5 C6 N4 -170.49(18) . . . . ?
N4 C7 C8 O4 7.9(3) . . . . ?
N4 C7 C8 N5 -175.06(18) . . . . ?
N5 C9 C10 O5 -11.3(3) . . . . ?
N5 C9 C10 N6 169.38(17) . . . . ?
N5 C25 C26 O9 -176.7(2) . . . . ?
N6 C11 C12 O6 -10.4(3) . . . . ?
N6 C11 C12 N1 167.51(17) . . . 3_565 ?
N6 C28 C29 O10 66.1(3) . . . . ?
C1 N1 C13 C14 84.6(3) . . . . ?
C2 N2 C3 C4 -92.3(2) . . . . ?
C2 N2 C16 C17 -88.9(3) . . . . ?
C3 N2 C2 O1 176.0(2) . . . . ?
C3 N2 C2 C1 -5.6(3) . . . . ?
C3 N2 C16 C17 95.4(3) . . . . ?
C4 N3 C5 C6 106.4(2) . . . . ?
C4 N3 C19 C20 137.1(2) . . . . ?
C5 N3 C4 O2 177.2(2) . . . . ?
C5 N3 C4 C3 -3.0(3) . . . . ?
C5 N3 C19 C20 -46.3(3) . . . . ?
C6 N4 C7 C8 80.3(2) . . . . ?
C6 N4 C22 C23 107.8(3) . . . . ?
C7 N4 C6 O3 -167.9(2) . . . . ?
C7 N4 C6 C5 15.6(3) . . . . ?
C7 N4 C22 C23 -86.1(3) . . . . ?
C8 N5 C9 C10 74.6(2) . . . . ?
C8 N5 C25 C26 -91.5(3) . . . . ?
C9 N5 C8 O4 -165.0(2) . . . . ?
C9 N5 C8 C7 18.0(3) . . . . ?
C9 N5 C25 C26 75.5(3) . . . . ?
C10 N6 C11 C12 -70.1(2) . . . . ?
C10 N6 C28 C29 -98.1(2) . . . . ?
C11 N6 C10 O5 -2.2(3) . . . . ?
C11 N6 C10 C9 177.10(17) . . . . ?
C11 N6 C28 C29 86.2(2) . . . . ?
C12 N1 C1 C2 -80.2(2) 3_565 . . . ?
C12 N1 C13 C14 -115.8(3) 3_565 . . . ?
C13 N1 C1 C2 78.5(2) . . . . ?
C13 C14 O7B C15 -136.8(7) . . . . ?
C15 O7A C14 C13 -173.0(4) . . . . ?
C16 N2 C2 O1 0.6(3) . . . . ?
C16 N2 C2 C1 178.97(19) . . . . ?
C16 N2 C3 C4 83.2(2) . . . . ?
C18 O8 C17 C16 -177.9(3) . . . . ?
C19 N3 C4 O2 -6.4(4) . . . . ?
C19 N3 C4 C3 173.5(2) . . . . ?
C19 N3 C5 C6 -70.1(3) . . . . ?
C22 N4 C6 O3 -2.7(3) . . . . ?
C22 N4 C6 C5 -179.19(19) . . . . ?
C22 N4 C7 C8 -85.1(2) . . . . ?
C25 N5 C8 O4 1.3(3) . . . . ?
C25 N5 C8 C7 -175.68(19) . . . . ?
C25 N5 C9 C10 -92.1(2) . . . . ?
C27 O9 C26 C25 172.9(3) . . . . ?
C28 N6 C10 O5 -178.04(19) . . . . ?
C28 N6 C10 C9 1.2(3) . . . . ?
C28 N6 C11 C12 106.1(2) . . . . ?
C30 O10 C29 C28 177.7(2) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 188 electrons were 
found in a volume of 700Å³ in 1 void per unit cell. 
This is consistent with the presence of 
2[C4H8O2] per Formula Unit 
which account for 192 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.228 0.194 0.086 175.0 46.9 '1 C4H8O2'
2 0.272 0.306 0.586 175.0 46.9 '1 C4H8O2'
3 -0.272 0.694 0.414 175.0 46.9 '1 C4H8O2'
4 0.228 0.806 -0.086 175.0 46.9 '1 C4H8O2'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: ethyl acetate/toluene'
