# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# 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. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 2127390'
loop_
_audit_author_name
_audit_author_address
'Qipu Lin'
;Fujian Institute of Research on the Structure of Matter,  Chinese Academy of Sciences
China
;
_audit_update_record             
;
2022-05-14 deposited with the CCDC.	2022-05-22 downloaded from the CCDC.
;
_audit_creation_date             2022-05-14
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        TCPP-HOF2
_chemical_formula_moiety         'C96 H57 N8 O16, 2(H4 N), 2(C2 H3 N)'
_chemical_formula_sum            'C100 H99 N12 O30'
_chemical_formula_weight         1948.91
_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 0.0137 0.0067 '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 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0389 0.0241 '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                   22.6949(7)
_cell_length_b                   9.6108(3)
_cell_length_c                   23.3758(8)
_cell_angle_alpha                90
_cell_angle_beta                 97.186(3)
_cell_angle_gamma                90
_cell_volume                     5058.6(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    17113
_cell_measurement_temperature    293
_cell_measurement_theta_max      60.0060
_cell_measurement_theta_min      2.2310
_shelx_estimated_absorpt_T_max   0.990
_shelx_estimated_absorpt_T_min   0.975
_exptl_absorpt_coefficient_mu    0.402
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark violet'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1766
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            38175
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        52.932
_diffrn_reflns_theta_max         52.932
_diffrn_reflns_theta_min         2.224
_diffrn_ambient_temperature      293.00
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     24.00  49.00   0.50    2.10    --   72.28-125.00  90.00   50
  2  ω     63.00 111.00   0.50    2.10    --   72.28-125.00  90.00   96
  3  ω     -2.00  73.00   0.50    2.10    --   72.28 -18.00  88.00  150
  4  ω     -1.00  31.00   0.50    2.10    --   72.28 -57.00 -30.00   64
  5  ω     37.00  89.00   0.50    2.10    --   72.28 -57.00 -30.00  104
  6  ω     56.00 133.00   0.50    2.10    --   72.28  18.00-102.00  154
  7  ω     97.00 122.00   0.50    2.10    --   72.28 125.00  30.00   50
  8  ω      4.00  29.00   0.50    0.52    --   -1.25  18.00-102.00   50
  9  ω    -17.00  71.00   0.50    0.52    --   -1.25  57.00-120.00  176
 10  ω    -72.00 -28.00   0.50    2.10    --  -74.78  18.00-102.00   88
 11  ω    -88.00 -19.00   0.50    2.10    --  -74.78  57.00 -30.00  138
 12  ω    -97.00 -22.00   0.50    2.10    --  -74.78  77.00   0.00  150
 13  ω   -150.00 -59.00   0.50    2.10    --  -74.78 -18.00  88.00  182
 14  ω    -71.00   4.00   0.50    0.52    --   -1.25 -18.00  88.00  150
 15  ω   -143.00-117.00   0.50    2.10    --  -74.78 -99.00-120.00   52
 16  ω   -148.00-104.00   0.50    2.10    --  -74.78-125.00-150.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7106
_reflns_number_total             8942
_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       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         8916
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0477
_refine_ls_restrained_S_all      1.222
_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)+(0.0746P)²+1.1127P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1323
_refine_ls_wR_factor_ref         0.1402
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All N(H,H) groups, All O(H) groups
2. Restrained distances
 H1AA-H1AB \\sim H1AA-H1AC \\sim H1AA-H1AD \\sim H1AB-H1AC \\sim H1AB-H1AD
\\sim H1AC-H1AD
 with sigma of 0.002
 N1A-H1AA \\sim N1A-H1AB \\sim N1A-H1AC \\sim N1A-H1AD
 with sigma of 0.001
3. Others
 Fixed Sof: H3(0.5) H2(0.5) H4(0.5) H1(0.5)
4.a Free rotating group:
 N1A(H1AA,H1AB)
4.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N2(H2), N4(H4), N1(H1), C41(H41), C42(H42), C25(H25), C18(H18),
 C19(H19), C24(H24), C21(H21), C22(H22), C13(H13), C15(H15), C6(H6), C27(H27),
 C33(H33), C16(H16), C7(H7), C01H(H01H), C34(H34), C12(H12), C9(H9), C46(H46),
 C45(H45), C38(H38), C10(H10), C37(H37)
4.c Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C)
4.d Idealised tetrahedral OH refined as rotating group:
 O8(H8), O3(H3A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O5 O 0.94845(5) 0.95870(14) 0.49776(6) 0.0498(4) Uani 1 1 d . . . . .
O1 O 0.10415(5) 0.49933(16) 0.46723(6) 0.0549(4) Uani 1 1 d . . . . .
O6 O 0.94130(6) 1.11336(16) 0.56609(6) 0.0577(4) Uani 1 1 d . . . . .
N3 N 0.60614(6) 0.68488(15) 0.58354(6) 0.0330(3) Uani 1 1 d . . . . .
H3 H 0.576157 0.696004 0.557572 0.040 Uiso 0.5 1 calc R U P A 1
N2 N 0.58460(6) 0.84027(16) 0.47503(6) 0.0366(3) Uani 1 1 d . . . . .
H2 H 0.562780 0.790957 0.494758 0.044 Uiso 0.5 1 calc R U P B 2
N4 N 0.48121(6) 0.61798(16) 0.57447(6) 0.0381(4) Uani 1 1 d . . . . .
H4 H 0.502612 0.672794 0.556570 0.046 Uiso 0.5 1 calc R U P C 2
O8 O 0.43132(7) 1.23466(17) 0.15657(6) 0.0613(4) Uani 1 1 d . . . . .
H8 H 0.435032 1.278626 0.127169 0.092 Uiso 1 1 calc R U . . .
O3 O 0.61853(6) 0.13244(17) 0.87240(7) 0.0602(4) Uani 1 1 d . . . . .
H3A H 0.615013 0.089076 0.901992 0.090 Uiso 1 1 calc R U . . .
N1 N 0.45958(6) 0.78315(16) 0.46844(6) 0.0369(3) Uani 1 1 d . . . . .
H1 H 0.490879 0.760250 0.491099 0.044 Uiso 0.5 1 calc R U P D 1
O4 O 0.53846(7) 0.24050(17) 0.89520(6) 0.0618(4) Uani 1 1 d . . . . .
O7 O 0.51006(7) 1.12210(19) 0.13302(7) 0.0714(5) Uani 1 1 d . . . . .
N1A N 0.98540(7) 0.66798(17) 0.48919(8) 0.0481(4) Uani 1 1 d DG . . . .
H1AA H 0.960197 0.615302 0.502340 0.072 Uiso 1 1 d DG U . . .
H1AB H 0.972831 0.749903 0.494077 0.072 Uiso 1 1 d DG U . . .
O2 O 0.10361(6) 0.6245(2) 0.54464(7) 0.0795(6) Uani 1 1 d . . . . .
C43 C 0.60728(7) 0.60856(18) 0.63317(7) 0.0323(4) Uani 1 1 d . . . . .
C26 C 0.49878(7) 0.97464(19) 0.33750(8) 0.0364(4) Uani 1 1 d . . . . .
C20 C 0.74373(7) 0.86418(19) 0.54255(8) 0.0358(4) Uani 1 1 d . . . . .
C14 C 0.56735(7) 0.45756(19) 0.70607(8) 0.0358(4) Uani 1 1 d . . . . .
C31 C 0.55887(7) 0.53618(18) 0.65061(7) 0.0347(4) Uani 1 1 d . . . . .
C35 C 0.45777(7) 0.85946(19) 0.41923(7) 0.0362(4) Uani 1 1 d . . . . .
C40 C 0.66190(7) 0.74032(18) 0.58302(7) 0.0332(4) Uani 1 1 d . . . . .
C3 C 0.92012(7) 1.01796(19) 0.53582(8) 0.0381(4) Uani 1 1 d . . . . .
C32 C 0.40217(7) 0.74967(19) 0.47509(8) 0.0361(4) Uani 1 1 d . . . . .
C29 C 0.50772(7) 0.91149(19) 0.39624(7) 0.0365(4) Uani 1 1 d . . . . .
C41 C 0.69885(7) 0.6976(2) 0.63424(8) 0.0387(4) Uani 1 1 d . . . . .
H41 H 0.738653 0.720196 0.644231 0.046 Uiso 1 1 calc R U . . .
C39 C 0.64407(7) 0.86635(19) 0.48948(8) 0.0370(4) Uani 1 1 d . . . . .
C17 C 0.85930(7) 0.96126(18) 0.53913(8) 0.0355(4) Uani 1 1 d . . . . .
C44 C 0.50116(7) 0.53725(19) 0.62110(8) 0.0377(4) Uani 1 1 d . . . . .
C30 C 0.67988(7) 0.82105(19) 0.53870(8) 0.0350(4) Uani 1 1 d . . . . .
C47 C 0.42142(7) 0.5968(2) 0.56112(8) 0.0391(4) Uani 1 1 d . . . . .
C36 C 0.56585(7) 0.9056(2) 0.42413(8) 0.0387(4) Uani 1 1 d . . . . .
C8 C 0.31881(7) 0.63744(19) 0.51526(8) 0.0368(4) Uani 1 1 d . . . . .
C42 C 0.66531(7) 0.6185(2) 0.66533(8) 0.0391(4) Uani 1 1 d . . . . .
H42 H 0.677536 0.578037 0.700977 0.047 Uiso 1 1 calc R U . . .
C28 C 0.38423(7) 0.66308(19) 0.51740(8) 0.0367(4) Uani 1 1 d . . . . .
C25 C 0.46172(8) 1.0885(2) 0.32463(8) 0.0437(4) Uani 1 1 d . . . . .
H25 H 0.442775 1.128815 0.353550 0.052 Uiso 1 1 calc R U . . .
C5 C 0.19613(7) 0.5951(2) 0.50927(8) 0.0397(4) Uani 1 1 d . . . . .
C18 C 0.83525(8) 0.8621(2) 0.50036(8) 0.0429(5) Uani 1 1 d . . . . .
H18 H 0.857747 0.827517 0.472913 0.051 Uiso 1 1 calc R U . . .
C19 C 0.77828(7) 0.8138(2) 0.50181(8) 0.0432(5) Uani 1 1 d . . . . .
H19 H 0.762745 0.746932 0.475365 0.052 Uiso 1 1 calc R U . . .
C24 C 0.45263(8) 1.1425(2) 0.26950(8) 0.0433(4) Uani 1 1 d . . . . .
H24 H 0.426722 1.216899 0.261388 0.052 Uiso 1 1 calc R U . . .
C21 C 0.76882(7) 0.9588(2) 0.58315(8) 0.0402(4) Uani 1 1 d . . . . .
H21 H 0.747159 0.989333 0.611979 0.048 Uiso 1 1 calc R U . . .
C22 C 0.82597(7) 1.0084(2) 0.58129(8) 0.0402(4) Uani 1 1 d . . . . .
H22 H 0.842033 1.073475 0.608310 0.048 Uiso 1 1 calc R U . . .
C11 C 0.57625(8) 0.3074(2) 0.80924(8) 0.0410(4) Uani 1 1 d . . . . .
C23 C 0.48195(8) 1.0865(2) 0.22600(8) 0.0404(4) Uani 1 1 d . . . . .
C1 C 0.13022(8) 0.5710(2) 0.50641(9) 0.0442(5) Uani 1 1 d . . . . .
C13 C 0.53285(8) 0.4912(2) 0.74954(8) 0.0442(5) Uani 1 1 d . . . . .
H13 H 0.506258 0.565036 0.744066 0.053 Uiso 1 1 calc R U . . .
C15 C 0.60815(8) 0.3499(2) 0.71657(8) 0.0425(4) Uani 1 1 d . . . . .
H15 H 0.632847 0.327843 0.688993 0.051 Uiso 1 1 calc R U . . .
C6 C 0.22741(8) 0.5450(2) 0.46664(9) 0.0442(5) Uani 1 1 d . . . . .
H6 H 0.207536 0.496245 0.435682 0.053 Uiso 1 1 calc R U . . .
C2 C 0.57609(8) 0.2238(2) 0.86327(8) 0.0449(5) Uani 1 1 d . . . . .
C27 C 0.52735(8) 0.9189(2) 0.29331(8) 0.0434(4) Uani 1 1 d . . . . .
H27 H 0.552194 0.842429 0.300931 0.052 Uiso 1 1 calc R U . . .
C33 C 0.36319(7) 0.8133(2) 0.42957(8) 0.0428(4) Uani 1 1 d . . . . .
H33 H 0.321907 0.810318 0.425160 0.051 Uiso 1 1 calc R U . . .
C16 C 0.61252(8) 0.2750(2) 0.76756(8) 0.0454(5) Uani 1 1 d . . . . .
H16 H 0.639838 0.202742 0.773865 0.054 Uiso 1 1 calc R U . . .
C7 C 0.28802(8) 0.5664(2) 0.46945(8) 0.0441(5) Uani 1 1 d . . . . .
H7 H 0.308303 0.532658 0.440161 0.053 Uiso 1 1 calc R U . . .
C4 C 0.47588(9) 1.1485(2) 0.16759(9) 0.0469(5) Uani 1 1 d . . . . .
C01H C 0.51961(8) 0.9746(2) 0.23856(8) 0.0453(5) Uani 1 1 d . . . . .
H01H H 0.539789 0.936797 0.209972 0.054 Uiso 1 1 calc R U . . .
C34 C 0.39681(8) 0.8778(2) 0.39447(8) 0.0421(4) Uani 1 1 d . . . . .
H34 H 0.383408 0.925274 0.360659 0.051 Uiso 1 1 calc R U . . .
C12 C 0.53737(8) 0.4175(2) 0.80017(9) 0.0465(5) Uani 1 1 d . . . . .
H12 H 0.514019 0.442011 0.828561 0.056 Uiso 1 1 calc R U . . .
C9 C 0.28760(8) 0.6856(2) 0.55829(9) 0.0519(5) Uani 1 1 d . . . . .
H9 H 0.307614 0.732385 0.589728 0.062 Uiso 1 1 calc R U . . .
C46 C 0.40374(8) 0.4944(2) 0.59964(9) 0.0516(5) Uani 1 1 d . . . . .
H46 H 0.365581 0.459188 0.599660 0.062 Uiso 1 1 calc R U . . .
C45 C 0.45175(8) 0.4579(2) 0.63584(9) 0.0506(5) Uani 1 1 d . . . . .
H45 H 0.452813 0.392599 0.665314 0.061 Uiso 1 1 calc R U . . .
C38 C 0.66272(8) 0.9542(2) 0.44536(9) 0.0521(5) Uani 1 1 d . . . . .
H38 H 0.700832 0.988965 0.444413 0.062 Uiso 1 1 calc R U . . .
C10 C 0.22677(8) 0.6651(2) 0.55527(9) 0.0547(6) Uani 1 1 d . . . . .
H10 H 0.206440 0.698869 0.584526 0.066 Uiso 1 1 calc R U . . .
C37 C 0.61559(8) 0.9775(2) 0.40572(9) 0.0516(5) Uani 1 1 d . . . . .
H37 H 0.615272 1.030555 0.372407 0.062 Uiso 1 1 calc R U . . .
N5 N 0.78516(14) 0.5132(4) 0.77538(15) 0.1135(10) Uani 1 1 d . . . . .
C48 C 0.78681(13) 0.4330(4) 0.73946(17) 0.0890(10) Uani 1 1 d . . . . .
C49 C 0.78858(16) 0.3323(5) 0.69404(17) 0.1173(12) Uani 1 1 d . . . . .
H49A H 0.828877 0.319944 0.686508 0.176 Uiso 1 1 calc R U . . .
H49B H 0.764909 0.364746 0.659723 0.176 Uiso 1 1 calc R U . . .
H49C H 0.773148 0.245149 0.705632 0.176 Uiso 1 1 calc R U . . .
H5 H 1.000000 1.000000 0.500000 0.20(3) Uiso 1 2 d S . P . .
H1AC H 0.9862(6) 0.6524(16) 0.45389(17) 0.086(9) Uiso 1 1 d D . . . .
H1AD H 1.0192(3) 0.6570(15) 0.5080(5) 0.055(7) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O5 C3 1.293(2) . ?
O5 H5 1.2302(11) . ?
O1 C1 1.236(2) . ?
O6 C3 1.220(2) . ?
N3 H3 0.8600 . ?
N3 C43 1.370(2) . ?
N3 C40 1.374(2) . ?
N2 H2 0.8600 . ?
N2 C39 1.373(2) . ?
N2 C36 1.366(2) . ?
N4 H4 0.8600 . ?
N4 C44 1.368(2) . ?
N4 C47 1.369(2) . ?
O8 H8 0.8200 . ?
O8 C4 1.307(2) . ?
O3 H3A 0.8200 . ?
O3 C2 1.301(2) . ?
N1 H1 0.8600 . ?
N1 C35 1.360(2) . ?
N1 C32 1.370(2) . ?
O4 C2 1.213(2) . ?
O7 C4 1.215(2) . ?
N1A H1AA 0.8496 . ?
N1A H1AB 0.8499 . ?
N1A H1AC 0.8411 . ?
N1A H1AD 0.8411 . ?
O2 C1 1.250(2) . ?
C43 C31 1.403(2) . ?
C43 C42 1.436(2) . ?
C26 C29 1.492(2) . ?
C26 C25 1.390(3) . ?
C26 C27 1.394(3) . ?
C20 C30 1.499(2) . ?
C20 C19 1.394(2) . ?
C20 C21 1.384(3) . ?
C14 C31 1.492(2) . ?
C14 C13 1.396(2) . ?
C14 C15 1.390(3) . ?
C31 C44 1.402(2) . ?
C35 C29 1.406(2) . ?
C35 C34 1.442(2) . ?
C40 C41 1.433(2) . ?
C40 C30 1.396(2) . ?
C3 C17 1.495(2) . ?
C32 C28 1.392(2) . ?
C32 C33 1.433(2) . ?
C29 C36 1.398(2) . ?
C41 H41 0.9300 . ?
C41 C42 1.350(2) . ?
C39 C30 1.393(2) . ?
C39 C38 1.437(2) . ?
C17 C18 1.379(3) . ?
C17 C22 1.391(2) . ?
C44 C45 1.433(2) . ?
C47 C28 1.395(2) . ?
C47 C46 1.425(3) . ?
C36 C37 1.435(2) . ?
C8 C28 1.500(2) . ?
C8 C7 1.383(3) . ?
C8 C9 1.381(3) . ?
C42 H42 0.9300 . ?
C25 H25 0.9300 . ?
C25 C24 1.381(3) . ?
C5 C1 1.507(2) . ?
C5 C6 1.381(2) . ?
C5 C10 1.380(3) . ?
C18 H18 0.9300 . ?
C18 C19 1.378(2) . ?
C19 H19 0.9300 . ?
C24 H24 0.9300 . ?
C24 C23 1.391(3) . ?
C21 H21 0.9300 . ?
C21 C22 1.388(2) . ?
C22 H22 0.9300 . ?
C11 C2 1.497(3) . ?
C11 C16 1.387(3) . ?
C11 C12 1.377(3) . ?
C23 C4 1.480(3) . ?
C23 C01H 1.382(3) . ?
C13 H13 0.9300 . ?
C13 C12 1.372(3) . ?
C15 H15 0.9300 . ?
C15 C16 1.386(3) . ?
C6 H6 0.9300 . ?
C6 C7 1.384(2) . ?
C27 H27 0.9300 . ?
C27 C01H 1.378(3) . ?
C33 H33 0.9300 . ?
C33 C34 1.340(2) . ?
C16 H16 0.9300 . ?
C7 H7 0.9300 . ?
C01H H01H 0.9300 . ?
C34 H34 0.9300 . ?
C12 H12 0.9300 . ?
C9 H9 0.9300 . ?
C9 C10 1.388(3) . ?
C46 H46 0.9300 . ?
C46 C45 1.340(3) . ?
C45 H45 0.9300 . ?
C38 H38 0.9300 . ?
C38 C37 1.343(3) . ?
C10 H10 0.9300 . ?
C37 H37 0.9300 . ?
N5 C48 1.144(5) . ?
C48 C49 1.441(5) . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 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
C3 O5 H5 112.37(12) . . ?
C43 N3 H3 126.4 . . ?
C43 N3 C40 107.16(13) . . ?
C40 N3 H3 126.4 . . ?
C39 N2 H2 125.7 . . ?
C36 N2 H2 125.7 . . ?
C36 N2 C39 108.66(14) . . ?
C44 N4 H4 125.8 . . ?
C44 N4 C47 108.49(14) . . ?
C47 N4 H4 125.8 . . ?
C4 O8 H8 109.5 . . ?
C2 O3 H3A 109.5 . . ?
C35 N1 H1 126.4 . . ?
C35 N1 C32 107.10(14) . . ?
C32 N1 H1 126.4 . . ?
H1AA N1A H1AB 104.5 . . ?
H1AA N1A H1AC 110.3 . . ?
H1AA N1A H1AD 110.3 . . ?
H1AB N1A H1AC 110.2 . . ?
H1AB N1A H1AD 110.2 . . ?
H1AC N1A H1AD 111.16(16) . . ?
N3 C43 C31 125.37(15) . . ?
N3 C43 C42 109.06(14) . . ?
C31 C43 C42 125.54(16) . . ?
C25 C26 C29 121.91(16) . . ?
C25 C26 C27 117.84(16) . . ?
C27 C26 C29 120.24(16) . . ?
C19 C20 C30 119.01(16) . . ?
C21 C20 C30 122.31(15) . . ?
C21 C20 C19 118.57(15) . . ?
C13 C14 C31 119.47(16) . . ?
C15 C14 C31 122.77(15) . . ?
C15 C14 C13 117.76(16) . . ?
C43 C31 C14 118.87(15) . . ?
C44 C31 C43 124.79(16) . . ?
C44 C31 C14 116.26(14) . . ?
N1 C35 C29 125.06(15) . . ?
N1 C35 C34 109.35(14) . . ?
C29 C35 C34 125.58(16) . . ?
N3 C40 C41 108.95(14) . . ?
N3 C40 C30 125.24(15) . . ?
C30 C40 C41 125.78(15) . . ?
O5 C3 C17 114.63(15) . . ?
O6 C3 O5 122.45(15) . . ?
O6 C3 C17 122.91(15) . . ?
N1 C32 C28 126.03(16) . . ?
N1 C32 C33 108.86(15) . . ?
C28 C32 C33 125.06(15) . . ?
C35 C29 C26 118.25(15) . . ?
C36 C29 C26 117.22(14) . . ?
C36 C29 C35 124.51(16) . . ?
C40 C41 H41 126.3 . . ?
C42 C41 C40 107.49(15) . . ?
C42 C41 H41 126.3 . . ?
N2 C39 C30 126.88(15) . . ?
N2 C39 C38 107.43(15) . . ?
C30 C39 C38 125.65(15) . . ?
C18 C17 C3 120.64(15) . . ?
C18 C17 C22 119.01(15) . . ?
C22 C17 C3 120.34(16) . . ?
N4 C44 C31 126.30(15) . . ?
N4 C44 C45 107.59(15) . . ?
C31 C44 C45 126.06(16) . . ?
C40 C30 C20 118.64(15) . . ?
C39 C30 C20 115.02(15) . . ?
C39 C30 C40 126.34(15) . . ?
N4 C47 C28 126.19(15) . . ?
N4 C47 C46 107.94(16) . . ?
C28 C47 C46 125.87(15) . . ?
N2 C36 C29 126.73(15) . . ?
N2 C36 C37 108.16(15) . . ?
C29 C36 C37 124.96(16) . . ?
C7 C8 C28 120.61(16) . . ?
C9 C8 C28 121.10(16) . . ?
C9 C8 C7 118.28(15) . . ?
C43 C42 H42 126.3 . . ?
C41 C42 C43 107.32(16) . . ?
C41 C42 H42 126.3 . . ?
C32 C28 C47 126.13(15) . . ?
C32 C28 C8 116.80(15) . . ?
C47 C28 C8 117.07(15) . . ?
C26 C25 H25 119.5 . . ?
C24 C25 C26 120.92(17) . . ?
C24 C25 H25 119.5 . . ?
C6 C5 C1 120.78(16) . . ?
C10 C5 C1 120.66(16) . . ?
C10 C5 C6 118.54(16) . . ?
C17 C18 H18 119.6 . . ?
C19 C18 C17 120.79(16) . . ?
C19 C18 H18 119.6 . . ?
C20 C19 H19 119.7 . . ?
C18 C19 C20 120.62(17) . . ?
C18 C19 H19 119.7 . . ?
C25 C24 H24 119.8 . . ?
C25 C24 C23 120.49(17) . . ?
C23 C24 H24 119.8 . . ?
C20 C21 H21 119.7 . . ?
C20 C21 C22 120.69(16) . . ?
C22 C21 H21 119.7 . . ?
C17 C22 H22 119.9 . . ?
C21 C22 C17 120.21(17) . . ?
C21 C22 H22 119.9 . . ?
C16 C11 C2 122.42(17) . . ?
C12 C11 C2 118.22(16) . . ?
C12 C11 C16 119.32(17) . . ?
C24 C23 C4 121.38(17) . . ?
C01H C23 C24 119.03(17) . . ?
C01H C23 C4 119.52(17) . . ?
O1 C1 O2 121.99(16) . . ?
O1 C1 C5 119.92(15) . . ?
O2 C1 C5 118.09(16) . . ?
C14 C13 H13 119.3 . . ?
C12 C13 C14 121.33(17) . . ?
C12 C13 H13 119.3 . . ?
C14 C15 H15 119.6 . . ?
C16 C15 C14 120.89(17) . . ?
C16 C15 H15 119.6 . . ?
C5 C6 H6 119.6 . . ?
C5 C6 C7 120.76(17) . . ?
C7 C6 H6 119.6 . . ?
O3 C2 C11 114.87(16) . . ?
O4 C2 O3 123.50(18) . . ?
O4 C2 C11 121.62(18) . . ?
C26 C27 H27 119.3 . . ?
C01H C27 C26 121.47(17) . . ?
C01H C27 H27 119.3 . . ?
C32 C33 H33 126.1 . . ?
C34 C33 C32 107.82(15) . . ?
C34 C33 H33 126.1 . . ?
C11 C16 H16 119.9 . . ?
C15 C16 C11 120.16(17) . . ?
C15 C16 H16 119.9 . . ?
C8 C7 C6 120.86(17) . . ?
C8 C7 H7 119.6 . . ?
C6 C7 H7 119.6 . . ?
O8 C4 C23 114.65(16) . . ?
O7 C4 O8 122.95(18) . . ?
O7 C4 C23 122.39(18) . . ?
C23 C01H H01H 119.9 . . ?
C27 C01H C23 120.20(17) . . ?
C27 C01H H01H 119.9 . . ?
C35 C34 H34 126.6 . . ?
C33 C34 C35 106.77(16) . . ?
C33 C34 H34 126.6 . . ?
C11 C12 H12 119.8 . . ?
C13 C12 C11 120.45(17) . . ?
C13 C12 H12 119.8 . . ?
C8 C9 H9 119.6 . . ?
C8 C9 C10 120.87(18) . . ?
C10 C9 H9 119.6 . . ?
C47 C46 H46 126.0 . . ?
C45 C46 C47 108.00(16) . . ?
C45 C46 H46 126.0 . . ?
C44 C45 H45 126.0 . . ?
C46 C45 C44 107.91(17) . . ?
C46 C45 H45 126.0 . . ?
C39 C38 H38 125.9 . . ?
C37 C38 C39 108.20(16) . . ?
C37 C38 H38 125.9 . . ?
C5 C10 C9 120.67(18) . . ?
C5 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C36 C37 H37 126.2 . . ?
C38 C37 C36 107.54(16) . . ?
C38 C37 H37 126.2 . . ?
N5 C48 C49 179.7(4) . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 N2 0.86 2.40 2.931(2) 120.2 . yes
N3 H3 N4 0.86 2.36 2.8892(18) 120.0 . yes
N2 H2 N3 0.86 2.41 2.931(2) 119.6 . yes
N2 H2 N1 0.86 2.35 2.8751(18) 120.0 . yes
N4 H4 N3 0.86 2.36 2.8892(18) 120.3 . yes
N4 H4 N1 0.86 2.41 2.933(2) 119.5 . yes
O8 H8 O6 0.82 1.79 2.6034(18) 175.3 4_585 yes
O3 H3A O1 0.82 1.79 2.6087(18) 176.9 4_666 yes
N1 H1 N2 0.86 2.34 2.8751(18) 121.0 . yes
N1 H1 N4 0.86 2.41 2.933(2) 119.4 . yes
N1A H1AA O1 0.85 2.03 2.876(2) 176.0 3_666 yes
N1A H1AB O5 0.85 2.09 2.931(2) 172.6 . yes
N1A H1AB O4 0.85 2.63 2.907(2) 100.1 2_656 yes
N1A H1AC O7 0.84 2.065(2) 2.905(2) 177.5(16) 2_645 yes
N1A H1AD O2 0.84 2.023(3) 2.860(2) 173.5(14) 1_655 yes

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
O5 C3 C17 C18 -5.4(3) . . . . ?
O5 C3 C17 C22 174.99(17) . . . . ?
O6 C3 C17 C18 174.0(2) . . . . ?
O6 C3 C17 C22 -5.7(3) . . . . ?
N3 C43 C31 C14 179.97(16) . . . . ?
N3 C43 C31 C44 -3.5(3) . . . . ?
N3 C43 C42 C41 -1.5(2) . . . . ?
N3 C40 C41 C42 -0.6(2) . . . . ?
N3 C40 C30 C20 -175.14(16) . . . . ?
N3 C40 C30 C39 4.2(3) . . . . ?
N2 C39 C30 C20 179.19(17) . . . . ?
N2 C39 C30 C40 -0.2(3) . . . . ?
N2 C39 C38 C37 -0.8(2) . . . . ?
N2 C36 C37 C38 0.0(3) . . . . ?
N4 C44 C45 C46 -1.7(2) . . . . ?
N4 C47 C28 C32 8.4(3) . . . . ?
N4 C47 C28 C8 -172.37(18) . . . . ?
N4 C47 C46 C45 1.3(3) . . . . ?
N1 C35 C29 C26 170.89(17) . . . . ?
N1 C35 C29 C36 -7.7(3) . . . . ?
N1 C35 C34 C33 0.6(2) . . . . ?
N1 C32 C28 C47 1.1(3) . . . . ?
N1 C32 C28 C8 -178.09(17) . . . . ?
N1 C32 C33 C34 3.1(2) . . . . ?
C43 N3 C40 C41 -0.32(19) . . . . ?
C43 N3 C40 C30 177.65(16) . . . . ?
C43 C31 C44 N4 -6.8(3) . . . . ?
C43 C31 C44 C45 175.92(19) . . . . ?
C26 C29 C36 N2 -172.94(18) . . . . ?
C26 C29 C36 C37 12.1(3) . . . . ?
C26 C25 C24 C23 -2.0(3) . . . . ?
C26 C27 C01H C23 -1.3(3) . . . . ?
C20 C21 C22 C17 -1.4(3) . . . . ?
C14 C31 C44 N4 169.84(17) . . . . ?
C14 C31 C44 C45 -7.4(3) . . . . ?
C14 C13 C12 C11 -0.2(3) . . . . ?
C14 C15 C16 C11 -0.5(3) . . . . ?
C31 C43 C42 C41 -179.50(17) . . . . ?
C31 C14 C13 C12 177.08(18) . . . . ?
C31 C14 C15 C16 -176.73(18) . . . . ?
C31 C44 C45 C46 176.0(2) . . . . ?
C35 N1 C32 C28 174.61(18) . . . . ?
C35 N1 C32 C33 -2.7(2) . . . . ?
C35 C29 C36 N2 5.6(3) . . . . ?
C35 C29 C36 C37 -169.3(2) . . . . ?
C40 N3 C43 C31 179.12(17) . . . . ?
C40 N3 C43 C42 1.08(19) . . . . ?
C40 C41 C42 C43 1.2(2) . . . . ?
C3 C17 C18 C19 -177.33(19) . . . . ?
C3 C17 C22 C21 178.01(18) . . . . ?
C32 N1 C35 C29 -178.37(18) . . . . ?
C32 N1 C35 C34 1.4(2) . . . . ?
C32 C33 C34 C35 -2.2(2) . . . . ?
C29 C26 C25 C24 -177.93(18) . . . . ?
C29 C26 C27 C01H 179.59(17) . . . . ?
C29 C35 C34 C33 -179.68(19) . . . . ?
C29 C36 C37 C38 175.8(2) . . . . ?
C41 C40 C30 C20 2.5(3) . . . . ?
C41 C40 C30 C39 -178.17(18) . . . . ?
C39 N2 C36 C29 -176.20(19) . . . . ?
C39 N2 C36 C37 -0.5(2) . . . . ?
C39 C38 C37 C36 0.4(3) . . . . ?
C17 C18 C19 C20 0.0(3) . . . . ?
C44 N4 C47 C28 177.90(19) . . . . ?
C44 N4 C47 C46 -2.3(2) . . . . ?
C30 C20 C19 C18 173.30(18) . . . . ?
C30 C20 C21 C22 -172.50(18) . . . . ?
C30 C40 C41 C42 -178.55(17) . . . . ?
C30 C39 C38 C37 -178.7(2) . . . . ?
C47 N4 C44 C31 -175.23(18) . . . . ?
C47 N4 C44 C45 2.5(2) . . . . ?
C47 C46 C45 C44 0.2(3) . . . . ?
C36 N2 C39 C30 178.64(18) . . . . ?
C36 N2 C39 C38 0.8(2) . . . . ?
C8 C9 C10 C5 0.5(4) . . . . ?
C42 C43 C31 C14 -2.3(3) . . . . ?
C42 C43 C31 C44 174.25(18) . . . . ?
C28 C32 C33 C34 -174.23(19) . . . . ?
C28 C47 C46 C45 -179.0(2) . . . . ?
C28 C8 C7 C6 -178.64(18) . . . . ?
C28 C8 C9 C10 178.1(2) . . . . ?
C25 C26 C29 C35 59.2(2) . . . . ?
C25 C26 C29 C36 -122.1(2) . . . . ?
C25 C26 C27 C01H 0.3(3) . . . . ?
C25 C24 C23 C4 -176.00(18) . . . . ?
C25 C24 C23 C01H 1.0(3) . . . . ?
C5 C6 C7 C8 0.6(3) . . . . ?
C18 C17 C22 C21 -1.6(3) . . . . ?
C19 C20 C30 C40 114.9(2) . . . . ?
C19 C20 C30 C39 -64.5(2) . . . . ?
C19 C20 C21 C22 3.7(3) . . . . ?
C24 C23 C4 O8 -15.7(3) . . . . ?
C24 C23 C4 O7 163.6(2) . . . . ?
C24 C23 C01H C27 0.6(3) . . . . ?
C21 C20 C30 C40 -68.9(2) . . . . ?
C21 C20 C30 C39 111.7(2) . . . . ?
C21 C20 C19 C18 -3.0(3) . . . . ?
C22 C17 C18 C19 2.3(3) . . . . ?
C1 C5 C6 C7 -179.63(19) . . . . ?
C1 C5 C10 C9 179.1(2) . . . . ?
C13 C14 C31 C43 120.77(19) . . . . ?
C13 C14 C31 C44 -56.1(2) . . . . ?
C13 C14 C15 C16 2.6(3) . . . . ?
C15 C14 C31 C43 -59.9(2) . . . . ?
C15 C14 C31 C44 123.3(2) . . . . ?
C15 C14 C13 C12 -2.3(3) . . . . ?
C6 C5 C1 O1 3.9(3) . . . . ?
C6 C5 C1 O2 -176.5(2) . . . . ?
C6 C5 C10 C9 0.5(3) . . . . ?
C2 C11 C16 C15 175.66(18) . . . . ?
C2 C11 C12 C13 -175.41(18) . . . . ?
C27 C26 C29 C35 -120.0(2) . . . . ?
C27 C26 C29 C36 58.7(2) . . . . ?
C27 C26 C25 C24 1.3(3) . . . . ?
C33 C32 C28 C47 178.03(19) . . . . ?
C33 C32 C28 C8 -1.2(3) . . . . ?
C16 C11 C2 O3 10.1(3) . . . . ?
C16 C11 C2 O4 -169.1(2) . . . . ?
C16 C11 C12 C13 2.5(3) . . . . ?
C7 C8 C28 C32 65.4(2) . . . . ?
C7 C8 C28 C47 -113.9(2) . . . . ?
C7 C8 C9 C10 -0.9(3) . . . . ?
C4 C23 C01H C27 177.69(18) . . . . ?
C01H C23 C4 O8 167.30(19) . . . . ?
C01H C23 C4 O7 -13.4(3) . . . . ?
C34 C35 C29 C26 -8.8(3) . . . . ?
C34 C35 C29 C36 172.62(19) . . . . ?
C12 C11 C2 O3 -172.13(19) . . . . ?
C12 C11 C2 O4 8.6(3) . . . . ?
C12 C11 C16 C15 -2.1(3) . . . . ?
C9 C8 C28 C32 -113.7(2) . . . . ?
C9 C8 C28 C47 67.1(3) . . . . ?
C9 C8 C7 C6 0.4(3) . . . . ?
C46 C47 C28 C32 -171.3(2) . . . . ?
C46 C47 C28 C8 7.9(3) . . . . ?
C38 C39 C30 C20 -3.3(3) . . . . ?
C38 C39 C30 C40 177.29(19) . . . . ?
C10 C5 C1 O1 -174.6(2) . . . . ?
C10 C5 C1 O2 4.9(3) . . . . ?
C10 C5 C6 C7 -1.1(3) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 278 electrons were 
found in a volume of 1218Å³ in 1 void per unit cell. 
This is consistent with the presence of 7[H2O] per Formula Unit 
which account for 280 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 0.250 0.194 0.750 609.2 139.2 '14 water'
2 -0.250 0.835 0.250 609.2 139.2 '14 water'

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
