# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_tx401
_database_code_depnum_ccdc_archive 'CCDC 1922443'
loop_
_audit_author_name
_audit_author_address
TRZ-OAC
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2019-06-12 deposited with the CCDC.	2019-07-18 downloaded from the CCDC.
;
_audit_creation_date             2019-03-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H28 N4 O2'
_chemical_formula_sum            'C36 H28 N4 O2'
_chemical_formula_weight         548.62
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNO
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      orthorhombic
_space_group_IT_number           52
_space_group_name_H-M_alt        'P n n a'
_space_group_name_Hall           '-P 2a 2bc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x, y-1/2, z-1/2'

_cell_length_a                   11.45750(10)
_cell_length_b                   10.69620(10)
_cell_length_c                   27.0458(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3314.51(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    22436
_cell_measurement_temperature    170.01(10)
_cell_measurement_theta_max      75.2760
_cell_measurement_theta_min      3.8830
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.550
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.099
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.355
_exptl_crystal_size_mid          0.345
_exptl_crystal_size_min          0.324
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_unetI/netI     0.0098
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            30875
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.336
_diffrn_reflns_theta_min         4.445
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -60.00  25.00   0.50    0.05    --  -47.20  46.00-128.00  170
  2  ω   -120.00 -34.00   0.50    0.05    --  -47.20 -46.00  81.00  172
  3  ω     35.00 120.00   0.50    0.05    --   47.20  46.00-128.00  170
  4  ω    -24.00  60.00   0.50    0.05    --   47.20 -46.00  81.00  168
  5  ω   -112.00 -26.00   0.50    0.08    --  -99.00  46.00-128.00  172
  6  ω   -168.00 -86.00   0.50    0.08    --  -99.00 -46.00  81.00  164
  7  ω     31.00 116.00   0.50    0.08    --  103.25 -46.00  81.00  170
  8  ω     91.00 169.00   0.50    0.08    --  103.25  46.00-128.00  156
  9  ω   -120.00 -71.00   0.50    0.05    --  -47.20-125.00-180.00   98
 10  ω     16.00  95.00   0.50    0.05    --   47.20-125.00 -60.00  158
 11  ω   -113.00 -24.00   0.50    0.08    --  -99.00  15.00  90.00  178
 12  ω   -112.00 -24.00   0.50    0.08    --  -99.00  30.00  30.00  176
 13  ω   -115.00 -26.00   0.50    0.08    --  -99.00  61.00 120.00  178
 14  ω   -168.00 -90.00   0.50    0.08    --  -99.00 -30.00 -30.00  156
 15  ω   -160.00 -86.00   0.50    0.08    --  -99.00 -45.00 120.00  148
 16  ω   -112.00 -45.00   0.50    0.08    --  -99.00  45.00  60.00  134
 17  ω     92.00 158.00   0.50    0.08    --  103.25  15.00  30.00  132
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0701978000
_diffrn_orient_matrix_UB_12      0.0553368000
_diffrn_orient_matrix_UB_13      -0.0433988000
_diffrn_orient_matrix_UB_21      -0.0300799000
_diffrn_orient_matrix_UB_22      0.1329845000
_diffrn_orient_matrix_UB_23      0.0177794000
_diffrn_orient_matrix_UB_31      0.1106477000
_diffrn_orient_matrix_UB_32      0.0011203000
_diffrn_orient_matrix_UB_33      0.0323276000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3090
_reflns_number_total             3289
_reflns_odcompleteness_completeness 99.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.184
_refine_diff_density_rms         0.035
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         3289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0404
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0648P)²+0.8321P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1217
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C14(H14),
 C15(H15), C16(H16), C17(H17)
2.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 0.41592(8) 0.61055(9) 0.95166(3) 0.0451(2) Uani 1 1 d . . . . .
N1 N 0.250000 0.500000 0.95247(5) 0.0399(3) Uani 1 2 d S T P . .
N2 N 0.33699(9) 0.55997(9) 0.87603(3) 0.0365(2) Uani 1 1 d . . . . .
N3 N 0.250000 0.500000 0.64283(4) 0.0369(3) Uani 1 2 d S T P . .
C1 C 0.50775(11) 0.66980(12) 0.92648(4) 0.0406(3) Uani 1 1 d . . . . .
C2 C 0.61823(12) 0.62303(13) 0.93420(5) 0.0483(3) Uani 1 1 d . . . . .
H2 H 0.629543 0.551605 0.953215 0.058 Uiso 1 1 calc R . . . .
C3 C 0.71188(13) 0.68440(15) 0.91311(6) 0.0588(4) Uani 1 1 d . . . . .
H3 H 0.786998 0.653628 0.917765 0.071 Uiso 1 1 calc R . . . .
C4 C 0.69518(14) 0.79071(17) 0.88525(6) 0.0607(4) Uani 1 1 d . . . . .
H4 H 0.758720 0.831272 0.871096 0.073 Uiso 1 1 calc R . . . .
C5 C 0.58334(14) 0.83706(15) 0.87839(5) 0.0564(4) Uani 1 1 d . . . . .
H5 H 0.572041 0.909332 0.859878 0.068 Uiso 1 1 calc R . . . .
C6 C 0.48895(12) 0.77652(14) 0.89885(5) 0.0472(3) Uani 1 1 d . . . . .
H6 H 0.413741 0.806997 0.894153 0.057 Uiso 1 1 calc R . . . .
C7 C 0.33058(10) 0.55531(12) 0.92504(4) 0.0379(3) Uani 1 1 d . . . . .
C8 C 0.250000 0.500000 0.85337(5) 0.0334(3) Uani 1 2 d S T P . .
C9 C 0.250000 0.500000 0.79851(5) 0.0338(3) Uani 1 2 d S T P . .
C10 C 0.17022(12) 0.42822(13) 0.77283(4) 0.0477(3) Uani 1 1 d . . . . .
H10 H 0.116115 0.379957 0.789935 0.057 Uiso 1 1 calc R . . . .
C11 C 0.17071(12) 0.42804(14) 0.72148(4) 0.0492(3) Uani 1 1 d . . . . .
H11 H 0.117291 0.379137 0.704274 0.059 Uiso 1 1 calc R . . . .
C12 C 0.250000 0.500000 0.69600(5) 0.0359(4) Uani 1 2 d S T P . .
C13 C 0.31781(9) 0.41113(10) 0.61768(4) 0.0309(2) Uani 1 1 d . . . . .
C14 C 0.38535(11) 0.32494(11) 0.64426(4) 0.0396(3) Uani 1 1 d . . . . .
H14 H 0.385262 0.327438 0.678630 0.048 Uiso 1 1 calc R . . . .
C15 C 0.45206(11) 0.23633(12) 0.62010(5) 0.0431(3) Uani 1 1 d . . . . .
H15 H 0.496817 0.180112 0.638223 0.052 Uiso 1 1 calc R . . . .
C16 C 0.45238(11) 0.23113(12) 0.56903(5) 0.0427(3) Uani 1 1 d . . . . .
H16 H 0.496625 0.171366 0.552526 0.051 Uiso 1 1 calc R . . . .
C17 C 0.38583(10) 0.31625(11) 0.54292(4) 0.0369(3) Uani 1 1 d . . . . .
H17 H 0.386385 0.312400 0.508573 0.044 Uiso 1 1 calc R . . . .
C18 C 0.31793(9) 0.40757(10) 0.56575(4) 0.0295(2) Uani 1 1 d . . . . .
C19 C 0.250000 0.500000 0.53393(5) 0.0299(3) Uani 1 2 d S T P . .
C20 C 0.16318(10) 0.42895(12) 0.50046(4) 0.0391(3) Uani 1 1 d . . . . .
H20A H 0.204120 0.365698 0.482209 0.059 Uiso 1 1 calc GR . . . .
H20B H 0.127332 0.486502 0.477849 0.059 Uiso 1 1 calc GR . . . .
H20C H 0.104118 0.390512 0.520533 0.059 Uiso 1 1 calc GR . . . .


_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 C1 1.4045(16) . ?
O1 C7 1.3505(15) . ?
N1 C7 1.3239(14) . ?
N1 C7 1.3240(14) 2_565 ?
N2 C7 1.3284(14) . ?
N2 C8 1.3343(12) . ?
N3 C12 1.4379(18) . ?
N3 C13 1.4034(12) . ?
N3 C13 1.4034(12) 2_565 ?
C1 C2 1.3769(17) . ?
C1 C6 1.3813(19) . ?
C2 C3 1.381(2) . ?
C3 C4 1.377(2) . ?
C4 C5 1.386(2) . ?
C5 C6 1.377(2) . ?
C8 C9 1.4837(19) . ?
C9 C10 1.3812(14) . ?
C9 C10 1.3812(15) 2_565 ?
C10 C11 1.3887(17) . ?
C11 C12 1.3758(15) . ?
C13 C14 1.4019(16) . ?
C13 C18 1.4051(14) . ?
C14 C15 1.3818(18) . ?
C15 C16 1.3823(19) . ?
C16 C17 1.3815(18) . ?
C17 C18 1.3930(16) . ?
C18 C19 1.5245(13) . ?
C19 C20 1.5448(13) 2_565 ?
C19 C20 1.5447(13) . ?

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
C7 O1 C1 118.76(9) . . ?
C7 N1 C7 111.84(13) . 2_565 ?
C7 N2 C8 113.52(10) . . ?
C13 N3 C12 118.98(6) . . ?
C13 N3 C12 118.98(6) 2_565 . ?
C13 N3 C13 122.03(12) 2_565 . ?
C2 C1 O1 116.82(12) . . ?
C2 C1 C6 121.71(13) . . ?
C6 C1 O1 121.22(11) . . ?
C1 C2 C3 118.61(13) . . ?
C4 C3 C2 120.68(14) . . ?
C3 C4 C5 119.80(16) . . ?
C6 C5 C4 120.26(15) . . ?
C5 C6 C1 118.93(13) . . ?
N1 C7 O1 113.68(9) . . ?
N1 C7 N2 127.91(11) . . ?
N2 C7 O1 118.40(11) . . ?
N2 C8 N2 125.31(13) 2_565 . ?
N2 C8 C9 117.35(7) 2_565 . ?
N2 C8 C9 117.35(7) . . ?
C10 C9 C8 120.20(7) 2_565 . ?
C10 C9 C8 120.20(7) . . ?
C10 C9 C10 119.60(14) . 2_565 ?
C9 C10 C11 120.07(11) . . ?
C12 C11 C10 120.19(11) . . ?
C11 C12 N3 120.07(7) 2_565 . ?
C11 C12 N3 120.07(7) . . ?
C11 C12 C11 119.86(14) . 2_565 ?
N3 C13 C18 120.22(10) . . ?
C14 C13 N3 120.17(10) . . ?
C14 C13 C18 119.61(10) . . ?
C15 C14 C13 120.93(11) . . ?
C14 C15 C16 120.10(11) . . ?
C17 C16 C15 118.86(11) . . ?
C16 C17 C18 122.95(11) . . ?
C13 C18 C19 123.11(9) . . ?
C17 C18 C13 117.55(10) . . ?
C17 C18 C19 119.32(9) . . ?
C18 C19 C18 111.25(11) . 2_565 ?
C18 C19 C20 109.91(6) . . ?
C18 C19 C20 109.91(6) 2_565 2_565 ?
C18 C19 C20 108.72(6) 2_565 . ?
C18 C19 C20 108.72(6) . 2_565 ?
C20 C19 C20 108.27(12) . 2_565 ?

_smtbx_masks_special_details     ?
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 0.032 0.250 370.9 83.7 ?
2 -0.250 -0.777 0.750 370.9 83.8 ?

_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.318
_oxdiff_exptl_absorpt_empirical_full_min 0.725
####################################################################### 
# 
# 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_tx457_sq
_database_code_depnum_ccdc_archive 'CCDC 1922444'
loop_
_audit_author_name
_audit_author_address
TAT-DMAC
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2019-06-12 deposited with the CCDC.	2019-07-18 downloaded from the CCDC.
;
_audit_creation_date             2019-03-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H44 N8 O4'
_chemical_formula_sum            'C60 H44 N8 O4'
_chemical_formula_weight         941.03
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHONCl
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                   9.64598(5)
_cell_length_b                   27.23322(15)
_cell_length_c                   18.74004(10)
_cell_angle_alpha                90
_cell_angle_beta                 101.9258(5)
_cell_angle_gamma                90
_cell_volume                     4816.58(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    24203
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      75.1960
_cell_measurement_theta_min      2.8990
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61164
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.257
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34940
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.506
_diffrn_reflns_theta_min         2.905
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -61.00  12.00   0.50    0.20    --  -47.20  54.00  89.00  146
  2  ω     -5.00  37.00   0.50    0.20    --   47.20 -54.00 -54.00   84
  3  ω     38.00  87.00   0.50    0.20    --   47.20  54.00  89.00   98
  4  ω    -70.00 -45.00   0.50    1.00    --  -99.00  54.00  89.00   50
  5  ω   -164.00-105.00   0.50    1.00    --  -99.00 -54.00 -54.00  118
  6  ω    144.00 169.00   0.50    1.00    --  103.25  54.00  89.00   50
  7  ω     92.00 118.00   0.50    1.00    --  103.25  54.00  89.00   52
  8  ω     31.00 117.00   0.50    1.00    --  103.25 -54.00 -54.00  172
  9  ω   -119.00 -72.00   0.50    0.20    --  -47.20-125.00  90.00   94
 10  ω   -100.00 -35.00   0.50    0.20    --  -47.20 -54.00 -54.00  130
 11  ω   -116.00 -91.00   0.50    0.20    --  -47.20-125.00  60.00   50
 12  ω   -146.00 -85.00   0.50    1.00    --  -99.00 -15.00-150.00  122
 13  ω   -167.00-101.00   0.50    1.00    --  -99.00 -45.00 -30.00  132
 14  ω   -112.00 -28.00   0.50    1.00    --  -99.00  30.00 -90.00  168
 15  ω   -160.00 -85.00   0.50    1.00    --  -99.00 -15.00 -30.00  150
 16  ω     32.00  79.00   0.50    1.00    --  103.25 -94.00-180.00   94
 17  ω     91.00 163.00   0.50    1.00    --  103.25  30.00-150.00  144
 18  ω     69.00  95.00   0.50    1.00    --  103.25 -30.00  30.00   52
 19  ω     28.00  53.00   0.50    1.00    --  103.25 -30.00  30.00   50
 20  ω     60.00  95.00   0.50    1.00    --  103.25 -45.00  90.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0907458000
_diffrn_orient_matrix_UB_12      -0.0352831000
_diffrn_orient_matrix_UB_13      -0.0548394000
_diffrn_orient_matrix_UB_21      -0.0926609000
_diffrn_orient_matrix_UB_22      -0.0112268000
_diffrn_orient_matrix_UB_23      0.0558357000
_diffrn_orient_matrix_UB_31      -0.0990616000
_diffrn_orient_matrix_UB_32      0.0427851000
_diffrn_orient_matrix_UB_33      -0.0305502000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8570
_reflns_number_total             9511
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         9511
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0466
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0662P)²+2.0275P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1355
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C33, C34
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3.a Aromatic/amide H refined with riding coordinates:
 C44(H44), C45(H45), C41(H41), C21(H21), C20(H20), C16(H16), C5(H5), C42(H42),
 C18(H18), C47(H47), C14(H14), C23(H23), C57(H57), C24(H24), C26(H26), C36(H36),
  C35(H35), C15(H15), C48(H48), C34(H34), C50(H50), C7(H7), C54(H54), C33(H33),
 C27(H27), C29(H29), C28(H28), C56(H56), C9(H9), C49(H49), C8(H8), C55(H55)
3.b Idealised Me refined as rotating group:
 C59(H59A,H59B,H59C), C39(H39A,H39B,H39C), C38(H38A,H38B,H38C), C60(H60A,H60B,
 H60C)
;
_atom_sites_solution_hydrogens   geom
_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
O2 O 0.26979(15) 0.50604(5) 0.12200(6) 0.0556(3) Uani 1 1 d . . . . .
O1 O 0.43142(13) 0.53314(5) 0.37939(7) 0.0473(3) Uani 1 1 d . . . . .
O3 O -0.16716(14) 0.55879(6) 0.15051(7) 0.0568(3) Uani 1 1 d . . . . .
O4 O -0.02390(13) 0.55421(6) 0.41168(6) 0.0535(3) Uani 1 1 d . . . . .
N6 N 0.19911(14) 0.54100(5) 0.38963(7) 0.0381(3) Uani 1 1 d . . . . .
N5 N 0.38958(14) 0.58176(5) 0.46804(7) 0.0391(3) Uani 1 1 d . . . . .
N8 N 0.49710(15) 0.74281(5) 0.72278(7) 0.0400(3) Uani 1 1 d . . . . .
N4 N 0.15529(15) 0.59227(5) 0.48547(7) 0.0406(3) Uani 1 1 d . . . . .
N1 N -0.08426(15) 0.58265(5) 0.05312(7) 0.0439(3) Uani 1 1 d . . . . .
N2 N 0.05368(16) 0.53077(5) 0.14300(7) 0.0427(3) Uani 1 1 d . . . . .
N3 N 0.13980(17) 0.55383(5) 0.03760(7) 0.0455(3) Uani 1 1 d . . . . .
N7 N -0.01453(16) 0.70020(5) -0.23557(7) 0.0423(3) Uani 1 1 d . . . . .
C11 C 0.29447(16) 0.60127(6) 0.50207(8) 0.0347(3) Uani 1 1 d . . . . .
C12 C 0.33406(17) 0.55230(6) 0.41327(8) 0.0368(3) Uani 1 1 d . . . . .
C44 C 0.53486(18) 0.68859(6) 0.62551(8) 0.0384(3) Uani 1 1 d . . . . .
H44 H 0.627556 0.699988 0.632321 0.046 Uiso 1 1 calc R . . . .
C45 C 0.48531(17) 0.65445(6) 0.57174(8) 0.0375(3) Uani 1 1 d . . . . .
H45 H 0.545032 0.643087 0.542241 0.045 Uiso 1 1 calc R . . . .
C10 C 0.11635(17) 0.56253(6) 0.42875(8) 0.0393(3) Uani 1 1 d . . . . .
C40 C 0.34730(16) 0.63688(5) 0.56121(8) 0.0345(3) Uani 1 1 d . . . . .
C43 C 0.44592(17) 0.70575(6) 0.66916(8) 0.0372(3) Uani 1 1 d . . . . .
C41 C 0.25943(18) 0.65382(6) 0.60591(9) 0.0400(3) Uani 1 1 d . . . . .
H41 H 0.167342 0.641950 0.599963 0.048 Uiso 1 1 calc R . . . .
C13 C 0.38834(17) 0.50156(6) 0.31971(8) 0.0380(3) Uani 1 1 d . . . . .
C21 C -0.11624(18) 0.66951(6) -0.13546(8) 0.0402(3) Uani 1 1 d . . . . .
H21 H -0.194920 0.689436 -0.151201 0.048 Uiso 1 1 calc R . . . .
C17 C 0.30964(18) 0.48844(6) 0.19364(8) 0.0406(4) Uani 1 1 d . . . . .
C1 C 0.02063(18) 0.58003(6) 0.01666(8) 0.0389(3) Uani 1 1 d . . . . .
C46 C 0.49229(16) 0.79211(6) 0.69932(8) 0.0367(3) Uani 1 1 d . . . . .
C2 C -0.06044(18) 0.55684(6) 0.11474(8) 0.0420(4) Uani 1 1 d . . . . .
C37 C -0.05425(17) 0.67857(6) -0.30521(8) 0.0389(3) Uani 1 1 d . . . . .
C20 C -0.10840(18) 0.63984(6) -0.07418(8) 0.0394(3) Uani 1 1 d . . . . .
H20 H -0.182087 0.640048 -0.049064 0.047 Uiso 1 1 calc R . . . .
C16 C 0.33534(19) 0.43917(6) 0.20252(9) 0.0435(4) Uani 1 1 d . . . . .
H16 H 0.318740 0.418141 0.162559 0.052 Uiso 1 1 calc R . . . .
C19 C 0.00875(18) 0.60996(6) -0.05034(8) 0.0391(3) Uani 1 1 d . . . . .
C5 C -0.08283(17) 0.55550(6) 0.28031(9) 0.0421(4) Uani 1 1 d . . . . .
H5 H -0.035307 0.585130 0.279403 0.051 Uiso 1 1 calc R . . . .
C58 C 0.51236(17) 0.73177(6) 0.79744(8) 0.0379(3) Uani 1 1 d . . . . .
C42 C 0.30872(18) 0.68836(6) 0.65937(9) 0.0419(4) Uani 1 1 d . . . . .
H42 H 0.249163 0.699924 0.688828 0.050 Uiso 1 1 calc R . . . .
C18 C 0.33647(19) 0.52080(6) 0.25159(9) 0.0429(4) Uani 1 1 d . . . . .
H18 H 0.320092 0.554293 0.244807 0.052 Uiso 1 1 calc R . . . .
C25 C 0.05840(17) 0.74540(6) -0.22713(9) 0.0390(3) Uani 1 1 d . . . . .
C51 C 0.55123(17) 0.82888(6) 0.74876(9) 0.0406(3) Uani 1 1 d . . . . .
C47 C 0.42911(18) 0.80433(6) 0.62745(9) 0.0425(4) Uani 1 1 d . . . . .
H47 H 0.389425 0.779836 0.594999 0.051 Uiso 1 1 calc R . . . .
C6 C -0.08415(17) 0.53153(7) 0.34498(9) 0.0429(4) Uani 1 1 d . . . . .
C22 C -0.00697(18) 0.66924(6) -0.17272(8) 0.0404(4) Uani 1 1 d . . . . .
C3 C 0.14885(19) 0.53127(6) 0.10094(8) 0.0428(4) Uani 1 1 d . . . . .
C53 C 0.56735(17) 0.76770(7) 0.84924(9) 0.0420(4) Uani 1 1 d . . . . .
C32 C -0.06196(17) 0.70764(6) -0.36780(9) 0.0413(4) Uani 1 1 d . . . . .
C30 C 0.05464(18) 0.77596(6) -0.28766(9) 0.0418(4) Uani 1 1 d . . . . .
C14 C 0.4130(2) 0.45241(6) 0.33106(9) 0.0449(4) Uani 1 1 d . . . . .
H14 H 0.447129 0.440219 0.377741 0.054 Uiso 1 1 calc R . . . .
C4 C -0.15486(18) 0.53371(7) 0.21709(9) 0.0453(4) Uani 1 1 d . . . . .
C23 C 0.1105(2) 0.63936(8) -0.14947(9) 0.0515(4) Uani 1 1 d . . . . .
H23 H 0.183777 0.639096 -0.174844 0.062 Uiso 1 1 calc R . . . .
C57 C 0.47749(19) 0.68545(7) 0.82025(9) 0.0459(4) Uani 1 1 d . . . . .
H57 H 0.444236 0.661367 0.785773 0.055 Uiso 1 1 calc R . . . .
C24 C 0.1182(2) 0.61001(7) -0.08857(9) 0.0502(4) Uani 1 1 d . . . . .
H24 H 0.197045 0.590151 -0.073002 0.060 Uiso 1 1 calc R . . . .
C26 C 0.13280(19) 0.76006(7) -0.15820(10) 0.0466(4) Uani 1 1 d . . . . .
H26 H 0.135107 0.739724 -0.118101 0.056 Uiso 1 1 calc R . . . .
C36 C -0.08541(19) 0.62854(7) -0.31193(10) 0.0464(4) Uani 1 1 d . . . . .
H36 H -0.080531 0.609325 -0.270463 0.056 Uiso 1 1 calc R . . . .
C52 C 0.62624(19) 0.81549(6) 0.82627(9) 0.0446(4) Uani 1 1 d . . . . .
C35 C -0.12370(19) 0.60755(8) -0.38062(10) 0.0521(4) Uani 1 1 d . . . . .
H35 H -0.144226 0.574175 -0.384735 0.063 Uiso 1 1 calc R . . . .
C15 C 0.3861(2) 0.42136(6) 0.27155(10) 0.0493(4) Uani 1 1 d . . . . .
H15 H 0.402600 0.387869 0.278314 0.059 Uiso 1 1 calc R . . . .
C48 C 0.4254(2) 0.85257(7) 0.60444(10) 0.0523(4) Uani 1 1 d . . . . .
H48 H 0.382574 0.860553 0.556722 0.063 Uiso 1 1 calc R . . . .
C34 C -0.13154(19) 0.63420(8) -0.44046(11) 0.0531(5) Uani 1 1 d . U . . .
H34 H -0.157678 0.619493 -0.486058 0.064 Uiso 1 1 calc R . . . .
C31 C -0.0364(2) 0.76285(7) -0.36246(10) 0.0479(4) Uani 1 1 d . . . . .
C50 C 0.5467(2) 0.87660(7) 0.72357(11) 0.0534(4) Uani 1 1 d . . . . .
H50 H 0.586335 0.901388 0.755481 0.064 Uiso 1 1 calc R . . . .
C7 C -0.1538(2) 0.48774(8) 0.34801(10) 0.0563(5) Uani 1 1 d . . . . .
H7 H -0.152711 0.472314 0.392399 0.068 Uiso 1 1 calc R . . . .
C54 C 0.5779(2) 0.75556(9) 0.92260(9) 0.0554(5) Uani 1 1 d . . . . .
H54 H 0.611866 0.779098 0.957837 0.067 Uiso 1 1 calc R . . . .
C33 C -0.10084(19) 0.68398(8) -0.43524(9) 0.0501(4) Uani 1 1 d . U . . .
H33 H -0.106254 0.702142 -0.477751 0.060 Uiso 1 1 calc R . . . .
C27 C 0.2026(2) 0.80449(7) -0.14950(11) 0.0557(5) Uani 1 1 d . . . . .
H27 H 0.251685 0.813997 -0.103522 0.067 Uiso 1 1 calc R . . . .
C59 C 0.7848(2) 0.80744(8) 0.82803(13) 0.0642(6) Uani 1 1 d . . . . .
H59A H 0.796002 0.780766 0.796211 0.096 Uiso 1 1 calc GR . . . .
H59B H 0.832859 0.799756 0.876889 0.096 Uiso 1 1 calc GR . . . .
H59C H 0.824509 0.836784 0.812088 0.096 Uiso 1 1 calc GR . . . .
C29 C 0.1271(2) 0.82052(7) -0.27643(12) 0.0547(5) Uani 1 1 d . . . . .
H29 H 0.126315 0.841259 -0.315940 0.066 Uiso 1 1 calc R . . . .
C28 C 0.2002(2) 0.83469(7) -0.20803(13) 0.0600(5) Uani 1 1 d . . . . .
H28 H 0.247474 0.864643 -0.201902 0.072 Uiso 1 1 calc R . . . .
C56 C 0.4919(2) 0.67502(9) 0.89360(10) 0.0582(5) Uani 1 1 d . . . . .
H56 H 0.468897 0.643967 0.908249 0.070 Uiso 1 1 calc R . . . .
C9 C -0.2273(2) 0.49010(9) 0.21764(10) 0.0602(5) Uani 1 1 d . . . . .
H9 H -0.276507 0.476364 0.174330 0.072 Uiso 1 1 calc R . . . .
C49 C 0.4851(3) 0.88879(7) 0.65215(12) 0.0623(5) Uani 1 1 d . . . . .
H49 H 0.484103 0.921255 0.636655 0.075 Uiso 1 1 calc R . . . .
C8 C -0.2254(3) 0.46724(9) 0.28327(12) 0.0673(6) Uani 1 1 d . . . . .
H8 H -0.273022 0.437620 0.284148 0.081 Uiso 1 1 calc R . . . .
C55 C 0.5401(2) 0.71043(10) 0.94483(10) 0.0659(6) Uani 1 1 d . . . . .
H55 H 0.547167 0.703875 0.994152 0.079 Uiso 1 1 calc R . . . .
C39 C -0.1792(2) 0.78906(8) -0.37019(13) 0.0664(6) Uani 1 1 d . . . . .
H39A H -0.236888 0.782032 -0.417266 0.100 Uiso 1 1 calc GR . . . .
H39B H -0.163899 0.823834 -0.365268 0.100 Uiso 1 1 calc GR . . . .
H39C H -0.226313 0.777736 -0.332891 0.100 Uiso 1 1 calc GR . . . .
C38 C 0.0353(3) 0.78059(9) -0.42459(12) 0.0687(6) Uani 1 1 d . . . . .
H38A H 0.124536 0.764166 -0.420888 0.103 Uiso 1 1 calc GR . . . .
H38B H 0.050610 0.815402 -0.420496 0.103 Uiso 1 1 calc GR . . . .
H38C H -0.024888 0.773211 -0.470873 0.103 Uiso 1 1 calc GR . . . .
C60 C 0.6124(3) 0.85720(9) 0.87888(12) 0.0765(7) Uani 1 1 d . . . . .
H60A H 0.655267 0.886375 0.864463 0.115 Uiso 1 1 calc GR . . . .
H60B H 0.659196 0.848146 0.927391 0.115 Uiso 1 1 calc GR . . . .
H60C H 0.513948 0.863288 0.877840 0.115 Uiso 1 1 calc GR . . . .


_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
O2 C17 1.4023(18) . ?
O2 C3 1.341(2) . ?
O1 C12 1.3430(19) . ?
O1 C13 1.4040(18) . ?
O3 C2 1.341(2) . ?
O3 C4 1.406(2) . ?
O4 C10 1.344(2) . ?
O4 C6 1.4077(19) . ?
N6 C12 1.322(2) . ?
N6 C10 1.327(2) . ?
N5 C11 1.331(2) . ?
N5 C12 1.325(2) . ?
N8 C43 1.4378(19) . ?
N8 C46 1.411(2) . ?
N8 C58 1.4086(19) . ?
N4 C11 1.337(2) . ?
N4 C10 1.327(2) . ?
N1 C1 1.335(2) . ?
N1 C2 1.331(2) . ?
N2 C2 1.325(2) . ?
N2 C3 1.328(2) . ?
N3 C1 1.341(2) . ?
N3 C3 1.323(2) . ?
N7 C37 1.411(2) . ?
N7 C25 1.410(2) . ?
N7 C22 1.438(2) . ?
C11 C40 1.482(2) . ?
C44 C45 1.382(2) . ?
C44 C43 1.383(2) . ?
C45 C40 1.390(2) . ?
C40 C41 1.388(2) . ?
C43 C42 1.382(2) . ?
C41 C42 1.385(2) . ?
C13 C18 1.375(2) . ?
C13 C14 1.368(2) . ?
C21 C20 1.393(2) . ?
C21 C22 1.379(2) . ?
C17 C16 1.368(2) . ?
C17 C18 1.381(2) . ?
C1 C19 1.481(2) . ?
C46 C51 1.402(2) . ?
C46 C47 1.399(2) . ?
C37 C32 1.404(2) . ?
C37 C36 1.395(2) . ?
C20 C19 1.389(2) . ?
C16 C15 1.374(2) . ?
C19 C24 1.393(2) . ?
C5 C6 1.379(2) . ?
C5 C4 1.378(2) . ?
C58 C53 1.403(2) . ?
C58 C57 1.395(2) . ?
C25 C30 1.401(2) . ?
C25 C26 1.400(2) . ?
C51 C52 1.527(2) . ?
C51 C50 1.380(3) . ?
C47 C48 1.381(3) . ?
C6 C7 1.376(3) . ?
C22 C23 1.390(3) . ?
C53 C52 1.518(3) . ?
C53 C54 1.397(2) . ?
C32 C31 1.524(3) . ?
C32 C33 1.399(2) . ?
C30 C31 1.535(2) . ?
C30 C29 1.395(3) . ?
C14 C15 1.381(2) . ?
C4 C9 1.379(3) . ?
C23 C24 1.383(2) . ?
C57 C56 1.382(2) . ?
C26 C27 1.378(3) . ?
C36 C35 1.387(2) . ?
C52 C59 1.539(3) . ?
C52 C60 1.528(3) . ?
C35 C34 1.325(3) . ?
C48 C49 1.375(3) . ?
C34 C33 1.387(3) . ?
C31 C39 1.531(3) . ?
C31 C38 1.549(3) . ?
C50 C49 1.388(3) . ?
C7 C8 1.384(3) . ?
C54 C55 1.371(3) . ?
C27 C28 1.367(3) . ?
C29 C28 1.384(3) . ?
C56 C55 1.373(3) . ?
C9 C8 1.375(3) . ?

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 O2 C17 120.44(13) . . ?
C12 O1 C13 119.60(13) . . ?
C2 O3 C4 119.47(14) . . ?
C10 O4 C6 119.74(12) . . ?
C12 N6 C10 112.03(13) . . ?
C12 N5 C11 113.86(14) . . ?
C46 N8 C43 117.78(12) . . ?
C58 N8 C43 119.65(13) . . ?
C58 N8 C46 120.16(13) . . ?
C10 N4 C11 113.75(13) . . ?
C2 N1 C1 113.76(14) . . ?
C2 N2 C3 112.11(14) . . ?
C3 N3 C1 113.78(15) . . ?
C37 N7 C22 118.11(13) . . ?
C25 N7 C37 120.12(13) . . ?
C25 N7 C22 118.69(13) . . ?
N5 C11 N4 125.00(14) . . ?
N5 C11 C40 117.07(14) . . ?
N4 C11 C40 117.89(13) . . ?
N6 C12 O1 119.17(13) . . ?
N6 C12 N5 127.79(14) . . ?
N5 C12 O1 113.03(14) . . ?
C45 C44 C43 119.68(15) . . ?
C44 C45 C40 120.80(14) . . ?
N6 C10 O4 119.02(14) . . ?
N6 C10 N4 127.53(15) . . ?
N4 C10 O4 113.45(14) . . ?
C45 C40 C11 120.18(13) . . ?
C41 C40 C11 120.69(14) . . ?
C41 C40 C45 119.11(14) . . ?
C44 C43 N8 119.01(14) . . ?
C42 C43 N8 120.96(14) . . ?
C42 C43 C44 120.00(14) . . ?
C42 C41 C40 120.07(15) . . ?
C18 C13 O1 119.81(15) . . ?
C14 C13 O1 117.52(14) . . ?
C14 C13 C18 122.37(15) . . ?
C22 C21 C20 119.81(15) . . ?
C16 C17 O2 117.29(15) . . ?
C16 C17 C18 122.03(15) . . ?
C18 C17 O2 120.29(15) . . ?
N1 C1 N3 124.98(14) . . ?
N1 C1 C19 118.06(14) . . ?
N3 C1 C19 116.90(15) . . ?
C51 C46 N8 119.41(14) . . ?
C47 C46 N8 120.40(14) . . ?
C47 C46 C51 120.18(15) . . ?
N1 C2 O3 113.60(15) . . ?
N2 C2 O3 118.80(14) . . ?
N2 C2 N1 127.60(16) . . ?
C32 C37 N7 119.65(15) . . ?
C36 C37 N7 120.22(14) . . ?
C36 C37 C32 120.13(15) . . ?
C19 C20 C21 120.44(16) . . ?
C17 C16 C15 118.76(15) . . ?
C20 C19 C1 120.68(15) . . ?
C20 C19 C24 119.11(15) . . ?
C24 C19 C1 120.16(15) . . ?
C4 C5 C6 117.21(16) . . ?
C53 C58 N8 119.05(15) . . ?
C57 C58 N8 120.99(14) . . ?
C57 C58 C53 119.94(15) . . ?
C43 C42 C41 120.33(15) . . ?
C13 C18 C17 117.39(15) . . ?
C30 C25 N7 119.91(14) . . ?
C26 C25 N7 120.07(15) . . ?
C26 C25 C30 120.01(16) . . ?
C46 C51 C52 120.37(15) . . ?
C50 C51 C46 117.81(16) . . ?
C50 C51 C52 121.70(16) . . ?
C48 C47 C46 120.32(17) . . ?
C5 C6 O4 119.71(16) . . ?
C7 C6 O4 117.34(15) . . ?
C7 C6 C5 122.68(15) . . ?
C21 C22 N7 119.79(15) . . ?
C21 C22 C23 120.21(15) . . ?
C23 C22 N7 120.01(16) . . ?
N2 C3 O2 119.08(14) . . ?
N3 C3 O2 113.21(15) . . ?
N3 C3 N2 127.71(16) . . ?
C58 C53 C52 120.80(14) . . ?
C54 C53 C58 117.14(17) . . ?
C54 C53 C52 121.78(16) . . ?
C37 C32 C31 121.44(15) . . ?
C33 C32 C37 116.93(16) . . ?
C33 C32 C31 121.56(15) . . ?
C25 C30 C31 121.03(15) . . ?
C29 C30 C25 117.80(17) . . ?
C29 C30 C31 120.98(16) . . ?
C13 C14 C15 118.42(15) . . ?
C5 C4 O3 119.29(17) . . ?
C5 C4 C9 122.06(16) . . ?
C9 C4 O3 118.36(16) . . ?
C24 C23 C22 119.89(17) . . ?
C56 C57 C58 120.63(17) . . ?
C23 C24 C19 120.54(16) . . ?
C27 C26 C25 120.29(18) . . ?
C35 C36 C37 119.82(17) . . ?
C51 C52 C59 109.15(15) . . ?
C51 C52 C60 110.42(16) . . ?
C53 C52 C51 110.06(14) . . ?
C53 C52 C59 107.48(15) . . ?
C53 C52 C60 111.52(17) . . ?
C60 C52 C59 108.13(18) . . ?
C34 C35 C36 121.17(19) . . ?
C16 C15 C14 121.01(16) . . ?
C49 C48 C47 119.94(18) . . ?
C35 C34 C33 120.11(17) . . ?
C32 C31 C30 110.11(13) . . ?
C32 C31 C39 108.88(16) . . ?
C32 C31 C38 110.47(16) . . ?
C30 C31 C38 110.72(16) . . ?
C39 C31 C30 108.17(16) . . ?
C39 C31 C38 108.42(17) . . ?
C51 C50 C49 122.14(18) . . ?
C6 C7 C8 118.24(17) . . ?
C55 C54 C53 122.77(18) . . ?
C34 C33 C32 121.84(17) . . ?
C28 C27 C26 120.42(18) . . ?
C28 C29 C30 121.73(19) . . ?
C27 C28 C29 119.75(18) . . ?
C55 C56 C57 120.07(19) . . ?
C8 C9 C4 118.92(17) . . ?
C48 C49 C50 119.59(18) . . ?
C9 C8 C7 120.88(19) . . ?
C54 C55 C56 119.36(17) . . ?

_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.344
_oxdiff_exptl_absorpt_empirical_full_min 0.647
####################################################################### 
# 
# 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_tx402a_sq
_database_code_depnum_ccdc_archive 'CCDC 1922445'
loop_
_audit_author_name
_audit_author_address
TAT-SpiroAC
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2019-06-12 deposited with the CCDC.	2019-07-18 downloaded from the CCDC.
;
_audit_creation_date             2019-03-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C80 H48 N8 O4'
_chemical_formula_sum            'C80 H48 N8 O4'
_chemical_formula_weight         1185.26
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNO
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                   14.9786(4)
_cell_length_b                   9.0590(2)
_cell_length_c                   57.2212(11)
_cell_angle_alpha                90
_cell_angle_beta                 94.208(2)
_cell_angle_gamma                90
_cell_volume                     7743.5(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    18786
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      75.6740
_cell_measurement_theta_min      3.0500
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.507
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.017
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.034
_exptl_crystal_size_min          0.023
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       71
_diffrn_reflns_limit_l_min       -71
_diffrn_reflns_number            52610
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         75.626
_diffrn_reflns_theta_min         3.002
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -60.00  28.00   0.25    1.00    --  -47.20  19.00 -90.00  352
  2  ω     15.00  71.00   0.25    1.00    --   47.20 -88.00-150.00  224
  3  ω     32.00  69.50   0.25    4.00    --  103.25 -88.00-150.00  150
  4  ω     81.00 115.00   0.25    4.00    --  103.25 -30.00 -30.00  136
  5  ω    106.00 145.00   0.25    4.00    --  103.25  30.00-120.00  156
  6  ω     92.00 168.00   0.25    4.00    --  103.25  45.00 -60.00  304
  7  ω     91.00 165.00   0.25    4.00    --  103.25  45.00 -90.00  296
  8  ω     83.00 151.00   0.25    4.00    --  103.25  88.00 -34.00  272
  9  ω     28.00  73.00   0.25    4.00    --  103.25 -30.00 -30.00  180
 10  ω     38.00 109.00   0.25    4.00    --  103.25 -94.00 -30.00  284
 11  ω    -15.00  11.00   0.25    1.00    --   47.20 -88.00-150.00  104
 12  ω    -75.00  10.00   0.25    1.00    --  -47.20  88.00 -34.00  340
 13  ω   -101.00 -76.00   0.25    4.00    --  -99.00  88.00 -34.00  100
 14  ω   -167.00 -86.00   0.25    4.00    --  -99.00 -45.00-120.00  324
 15  ω   -120.00 -76.00   0.25    1.00    --  -47.20-125.00-150.00  176
 16  ω   -100.00 -73.00   0.25    4.00    --  -99.00-125.00 -60.00  108
 17  ω   -120.00 -72.00   0.25    1.00    --  -47.20-125.00   0.00  192
 18  ω   -137.00-110.00   0.25    4.00    --  -99.00-125.00 -60.00  108
 19  ω   -155.00-129.00   0.25    4.00    --  -99.00 -88.00-150.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0374455000
_diffrn_orient_matrix_UB_12      -0.0073019000
_diffrn_orient_matrix_UB_13      0.0243493000
_diffrn_orient_matrix_UB_21      -0.0398126000
_diffrn_orient_matrix_UB_22      -0.1534198000
_diffrn_orient_matrix_UB_23      -0.0059363000
_diffrn_orient_matrix_UB_31      0.0874603000
_diffrn_orient_matrix_UB_32      -0.0729050000
_diffrn_orient_matrix_UB_33      0.0100529000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11977
_reflns_number_total             15105
_reflns_odcompleteness_completeness 98.25
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         15105
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0832
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1031P)²+10.3369P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2327
_refine_ls_wR_factor_ref         0.2421
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C16(H16), C17(H17), C18(H18), C19(H19), C23(H23), C24(H24), C25(H25), C26(H26),
  C28(H28), C29(H29), C31(H31), C32(H32), C37(H37), C38(H38), C39(H39),
 C41(H41), C46(H46), C47(H47), C48(H48), C50(H50), C52(H52), C53(H53), C55(H55),
  C56(H56), C58(H58), C59(H59), C60(H60), C61(H61), C66(H66), C67(H67),
 C68(H68), C69(H69), C71(H71), C72(H72), C73(H73), C74(H74), C77(H77), C78(H78),
  C79(H79), C80(H80)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 0.81424(15) 0.7633(3) 0.74349(4) 0.0472(6) Uani 1 1 d . . . . .
O2 O 0.91828(17) 0.6108(3) 0.66968(4) 0.0490(6) Uani 1 1 d . . . . .
O3 O 0.69285(18) 0.8870(3) 0.63307(4) 0.0513(6) Uani 1 1 d . . . . .
O4 O 0.62626(15) 1.1015(2) 0.70598(4) 0.0418(5) Uani 1 1 d . . . . .
N1 N 0.33392(18) 0.7857(3) 0.81743(5) 0.0417(6) Uani 1 1 d . . . . .
N2 N 0.68361(18) 0.8161(3) 0.75803(4) 0.0390(6) Uani 1 1 d . . . . .
N3 N 0.72574(17) 0.9345(3) 0.72329(4) 0.0357(5) Uani 1 1 d . . . . .
N4 N 0.58562(17) 0.9888(3) 0.73815(4) 0.0371(6) Uani 1 1 d . . . . .
N5 N 0.80609(19) 0.7579(3) 0.65296(4) 0.0401(6) Uani 1 1 d . . . . .
N6 N 0.84952(19) 0.5300(3) 0.63631(5) 0.0406(6) Uani 1 1 d . . . . .
N7 N 0.7267(2) 0.6665(3) 0.61835(5) 0.0429(6) Uani 1 1 d . . . . .
N8 N 0.7590(2) 0.1728(3) 0.54033(5) 0.0422(6) Uani 1 1 d . . . . .
C1 C 0.2490(2) 0.7561(4) 0.80628(6) 0.0467(8) Uani 1 1 d . . . . .
C2 C 0.1788(2) 0.7183(4) 0.81990(6) 0.0412(7) Uani 1 1 d . . . . .
C3 C 0.0934(2) 0.6975(4) 0.80876(6) 0.0483(8) Uani 1 1 d . . . . .
H3 H 0.046161 0.673464 0.817742 0.058 Uiso 1 1 calc R . . . .
C4 C 0.0772(3) 0.7116(5) 0.78463(7) 0.0578(10) Uani 1 1 d . . . . .
H4 H 0.019598 0.701290 0.777585 0.069 Uiso 1 1 calc R . . . .
C5 C 0.1484(3) 0.7413(6) 0.77133(7) 0.0661(12) Uani 1 1 d . . . . .
H5 H 0.139099 0.747505 0.755110 0.079 Uiso 1 1 calc R . . . .
C6 C 0.2335(3) 0.7620(5) 0.78200(7) 0.0608(11) Uani 1 1 d . . . . .
H6 H 0.280987 0.780176 0.772808 0.073 Uiso 1 1 calc R . . . .
C7 C 0.1971(2) 0.6859(4) 0.84601(6) 0.0401(7) Uani 1 1 d . . . . .
C8 C 0.2160(2) 0.5201(4) 0.84886(6) 0.0463(8) Uani 1 1 d . . . . .
C9 C 0.2839(3) 0.4371(4) 0.84037(8) 0.0580(10) Uani 1 1 d . . . . .
H9 H 0.327976 0.481720 0.832167 0.070 Uiso 1 1 calc R . . . .
C10 C 0.2853(3) 0.2869(5) 0.84426(11) 0.0784(14) Uani 1 1 d . . . . .
H10 H 0.330327 0.230197 0.838420 0.094 Uiso 1 1 calc R . . . .
C11 C 0.2202(3) 0.2182(5) 0.85682(11) 0.0830(15) Uani 1 1 d . . . . .
H11 H 0.222826 0.117009 0.859562 0.100 Uiso 1 1 calc R . . . .
C12 C 0.1521(3) 0.3016(5) 0.86512(9) 0.0713(12) Uani 1 1 d . . . . .
H12 H 0.107559 0.256573 0.873113 0.086 Uiso 1 1 calc R . . . .
C13 C 0.1505(3) 0.4533(4) 0.86142(7) 0.0511(8) Uani 1 1 d . . . . .
C15 C 0.0864(2) 0.5674(4) 0.86796(6) 0.0443(7) Uani 1 1 d . . . . .
C16 C 0.0094(3) 0.5563(5) 0.88012(7) 0.0550(9) Uani 1 1 d . . . . .
H16 H -0.008717 0.465920 0.885871 0.066 Uiso 1 1 calc R . . . .
C17 C -0.0389(3) 0.6819(5) 0.88336(7) 0.0590(10) Uani 1 1 d . . . . .
H17 H -0.090826 0.676300 0.891274 0.071 Uiso 1 1 calc R . . . .
C18 C -0.0123(3) 0.8158(5) 0.87517(7) 0.0629(11) Uani 1 1 d . . . . .
H18 H -0.046003 0.899528 0.877828 0.075 Uiso 1 1 calc R . . . .
C19 C 0.0648(3) 0.8289(4) 0.86289(7) 0.0528(9) Uani 1 1 d . . . . .
H19 H 0.082455 0.919849 0.857243 0.063 Uiso 1 1 calc R . . . .
C20 C 0.1138(2) 0.7029(4) 0.85941(6) 0.0425(7) Uani 1 1 d . . . . .
C21 C 0.2756(2) 0.7810(3) 0.85592(5) 0.0373(6) Uani 1 1 d . . . . .
C22 C 0.3423(2) 0.8238(3) 0.84136(5) 0.0369(6) Uani 1 1 d . . . . .
C23 C 0.4158(2) 0.9051(4) 0.85065(6) 0.0425(7) Uani 1 1 d . . . . .
H23 H 0.460294 0.932913 0.841036 0.051 Uiso 1 1 calc R . . . .
C24 C 0.4227(2) 0.9441(4) 0.87389(6) 0.0463(8) Uani 1 1 d . . . . .
H24 H 0.471790 0.998350 0.879949 0.056 Uiso 1 1 calc R . . . .
C25 C 0.3570(3) 0.9032(4) 0.88829(6) 0.0507(8) Uani 1 1 d . . . . .
H25 H 0.361263 0.930849 0.903981 0.061 Uiso 1 1 calc R . . . .
C26 C 0.2851(2) 0.8212(4) 0.87934(6) 0.0465(8) Uani 1 1 d . . . . .
H26 H 0.241804 0.792048 0.889242 0.056 Uiso 1 1 calc R . . . .
C27 C 0.4060(2) 0.8205(4) 0.80321(6) 0.0403(7) Uani 1 1 d . . . . .
C28 C 0.4021(2) 0.9429(4) 0.78885(6) 0.0407(7) Uani 1 1 d . . . . .
H28 H 0.355160 1.009532 0.789534 0.049 Uiso 1 1 calc R . . . .
C29 C 0.4673(2) 0.9675(4) 0.77347(6) 0.0390(7) Uani 1 1 d . . . . .
H29 H 0.463471 1.049068 0.763587 0.047 Uiso 1 1 calc R . . . .
C30 C 0.5393(2) 0.8692(3) 0.77277(5) 0.0356(6) Uani 1 1 d . . . . .
C31 C 0.5461(2) 0.7503(4) 0.78821(6) 0.0420(7) Uani 1 1 d . . . . .
H31 H 0.595511 0.688033 0.788586 0.050 Uiso 1 1 calc R . . . .
C32 C 0.4785(2) 0.7256(4) 0.80301(6) 0.0424(7) Uani 1 1 d . . . . .
H32 H 0.481771 0.644267 0.812950 0.051 Uiso 1 1 calc R . . . .
C33 C 0.6073(2) 0.8921(3) 0.75557(5) 0.0339(6) Uani 1 1 d . . . . .
C34 C 0.6481(2) 1.0036(3) 0.72312(5) 0.0357(6) Uani 1 1 d . . . . .
C35 C 0.7379(2) 0.8421(4) 0.74128(5) 0.0378(7) Uani 1 1 d . . . . .
C36 C 0.8753(2) 0.7768(4) 0.72597(5) 0.0395(7) Uani 1 1 d . . . . .
C37 C 0.9497(2) 0.8611(4) 0.73042(6) 0.0465(8) Uani 1 1 d . . . . .
H37 H 0.958103 0.913835 0.744346 0.056 Uiso 1 1 calc R . . . .
C38 C 1.0132(2) 0.8673(4) 0.71387(6) 0.0475(8) Uani 1 1 d . . . . .
H38 H 1.064288 0.924697 0.716728 0.057 Uiso 1 1 calc R . . . .
C39 C 1.0007(2) 0.7891(4) 0.69332(6) 0.0467(8) Uani 1 1 d . . . . .
H39 H 1.042759 0.793287 0.682155 0.056 Uiso 1 1 calc R . . . .
C40 C 0.9250(2) 0.7047(4) 0.68961(5) 0.0393(7) Uani 1 1 d . . . . .
C41 C 0.8603(2) 0.6965(4) 0.70553(5) 0.0396(7) Uani 1 1 d . . . . .
H41 H 0.809069 0.639519 0.702639 0.047 Uiso 1 1 calc R . . . .
C42 C 0.8545(2) 0.6364(3) 0.65249(5) 0.0368(6) Uani 1 1 d . . . . .
C43 C 0.7839(2) 0.5517(3) 0.61953(5) 0.0384(7) Uani 1 1 d . . . . .
C44 C 0.7443(2) 0.7653(4) 0.63512(5) 0.0407(7) Uani 1 1 d . . . . .
C45 C 0.7093(2) 0.9970(4) 0.65025(5) 0.0410(7) Uani 1 1 d . . . . .
C46 C 0.7682(3) 1.1096(4) 0.64637(6) 0.0483(8) Uani 1 1 d . . . . .
H46 H 0.798222 1.112568 0.632715 0.058 Uiso 1 1 calc R . . . .
C47 C 0.7816(3) 1.2178(4) 0.66321(7) 0.0531(9) Uani 1 1 d . . . . .
H47 H 0.821767 1.293821 0.660954 0.064 Uiso 1 1 calc R . . . .
C48 C 0.7362(2) 1.2150(4) 0.68345(6) 0.0433(7) Uani 1 1 d . . . . .
H48 H 0.745167 1.288295 0.694760 0.052 Uiso 1 1 calc R . . . .
C49 C 0.6777(2) 1.1011(3) 0.68630(5) 0.0352(6) Uani 1 1 d . . . . .
C50 C 0.6619(2) 0.9909(3) 0.66991(5) 0.0388(7) Uani 1 1 d . . . . .
H50 H 0.621058 0.915695 0.672060 0.047 Uiso 1 1 calc R . . . .
C51 C 0.7731(2) 0.4422(3) 0.60032(5) 0.0384(7) Uani 1 1 d . . . . .
C52 C 0.6955(2) 0.4365(3) 0.58573(5) 0.0393(7) Uani 1 1 d . . . . .
H52 H 0.646954 0.495519 0.588808 0.047 Uiso 1 1 calc R . . . .
C53 C 0.6898(2) 0.3425(4) 0.56642(6) 0.0418(7) Uani 1 1 d . . . . .
H53 H 0.637050 0.337372 0.556811 0.050 Uiso 1 1 calc R . . . .
C54 C 0.7622(2) 0.2570(3) 0.56155(6) 0.0404(7) Uani 1 1 d . . . . .
C55 C 0.8389(2) 0.2576(4) 0.57644(6) 0.0472(8) Uani 1 1 d . . . . .
H55 H 0.886880 0.197442 0.573308 0.057 Uiso 1 1 calc R . . . .
C56 C 0.8445(2) 0.3484(4) 0.59622(6) 0.0459(8) Uani 1 1 d . . . . .
H56 H 0.895270 0.346405 0.606596 0.055 Uiso 1 1 calc R . . . .
C57 C 0.7852(2) 0.2408(3) 0.51994(6) 0.0380(7) Uani 1 1 d . . . . .
C58 C 0.8123(3) 0.3889(4) 0.52035(7) 0.0493(8) Uani 1 1 d . . . . .
H58 H 0.812791 0.441995 0.534269 0.059 Uiso 1 1 calc R . . . .
C59 C 0.8382(3) 0.4566(4) 0.50040(7) 0.0561(10) Uani 1 1 d . . . . .
H59 H 0.855379 0.555235 0.500949 0.067 Uiso 1 1 calc R . . . .
C60 C 0.8389(3) 0.3803(4) 0.47979(8) 0.0621(11) Uani 1 1 d . . . . .
H60 H 0.857478 0.425860 0.466410 0.075 Uiso 1 1 calc R . . . .
C61 C 0.8114(3) 0.2341(4) 0.47913(7) 0.0544(9) Uani 1 1 d . . . . .
H61 H 0.811344 0.182421 0.465083 0.065 Uiso 1 1 calc R . . . .
C62 C 0.7838(2) 0.1625(3) 0.49887(6) 0.0380(7) Uani 1 1 d . . . . .
C63 C 0.7530(2) 0.0021(3) 0.49685(5) 0.0345(6) Uani 1 1 d . . . . .
C64 C 0.7342(2) -0.0620(3) 0.52050(5) 0.0354(6) Uani 1 1 d . . . . .
C65 C 0.7373(2) 0.0223(3) 0.54095(5) 0.0336(6) Uani 1 1 d . . . . .
C66 C 0.7156(2) -0.0426(4) 0.56207(6) 0.0410(7) Uani 1 1 d . . . . .
H66 H 0.716702 0.014077 0.575643 0.049 Uiso 1 1 calc R . . . .
C67 C 0.6927(3) -0.1897(4) 0.56282(6) 0.0471(8) Uani 1 1 d . . . . .
H67 H 0.678893 -0.232198 0.576903 0.057 Uiso 1 1 calc R . . . .
C68 C 0.6902(3) -0.2742(4) 0.54267(7) 0.0562(9) Uani 1 1 d . . . . .
H68 H 0.674886 -0.373535 0.543150 0.067 Uiso 1 1 calc R . . . .
C69 C 0.7105(3) -0.2105(4) 0.52195(6) 0.0472(8) Uani 1 1 d . . . . .
H69 H 0.708303 -0.268084 0.508466 0.057 Uiso 1 1 calc R . . . .
C70 C 0.8206(2) -0.0922(3) 0.48468(6) 0.0390(7) Uani 1 1 d . . . . .
C71 C 0.9079(2) -0.1227(4) 0.49197(7) 0.0485(8) Uani 1 1 d . . . . .
H71 H 0.933099 -0.086027 0.506139 0.058 Uiso 1 1 calc R . . . .
C72 C 0.9582(3) -0.2099(4) 0.47769(9) 0.0643(12) Uani 1 1 d . . . . .
H72 H 1.017348 -0.232590 0.482377 0.077 Uiso 1 1 calc R . . . .
C73 C 0.9199(3) -0.2629(4) 0.45649(9) 0.0659(12) Uani 1 1 d . . . . .
H73 H 0.954334 -0.319887 0.447047 0.079 Uiso 1 1 calc R . . . .
C74 C 0.8330(3) -0.2333(5) 0.44921(8) 0.0640(11) Uani 1 1 d . . . . .
H74 H 0.808099 -0.270868 0.435077 0.077 Uiso 1 1 calc R . . . .
C75 C 0.7819(3) -0.1456(4) 0.46328(6) 0.0486(8) Uani 1 1 d . . . . .
C76 C 0.6887(2) -0.0971(4) 0.46006(6) 0.0492(8) Uani 1 1 d . . . . .
C77 C 0.6207(3) -0.1228(6) 0.44253(7) 0.0684(12) Uani 1 1 d . . . . .
H77 H 0.631614 -0.180415 0.429597 0.082 Uiso 1 1 calc R . . . .
C78 C 0.5366(3) -0.0615(6) 0.44457(8) 0.0736(13) Uani 1 1 d . . . . .
H78 H 0.491533 -0.076581 0.432747 0.088 Uiso 1 1 calc R . . . .
C79 C 0.5193(3) 0.0212(6) 0.46388(7) 0.0638(11) Uani 1 1 d . . . . .
H79 H 0.462198 0.059397 0.465175 0.077 Uiso 1 1 calc R . . . .
C80 C 0.5865(2) 0.0484(4) 0.48153(6) 0.0493(8) Uani 1 1 d . . . . .
H80 H 0.575038 0.105902 0.494440 0.059 Uiso 1 1 calc R . . . .
C81 C 0.6705(2) -0.0114(4) 0.47954(5) 0.0403(7) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C35 1.346(4) . ?
O1 C36 1.411(4) . ?
O2 C40 1.420(4) . ?
O2 C42 1.340(4) . ?
O3 C44 1.346(4) . ?
O3 C45 1.409(4) . ?
O4 C34 1.345(4) . ?
O4 C49 1.410(3) . ?
N1 C1 1.406(4) . ?
N1 C22 1.409(4) . ?
N1 C27 1.433(4) . ?
N2 C33 1.333(4) . ?
N2 C35 1.323(4) . ?
N3 C34 1.319(4) . ?
N3 C35 1.329(4) . ?
N4 C33 1.349(4) . ?
N4 C34 1.324(4) . ?
N5 C42 1.320(4) . ?
N5 C44 1.328(4) . ?
N6 C42 1.335(4) . ?
N6 C43 1.338(4) . ?
N7 C43 1.346(4) . ?
N7 C44 1.325(4) . ?
N8 C54 1.432(4) . ?
N8 C57 1.401(4) . ?
N8 C65 1.403(4) . ?
C1 C2 1.397(4) . ?
C1 C6 1.393(5) . ?
C2 C3 1.400(5) . ?
C2 C7 1.528(5) . ?
C3 H3 0.9300 . ?
C3 C4 1.390(5) . ?
C4 H4 0.9300 . ?
C4 C5 1.381(6) . ?
C5 H5 0.9300 . ?
C5 C6 1.385(6) . ?
C6 H6 0.9300 . ?
C7 C8 1.534(5) . ?
C7 C20 1.520(4) . ?
C7 C21 1.532(5) . ?
C8 C9 1.382(5) . ?
C8 C13 1.396(5) . ?
C9 H9 0.9300 . ?
C9 C10 1.378(6) . ?
C10 H10 0.9300 . ?
C10 C11 1.399(7) . ?
C11 H11 0.9300 . ?
C11 C12 1.382(7) . ?
C12 H12 0.9300 . ?
C12 C13 1.390(6) . ?
C13 C15 1.478(5) . ?
C15 C16 1.394(5) . ?
C15 C20 1.395(5) . ?
C16 H16 0.9300 . ?
C16 C17 1.368(6) . ?
C17 H17 0.9300 . ?
C17 C18 1.370(6) . ?
C18 H18 0.9300 . ?
C18 C19 1.400(5) . ?
C19 H19 0.9300 . ?
C19 C20 1.379(5) . ?
C21 C22 1.401(4) . ?
C21 C26 1.386(5) . ?
C22 C23 1.397(5) . ?
C23 H23 0.9300 . ?
C23 C24 1.372(5) . ?
C24 H24 0.9300 . ?
C24 C25 1.380(5) . ?
C25 H25 0.9300 . ?
C25 C26 1.375(5) . ?
C26 H26 0.9300 . ?
C27 C28 1.379(5) . ?
C27 C32 1.386(5) . ?
C28 H28 0.9300 . ?
C28 C29 1.379(4) . ?
C29 H29 0.9300 . ?
C29 C30 1.401(4) . ?
C30 C31 1.392(5) . ?
C30 C33 1.482(4) . ?
C31 H31 0.9300 . ?
C31 C32 1.385(4) . ?
C32 H32 0.9300 . ?
C36 C37 1.360(5) . ?
C36 C41 1.381(5) . ?
C37 H37 0.9300 . ?
C37 C38 1.391(5) . ?
C38 H38 0.9300 . ?
C38 C39 1.374(5) . ?
C39 H39 0.9300 . ?
C39 C40 1.371(5) . ?
C40 C41 1.380(4) . ?
C41 H41 0.9300 . ?
C43 C51 1.481(4) . ?
C45 C46 1.378(5) . ?
C45 C50 1.374(4) . ?
C46 H46 0.9300 . ?
C46 C47 1.379(5) . ?
C47 H47 0.9300 . ?
C47 C48 1.385(5) . ?
C48 H48 0.9300 . ?
C48 C49 1.371(5) . ?
C49 C50 1.379(4) . ?
C50 H50 0.9300 . ?
C51 C52 1.382(5) . ?
C51 C56 1.399(5) . ?
C52 H52 0.9300 . ?
C52 C53 1.392(5) . ?
C53 H53 0.9300 . ?
C53 C54 1.377(5) . ?
C54 C55 1.379(5) . ?
C55 H55 0.9300 . ?
C55 C56 1.397(5) . ?
C56 H56 0.9300 . ?
C57 C58 1.401(5) . ?
C57 C62 1.397(4) . ?
C58 H58 0.9300 . ?
C58 C59 1.377(5) . ?
C59 H59 0.9300 . ?
C59 C60 1.368(6) . ?
C60 H60 0.9300 . ?
C60 C61 1.387(5) . ?
C61 H61 0.9300 . ?
C61 C62 1.391(5) . ?
C62 C63 1.527(4) . ?
C63 C64 1.517(4) . ?
C63 C70 1.531(4) . ?
C63 C81 1.532(5) . ?
C64 C65 1.395(4) . ?
C64 C69 1.396(4) . ?
C65 C66 1.403(4) . ?
C66 H66 0.9300 . ?
C66 C67 1.377(5) . ?
C67 H67 0.9300 . ?
C67 C68 1.382(5) . ?
C68 H68 0.9300 . ?
C68 C69 1.372(5) . ?
C69 H69 0.9300 . ?
C70 C71 1.371(5) . ?
C70 C75 1.402(5) . ?
C71 H71 0.9300 . ?
C71 C72 1.397(5) . ?
C72 H72 0.9300 . ?
C72 C73 1.388(7) . ?
C73 H73 0.9300 . ?
C73 C74 1.364(7) . ?
C74 H74 0.9300 . ?
C74 C75 1.398(5) . ?
C75 C76 1.463(5) . ?
C76 C77 1.395(6) . ?
C76 C81 1.401(5) . ?
C77 H77 0.9300 . ?
C77 C78 1.389(7) . ?
C78 H78 0.9300 . ?
C78 C79 1.375(7) . ?
C79 H79 0.9300 . ?
C79 C80 1.395(6) . ?
C80 H80 0.9300 . ?
C80 C81 1.382(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C35 O1 C36 118.6(2) . . ?
C42 O2 C40 119.4(2) . . ?
C44 O3 C45 116.7(3) . . ?
C34 O4 C49 117.5(2) . . ?
C1 N1 C22 120.0(3) . . ?
C1 N1 C27 118.5(3) . . ?
C22 N1 C27 118.7(3) . . ?
C35 N2 C33 113.5(3) . . ?
C34 N3 C35 112.0(3) . . ?
C34 N4 C33 113.7(3) . . ?
C42 N5 C44 112.2(3) . . ?
C42 N6 C43 113.1(3) . . ?
C44 N7 C43 113.1(3) . . ?
C57 N8 C54 118.6(3) . . ?
C57 N8 C65 121.9(3) . . ?
C65 N8 C54 119.3(3) . . ?
C2 C1 N1 119.1(3) . . ?
C6 C1 N1 121.6(3) . . ?
C6 C1 C2 119.2(3) . . ?
C1 C2 C3 118.7(3) . . ?
C1 C2 C7 120.2(3) . . ?
C3 C2 C7 120.8(3) . . ?
C2 C3 H3 119.1 . . ?
C4 C3 C2 121.8(3) . . ?
C4 C3 H3 119.1 . . ?
C3 C4 H4 120.7 . . ?
C5 C4 C3 118.7(4) . . ?
C5 C4 H4 120.7 . . ?
C4 C5 H5 119.8 . . ?
C4 C5 C6 120.4(4) . . ?
C6 C5 H5 119.8 . . ?
C1 C6 H6 119.5 . . ?
C5 C6 C1 121.0(3) . . ?
C5 C6 H6 119.5 . . ?
C2 C7 C8 108.1(3) . . ?
C2 C7 C21 109.4(3) . . ?
C20 C7 C2 112.2(3) . . ?
C20 C7 C8 101.4(3) . . ?
C20 C7 C21 113.1(3) . . ?
C21 C7 C8 112.4(3) . . ?
C9 C8 C7 129.1(3) . . ?
C9 C8 C13 120.5(3) . . ?
C13 C8 C7 110.4(3) . . ?
C8 C9 H9 120.6 . . ?
C10 C9 C8 118.9(4) . . ?
C10 C9 H9 120.6 . . ?
C9 C10 H10 119.3 . . ?
C9 C10 C11 121.4(4) . . ?
C11 C10 H10 119.3 . . ?
C10 C11 H11 120.2 . . ?
C12 C11 C10 119.5(4) . . ?
C12 C11 H11 120.2 . . ?
C11 C12 H12 120.2 . . ?
C11 C12 C13 119.5(4) . . ?
C13 C12 H12 120.2 . . ?
C8 C13 C15 108.7(3) . . ?
C12 C13 C8 120.2(4) . . ?
C12 C13 C15 131.1(3) . . ?
C16 C15 C13 130.8(3) . . ?
C16 C15 C20 121.0(3) . . ?
C20 C15 C13 108.2(3) . . ?
C15 C16 H16 120.9 . . ?
C17 C16 C15 118.2(4) . . ?
C17 C16 H16 120.9 . . ?
C16 C17 H17 119.3 . . ?
C16 C17 C18 121.4(3) . . ?
C18 C17 H17 119.3 . . ?
C17 C18 H18 119.4 . . ?
C17 C18 C19 121.2(4) . . ?
C19 C18 H18 119.4 . . ?
C18 C19 H19 121.0 . . ?
C20 C19 C18 118.0(4) . . ?
C20 C19 H19 121.0 . . ?
C15 C20 C7 111.2(3) . . ?
C19 C20 C7 128.5(3) . . ?
C19 C20 C15 120.3(3) . . ?
C22 C21 C7 119.8(3) . . ?
C26 C21 C7 121.8(3) . . ?
C26 C21 C22 118.4(3) . . ?
C21 C22 N1 119.6(3) . . ?
C23 C22 N1 120.7(3) . . ?
C23 C22 C21 119.7(3) . . ?
C22 C23 H23 119.8 . . ?
C24 C23 C22 120.4(3) . . ?
C24 C23 H23 119.8 . . ?
C23 C24 H24 119.9 . . ?
C23 C24 C25 120.2(3) . . ?
C25 C24 H24 119.9 . . ?
C24 C25 H25 120.1 . . ?
C26 C25 C24 119.7(3) . . ?
C26 C25 H25 120.1 . . ?
C21 C26 H26 119.2 . . ?
C25 C26 C21 121.6(3) . . ?
C25 C26 H26 119.2 . . ?
C28 C27 N1 121.0(3) . . ?
C28 C27 C32 119.5(3) . . ?
C32 C27 N1 119.4(3) . . ?
C27 C28 H28 119.7 . . ?
C27 C28 C29 120.6(3) . . ?
C29 C28 H28 119.7 . . ?
C28 C29 H29 120.1 . . ?
C28 C29 C30 119.9(3) . . ?
C30 C29 H29 120.1 . . ?
C29 C30 C33 119.9(3) . . ?
C31 C30 C29 119.6(3) . . ?
C31 C30 C33 120.5(3) . . ?
C30 C31 H31 120.3 . . ?
C32 C31 C30 119.4(3) . . ?
C32 C31 H31 120.3 . . ?
C27 C32 H32 119.6 . . ?
C31 C32 C27 120.9(3) . . ?
C31 C32 H32 119.6 . . ?
N2 C33 N4 124.9(3) . . ?
N2 C33 C30 118.9(3) . . ?
N4 C33 C30 116.2(3) . . ?
N3 C34 O4 119.1(3) . . ?
N3 C34 N4 127.7(3) . . ?
N4 C34 O4 113.2(3) . . ?
N2 C35 O1 113.6(3) . . ?
N2 C35 N3 128.1(3) . . ?
N3 C35 O1 118.3(3) . . ?
C37 C36 O1 118.7(3) . . ?
C37 C36 C41 122.3(3) . . ?
C41 C36 O1 118.9(3) . . ?
C36 C37 H37 120.4 . . ?
C36 C37 C38 119.1(3) . . ?
C38 C37 H37 120.4 . . ?
C37 C38 H38 119.8 . . ?
C39 C38 C37 120.3(3) . . ?
C39 C38 H38 119.8 . . ?
C38 C39 H39 120.7 . . ?
C40 C39 C38 118.6(3) . . ?
C40 C39 H39 120.7 . . ?
C39 C40 O2 117.9(3) . . ?
C39 C40 C41 122.7(3) . . ?
C41 C40 O2 119.1(3) . . ?
C36 C41 H41 121.5 . . ?
C40 C41 C36 116.9(3) . . ?
C40 C41 H41 121.5 . . ?
N5 C42 O2 119.5(3) . . ?
N5 C42 N6 127.9(3) . . ?
N6 C42 O2 112.6(3) . . ?
N6 C43 N7 125.6(3) . . ?
N6 C43 C51 117.9(3) . . ?
N7 C43 C51 116.5(3) . . ?
N5 C44 O3 118.0(3) . . ?
N7 C44 O3 114.1(3) . . ?
N7 C44 N5 127.9(3) . . ?
C46 C45 O3 119.5(3) . . ?
C50 C45 O3 117.9(3) . . ?
C50 C45 C46 122.5(3) . . ?
C45 C46 H46 120.8 . . ?
C45 C46 C47 118.4(3) . . ?
C47 C46 H46 120.8 . . ?
C46 C47 H47 119.5 . . ?
C46 C47 C48 121.1(3) . . ?
C48 C47 H47 119.5 . . ?
C47 C48 H48 121.0 . . ?
C49 C48 C47 118.1(3) . . ?
C49 C48 H48 121.0 . . ?
C48 C49 O4 119.0(3) . . ?
C48 C49 C50 122.9(3) . . ?
C50 C49 O4 117.9(3) . . ?
C45 C50 C49 117.1(3) . . ?
C45 C50 H50 121.5 . . ?
C49 C50 H50 121.5 . . ?
C52 C51 C43 121.0(3) . . ?
C52 C51 C56 119.7(3) . . ?
C56 C51 C43 119.3(3) . . ?
C51 C52 H52 119.9 . . ?
C51 C52 C53 120.2(3) . . ?
C53 C52 H52 119.9 . . ?
C52 C53 H53 120.0 . . ?
C54 C53 C52 120.1(3) . . ?
C54 C53 H53 120.0 . . ?
C53 C54 N8 119.6(3) . . ?
C53 C54 C55 120.4(3) . . ?
C55 C54 N8 120.0(3) . . ?
C54 C55 H55 120.0 . . ?
C54 C55 C56 120.1(3) . . ?
C56 C55 H55 120.0 . . ?
C51 C56 H56 120.3 . . ?
C55 C56 C51 119.5(3) . . ?
C55 C56 H56 120.3 . . ?
N8 C57 C58 120.3(3) . . ?
C62 C57 N8 120.6(3) . . ?
C62 C57 C58 119.1(3) . . ?
C57 C58 H58 119.6 . . ?
C59 C58 C57 120.8(3) . . ?
C59 C58 H58 119.6 . . ?
C58 C59 H59 119.6 . . ?
C60 C59 C58 120.7(3) . . ?
C60 C59 H59 119.6 . . ?
C59 C60 H60 120.5 . . ?
C59 C60 C61 119.0(3) . . ?
C61 C60 H60 120.5 . . ?
C60 C61 H61 119.1 . . ?
C60 C61 C62 121.9(3) . . ?
C62 C61 H61 119.1 . . ?
C57 C62 C63 122.3(3) . . ?
C61 C62 C57 118.5(3) . . ?
C61 C62 C63 119.2(3) . . ?
C62 C63 C70 111.1(2) . . ?
C62 C63 C81 110.5(3) . . ?
C64 C63 C62 111.8(2) . . ?
C64 C63 C70 111.4(2) . . ?
C64 C63 C81 110.6(2) . . ?
C70 C63 C81 101.0(2) . . ?
C65 C64 C63 122.8(3) . . ?
C65 C64 C69 118.1(3) . . ?
C69 C64 C63 119.1(3) . . ?
N8 C65 C66 119.8(3) . . ?
C64 C65 N8 120.3(3) . . ?
C64 C65 C66 119.9(3) . . ?
C65 C66 H66 119.8 . . ?
C67 C66 C65 120.4(3) . . ?
C67 C66 H66 119.8 . . ?
C66 C67 H67 120.0 . . ?
C66 C67 C68 120.1(3) . . ?
C68 C67 H67 120.0 . . ?
C67 C68 H68 120.2 . . ?
C69 C68 C67 119.6(3) . . ?
C69 C68 H68 120.2 . . ?
C64 C69 H69 119.0 . . ?
C68 C69 C64 122.0(3) . . ?
C68 C69 H69 119.0 . . ?
C71 C70 C63 128.4(3) . . ?
C71 C70 C75 121.4(3) . . ?
C75 C70 C63 110.2(3) . . ?
C70 C71 H71 120.7 . . ?
C70 C71 C72 118.6(4) . . ?
C72 C71 H71 120.7 . . ?
C71 C72 H72 120.0 . . ?
C73 C72 C71 120.1(4) . . ?
C73 C72 H72 120.0 . . ?
C72 C73 H73 119.3 . . ?
C74 C73 C72 121.5(4) . . ?
C74 C73 H73 119.3 . . ?
C73 C74 H74 120.5 . . ?
C73 C74 C75 119.1(4) . . ?
C75 C74 H74 120.5 . . ?
C70 C75 C76 109.7(3) . . ?
C74 C75 C70 119.4(4) . . ?
C74 C75 C76 131.0(4) . . ?
C77 C76 C75 132.9(3) . . ?
C77 C76 C81 119.3(4) . . ?
C81 C76 C75 107.8(3) . . ?
C76 C77 H77 120.3 . . ?
C78 C77 C76 119.4(4) . . ?
C78 C77 H77 120.3 . . ?
C77 C78 H78 119.6 . . ?
C79 C78 C77 120.7(4) . . ?
C79 C78 H78 119.6 . . ?
C78 C79 H79 119.7 . . ?
C78 C79 C80 120.6(4) . . ?
C80 C79 H79 119.7 . . ?
C79 C80 H80 120.5 . . ?
C81 C80 C79 118.9(4) . . ?
C81 C80 H80 120.5 . . ?
C76 C81 C63 111.3(3) . . ?
C80 C81 C63 127.7(3) . . ?
C80 C81 C76 121.0(3) . . ?

_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.706
_oxdiff_exptl_absorpt_empirical_full_min 0.605
####################################################################### 
# 
# 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_tx372b_sq
_database_code_depnum_ccdc_archive 'CCDC 1922447'
loop_
_audit_author_name
_audit_author_address
TAT-PXZ
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2019-06-12 deposited with the CCDC.	2019-07-18 downloaded from the CCDC.
;
_audit_creation_date             2019-02-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C54 H32 N8 O6'
_chemical_formula_sum            'C54 H32 N8 O6'
_chemical_formula_weight         888.87
_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           13
_space_group_name_H-M_alt        'P 1 2/c 1'
_space_group_name_Hall           '-P 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   19.6993(3)
_cell_length_b                   13.7805(2)
_cell_length_c                   17.3821(3)
_cell_angle_alpha                90
_cell_angle_beta                 92.071(2)
_cell_angle_gamma                90
_cell_volume                     4715.57(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12782
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      72.6410
_cell_measurement_theta_min      2.2320
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.60295
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.054
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33472
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         75.519
_diffrn_reflns_theta_min         2.244
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'Rotating-anode X-ray tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6632
_reflns_number_total             9395
_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 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.184
_refine_diff_density_min         -0.141
_refine_diff_density_rms         0.032
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         9395
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0644
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0909P)²+1.2784P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1927
_refine_ls_wR_factor_ref         0.2088
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 N3, C20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C17(H17), C18(H18), C23(H23), C24(H24), C25(H25), C27(H27),
  C32(H32), C33(H33), C34(H34), C36(H36), C38(H38), C39(H39), C41(H41),
 C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C51(H51), C52(H52), C53(H53),
  C54(H54)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 0.17825(12) 0.71319(17) 0.16353(13) 0.1175(7) Uani 1 1 d . . . . .
O2 O 0.61717(11) 0.69576(19) 0.58568(15) 0.1318(9) Uani 1 1 d . . . . .
O3 O 0.67366(10) 0.43806(14) 0.43179(12) 0.1035(6) Uani 1 1 d . . . . .
O4 O 0.90895(9) 0.53002(13) 0.44982(12) 0.1008(6) Uani 1 1 d . . . . .
O5 O 0.84985(10) 0.80231(14) 0.58603(11) 0.1049(7) Uani 1 1 d . . . . .
O6 O 1.28092(11) 1.05571(18) 0.22160(15) 0.1181(7) Uani 1 1 d . . . . .
N1 N 0.29957(14) 0.6499(2) 0.23633(17) 0.1134(8) Uani 1 1 d . . . . .
N2 N 0.54670(13) 0.6491(2) 0.49000(17) 0.1152(9) Uani 1 1 d . . . . .
N3 N 0.57524(13) 0.51569(18) 0.41159(15) 0.0994(7) Uani 1 1 d . U . . .
N4 N 0.65298(12) 0.56756(18) 0.51201(15) 0.1025(8) Uani 1 1 d . . . . .
N5 N 0.87301(11) 0.66147(16) 0.52052(13) 0.0903(6) Uani 1 1 d . . . . .
N6 N 0.96210(10) 0.66979(15) 0.43194(12) 0.0864(6) Uani 1 1 d . . . . .
N7 N 0.93090(10) 0.81066(15) 0.50040(12) 0.0842(6) Uani 1 1 d . . . . .
N8 N 1.17415(10) 0.97376(16) 0.30047(13) 0.0852(6) Uani 1 1 d . . . . .
C1 C 0.23730(15) 0.6088(2) 0.25639(18) 0.0969(8) Uani 1 1 d . . . . .
C2 C 0.23200(16) 0.5378(2) 0.31151(18) 0.1000(9) Uani 1 1 d . . . . .
H2 H 0.270678 0.516970 0.338987 0.120 Uiso 1 1 calc R . . . .
C3 C 0.16931(17) 0.4970(2) 0.32645(19) 0.1014(9) Uani 1 1 d . . . . .
H3 H 0.166466 0.448956 0.363805 0.122 Uiso 1 1 calc R . . . .
C4 C 0.11190(17) 0.5265(2) 0.28686(19) 0.1034(9) Uani 1 1 d . . . . .
H4 H 0.070203 0.498216 0.296475 0.124 Uiso 1 1 calc R . . . .
C5 C 0.11639(16) 0.5989(2) 0.23240(18) 0.1024(9) Uani 1 1 d . . . . .
H5 H 0.077514 0.620101 0.205456 0.123 Uiso 1 1 calc R . . . .
C6 C 0.17772(17) 0.6394(2) 0.21811(18) 0.1002(9) Uani 1 1 d . . . . .
C7 C 0.23903(19) 0.7620(2) 0.1529(2) 0.1138(11) Uani 1 1 d . . . . .
C8 C 0.30019(19) 0.7295(2) 0.1865(2) 0.1158(11) Uani 1 1 d . . . . .
C9 C 0.3594(2) 0.7761(3) 0.1671(3) 0.1348(14) Uani 1 1 d . . . . .
H9 H 0.400980 0.754720 0.187636 0.162 Uiso 1 1 calc R . . . .
C10 C 0.3568(3) 0.8551(3) 0.1170(3) 0.1558(18) Uani 1 1 d . . . . .
H10 H 0.396834 0.884866 0.102983 0.187 Uiso 1 1 calc R . . . .
C11 C 0.2963(3) 0.8888(3) 0.0886(3) 0.1561(18) Uani 1 1 d . . . . .
H11 H 0.294842 0.943768 0.057449 0.187 Uiso 1 1 calc R . . . .
C12 C 0.2363(2) 0.8415(3) 0.1058(2) 0.1299(13) Uani 1 1 d . . . . .
H12 H 0.194786 0.863649 0.085509 0.156 Uiso 1 1 calc R . . . .
C13 C 0.35858(17) 0.6335(2) 0.2873(2) 0.1097(10) Uani 1 1 d . . . . .
C14 C 0.39596(16) 0.5499(2) 0.2797(2) 0.1049(9) Uani 1 1 d . . . . .
H14 H 0.383815 0.504584 0.242055 0.126 Uiso 1 1 calc R . . . .
C15 C 0.45171(16) 0.5342(2) 0.3285(2) 0.1040(9) Uani 1 1 d . . . . .
H15 H 0.476648 0.477300 0.323999 0.125 Uiso 1 1 calc R . . . .
C16 C 0.47121(15) 0.6020(2) 0.3844(2) 0.1036(9) Uani 1 1 d . . . . .
C17 C 0.43263(19) 0.6868(3) 0.3914(2) 0.1225(12) Uani 1 1 d . . . . .
H17 H 0.444705 0.733072 0.428413 0.147 Uiso 1 1 calc R . . . .
C18 C 0.3759(2) 0.7011(3) 0.3423(3) 0.1242(12) Uani 1 1 d . . . . .
H18 H 0.349728 0.756760 0.346985 0.149 Uiso 1 1 calc R . . . .
C19 C 0.53382(15) 0.5876(2) 0.43204(19) 0.1040(10) Uani 1 1 d . . . . .
C20 C 0.63256(16) 0.5112(2) 0.45361(19) 0.0991(9) Uani 1 1 d . U . . .
C21 C 0.60610(17) 0.6347(2) 0.5269(2) 0.1115(11) Uani 1 1 d . . . . .
C22 C 0.73908(14) 0.4277(2) 0.46430(17) 0.0930(8) Uani 1 1 d . . . . .
C23 C 0.75245(16) 0.3461(2) 0.50777(18) 0.0986(9) Uani 1 1 d . . . . .
H23 H 0.717828 0.303207 0.519438 0.118 Uiso 1 1 calc R . . . .
C24 C 0.81801(17) 0.3293(2) 0.53350(19) 0.1037(9) Uani 1 1 d . . . . .
H24 H 0.827889 0.274419 0.562960 0.124 Uiso 1 1 calc R . . . .
C25 C 0.86980(15) 0.3930(2) 0.51627(18) 0.0972(8) Uani 1 1 d . . . . .
H25 H 0.914205 0.381362 0.533869 0.117 Uiso 1 1 calc R . . . .
C26 C 0.85426(14) 0.4728(2) 0.47304(17) 0.0908(8) Uani 1 1 d . . . . .
C27 C 0.78942(15) 0.4929(2) 0.44633(17) 0.0943(8) Uani 1 1 d . . . . .
H27 H 0.779704 0.548115 0.417264 0.113 Uiso 1 1 calc R . . . .
C28 C 0.91351(13) 0.62422(19) 0.46872(16) 0.0876(7) Uani 1 1 d . . . . .
C29 C 0.96779(12) 0.76400(18) 0.44936(14) 0.0778(6) Uani 1 1 d . . . . .
C30 C 0.88520(13) 0.7545(2) 0.53370(15) 0.0877(7) Uani 1 1 d . . . . .
C31 C 0.79543(16) 0.7564(2) 0.62284(18) 0.0997(9) Uani 1 1 d . . . . .
C32 C 0.80320(18) 0.7403(2) 0.70015(19) 0.1090(10) Uani 1 1 d . . . . .
H32 H 0.844288 0.752828 0.726280 0.131 Uiso 1 1 calc R . . . .
C33 C 0.7478(2) 0.7044(2) 0.7386(2) 0.1188(12) Uani 1 1 d . . . . .
H33 H 0.751879 0.691884 0.791184 0.143 Uiso 1 1 calc R . . . .
C34 C 0.68715(19) 0.6875(2) 0.6995(2) 0.1202(12) Uani 1 1 d . . . . .
H34 H 0.649943 0.664642 0.725576 0.144 Uiso 1 1 calc R . . . .
C35 C 0.68186(17) 0.7043(2) 0.6222(2) 0.1111(11) Uani 1 1 d . . . . .
C36 C 0.73563(16) 0.7401(2) 0.58141(19) 0.1055(10) Uani 1 1 d . . . . .
H36 H 0.731534 0.752464 0.528844 0.127 Uiso 1 1 calc R . . . .
C37 C 1.01973(11) 0.82026(17) 0.40874(13) 0.0721(6) Uani 1 1 d . . . . .
C38 C 1.04946(16) 0.7842(2) 0.34482(18) 0.1102(11) Uani 1 1 d . . . . .
H38 H 1.035906 0.724041 0.325496 0.132 Uiso 1 1 calc R . . . .
C39 C 1.09935(16) 0.8357(2) 0.30844(18) 0.1084(10) Uani 1 1 d . . . . .
H39 H 1.118566 0.810724 0.264544 0.130 Uiso 1 1 calc R . . . .
C40 C 1.12024(11) 0.92332(18) 0.33719(14) 0.0749(6) Uani 1 1 d . . . . .
C41 C 1.09055(13) 0.96046(19) 0.39974(15) 0.0872(7) Uani 1 1 d . . . . .
H41 H 1.104307 1.020454 0.419216 0.105 Uiso 1 1 calc R . . . .
C42 C 1.03960(12) 0.90904(19) 0.43483(15) 0.0841(7) Uani 1 1 d . . . . .
H42 H 1.018684 0.935883 0.476964 0.101 Uiso 1 1 calc R . . . .
C43 C 1.24003(12) 0.97122(18) 0.33329(17) 0.0832(7) Uani 1 1 d . . . . .
C44 C 1.25656(13) 0.9292(2) 0.40328(18) 0.0902(7) Uani 1 1 d . . . . .
H44 H 1.222500 0.900438 0.431116 0.108 Uiso 1 1 calc R . . . .
C45 C 1.32249(14) 0.9287(2) 0.4333(2) 0.1080(9) Uani 1 1 d . . . . .
H45 H 1.332292 0.899444 0.480600 0.130 Uiso 1 1 calc R . . . .
C46 C 1.37322(17) 0.9708(3) 0.3937(3) 0.1282(13) Uani 1 1 d . . . . .
H46 H 1.417499 0.971134 0.414173 0.154 Uiso 1 1 calc R . . . .
C47 C 1.35846(16) 1.0127(3) 0.3235(3) 0.1238(12) Uani 1 1 d . . . . .
H47 H 1.393014 1.041118 0.296193 0.149 Uiso 1 1 calc R . . . .
C48 C 1.29272(14) 1.0132(2) 0.2930(2) 0.0990(9) Uani 1 1 d . . . . .
C49 C 1.21496(16) 1.0673(2) 0.19504(16) 0.0948(8) Uani 1 1 d . . . . .
C50 C 1.16095(14) 1.0267(2) 0.23362(15) 0.0862(7) Uani 1 1 d . . . . .
C51 C 1.09592(16) 1.0428(3) 0.20404(18) 0.1114(10) Uani 1 1 d . . . . .
H51 H 1.059198 1.015502 0.228342 0.134 Uiso 1 1 calc R . . . .
C52 C 1.0846(2) 1.0985(4) 0.1391(2) 0.1504(17) Uani 1 1 d . . . . .
H52 H 1.040595 1.109361 0.119905 0.180 Uiso 1 1 calc R . . . .
C53 C 1.1392(3) 1.1383(4) 0.1026(2) 0.1530(17) Uani 1 1 d . . . . .
H53 H 1.131862 1.176383 0.058903 0.184 Uiso 1 1 calc R . . . .
C54 C 1.2041(2) 1.1219(3) 0.13041(19) 0.1258(13) Uani 1 1 d . . . . .
H54 H 1.240778 1.147980 0.105234 0.151 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C6 1.391(4) . ?
O1 C7 1.392(4) . ?
O2 C21 1.336(4) . ?
O2 C35 1.408(4) . ?
O3 C20 1.355(3) . ?
O3 C22 1.396(4) . ?
O4 C26 1.406(3) . ?
O4 C28 1.341(3) . ?
O5 C30 1.339(3) . ?
O5 C31 1.417(3) . ?
O6 C48 1.384(4) . ?
O6 C49 1.372(4) . ?
N1 C1 1.406(3) . ?
N1 C8 1.398(4) . ?
N1 C13 1.454(5) . ?
N2 C19 1.334(4) . ?
N2 C21 1.329(5) . ?
N3 C19 1.340(4) . ?
N3 C20 1.324(4) . ?
N4 C20 1.329(4) . ?
N4 C21 1.339(4) . ?
N5 C28 1.328(3) . ?
N5 C30 1.323(3) . ?
N6 C28 1.328(3) . ?
N6 C29 1.337(3) . ?
N7 C29 1.332(3) . ?
N7 C30 1.335(3) . ?
N8 C40 1.438(3) . ?
N8 C43 1.399(3) . ?
N8 C50 1.389(3) . ?
C1 C2 1.376(4) . ?
C1 C6 1.393(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.390(4) . ?
C3 H3 0.9300 . ?
C3 C4 1.365(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.381(4) . ?
C5 H5 0.9300 . ?
C5 C6 1.362(4) . ?
C7 C8 1.393(5) . ?
C7 C12 1.367(5) . ?
C8 C9 1.383(4) . ?
C9 H9 0.9300 . ?
C9 C10 1.394(6) . ?
C10 H10 0.9300 . ?
C10 C11 1.356(7) . ?
C11 H11 0.9300 . ?
C11 C12 1.392(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.376(4) . ?
C13 C18 1.369(5) . ?
C14 H14 0.9300 . ?
C14 C15 1.381(5) . ?
C15 H15 0.9300 . ?
C15 C16 1.391(4) . ?
C16 C17 1.402(5) . ?
C16 C19 1.474(5) . ?
C17 H17 0.9300 . ?
C17 C18 1.395(6) . ?
C18 H18 0.9300 . ?
C22 C23 1.375(4) . ?
C22 C27 1.382(3) . ?
C23 H23 0.9300 . ?
C23 C24 1.371(4) . ?
C24 H24 0.9300 . ?
C24 C25 1.387(4) . ?
C25 H25 0.9300 . ?
C25 C26 1.361(4) . ?
C26 C27 1.371(4) . ?
C27 H27 0.9300 . ?
C29 C37 1.483(3) . ?
C31 C32 1.365(5) . ?
C31 C36 1.377(4) . ?
C32 H32 0.9300 . ?
C32 C33 1.391(4) . ?
C33 H33 0.9300 . ?
C33 C34 1.373(5) . ?
C34 H34 0.9300 . ?
C34 C35 1.365(5) . ?
C35 C36 1.386(4) . ?
C36 H36 0.9300 . ?
C37 C38 1.368(3) . ?
C37 C42 1.357(3) . ?
C38 H38 0.9300 . ?
C38 C39 1.384(3) . ?
C39 H39 0.9300 . ?
C39 C40 1.364(4) . ?
C40 C41 1.354(3) . ?
C41 H41 0.9300 . ?
C41 C42 1.388(3) . ?
C42 H42 0.9300 . ?
C43 C44 1.376(4) . ?
C43 C48 1.398(3) . ?
C44 H44 0.9300 . ?
C44 C45 1.382(4) . ?
C45 H45 0.9300 . ?
C45 C46 1.363(5) . ?
C46 H46 0.9300 . ?
C46 C47 1.372(5) . ?
C47 H47 0.9300 . ?
C47 C48 1.382(5) . ?
C49 C50 1.395(3) . ?
C49 C54 1.363(5) . ?
C50 C51 1.381(4) . ?
C51 H51 0.9300 . ?
C51 C52 1.378(5) . ?
C52 H52 0.9300 . ?
C52 C53 1.381(5) . ?
C53 H53 0.9300 . ?
C53 C54 1.370(6) . ?
C54 H54 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
C6 O1 C7 118.1(3) . . ?
C21 O2 C35 121.2(3) . . ?
C20 O3 C22 121.0(2) . . ?
C28 O4 C26 121.16(18) . . ?
C30 O5 C31 120.50(19) . . ?
C49 O6 C48 118.5(2) . . ?
C1 N1 C13 118.1(3) . . ?
C8 N1 C1 119.8(3) . . ?
C8 N1 C13 118.4(3) . . ?
C21 N2 C19 114.2(3) . . ?
C20 N3 C19 113.8(3) . . ?
C20 N4 C21 111.1(3) . . ?
C30 N5 C28 112.48(19) . . ?
C28 N6 C29 114.0(2) . . ?
C29 N7 C30 113.7(2) . . ?
C43 N8 C40 119.7(2) . . ?
C50 N8 C40 120.4(2) . . ?
C50 N8 C43 119.8(2) . . ?
C2 C1 N1 123.2(3) . . ?
C2 C1 C6 117.6(3) . . ?
C6 C1 N1 119.2(3) . . ?
C1 C2 H2 119.7 . . ?
C1 C2 C3 120.6(3) . . ?
C3 C2 H2 119.7 . . ?
C2 C3 H3 119.7 . . ?
C4 C3 C2 120.7(3) . . ?
C4 C3 H3 119.7 . . ?
C3 C4 H4 120.4 . . ?
C3 C4 C5 119.3(3) . . ?
C5 C4 H4 120.4 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 C4 120.0(3) . . ?
C6 C5 H5 120.0 . . ?
O1 C6 C1 121.3(3) . . ?
C5 C6 O1 116.9(3) . . ?
C5 C6 C1 121.8(3) . . ?
O1 C7 C8 121.6(3) . . ?
C12 C7 O1 116.8(4) . . ?
C12 C7 C8 121.6(3) . . ?
C7 C8 N1 119.0(3) . . ?
C9 C8 N1 122.8(4) . . ?
C9 C8 C7 118.2(4) . . ?
C8 C9 H9 119.9 . . ?
C8 C9 C10 120.2(4) . . ?
C10 C9 H9 119.9 . . ?
C9 C10 H10 119.7 . . ?
C11 C10 C9 120.5(4) . . ?
C11 C10 H10 119.7 . . ?
C10 C11 H11 119.9 . . ?
C10 C11 C12 120.2(4) . . ?
C12 C11 H11 119.9 . . ?
C7 C12 C11 119.3(4) . . ?
C7 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C14 C13 N1 119.4(3) . . ?
C18 C13 N1 119.6(3) . . ?
C18 C13 C14 121.1(4) . . ?
C13 C14 H14 120.4 . . ?
C13 C14 C15 119.3(3) . . ?
C15 C14 H14 120.4 . . ?
C14 C15 H15 119.4 . . ?
C14 C15 C16 121.1(3) . . ?
C16 C15 H15 119.4 . . ?
C15 C16 C17 118.9(4) . . ?
C15 C16 C19 120.4(3) . . ?
C17 C16 C19 120.5(3) . . ?
C16 C17 H17 120.4 . . ?
C18 C17 C16 119.2(3) . . ?
C18 C17 H17 120.4 . . ?
C13 C18 C17 120.4(3) . . ?
C13 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
N2 C19 N3 124.7(3) . . ?
N2 C19 C16 118.1(3) . . ?
N3 C19 C16 117.1(3) . . ?
N3 C20 O3 112.8(3) . . ?
N3 C20 N4 128.5(3) . . ?
N4 C20 O3 118.7(3) . . ?
O2 C21 N4 119.2(3) . . ?
N2 C21 O2 113.1(3) . . ?
N2 C21 N4 127.7(3) . . ?
C23 C22 O3 117.5(2) . . ?
C23 C22 C27 122.1(3) . . ?
C27 C22 O3 120.1(3) . . ?
C22 C23 H23 120.8 . . ?
C24 C23 C22 118.5(3) . . ?
C24 C23 H23 120.8 . . ?
C23 C24 H24 119.5 . . ?
C23 C24 C25 121.0(3) . . ?
C25 C24 H24 119.5 . . ?
C24 C25 H25 120.7 . . ?
C26 C25 C24 118.6(3) . . ?
C26 C25 H25 120.7 . . ?
C25 C26 O4 116.9(3) . . ?
C25 C26 C27 122.5(2) . . ?
C27 C26 O4 120.3(3) . . ?
C22 C27 H27 121.3 . . ?
C26 C27 C22 117.4(3) . . ?
C26 C27 H27 121.3 . . ?
N5 C28 O4 120.2(2) . . ?
N5 C28 N6 127.2(2) . . ?
N6 C28 O4 112.5(2) . . ?
N6 C29 C37 117.0(2) . . ?
N7 C29 N6 125.2(2) . . ?
N7 C29 C37 117.9(2) . . ?
N5 C30 O5 119.9(2) . . ?
N5 C30 N7 127.4(2) . . ?
N7 C30 O5 112.6(2) . . ?
C32 C31 O5 117.2(3) . . ?
C32 C31 C36 123.5(3) . . ?
C36 C31 O5 118.9(3) . . ?
C31 C32 H32 121.0 . . ?
C31 C32 C33 118.0(3) . . ?
C33 C32 H32 121.0 . . ?
C32 C33 H33 119.8 . . ?
C34 C33 C32 120.4(3) . . ?
C34 C33 H33 119.8 . . ?
C33 C34 H34 120.2 . . ?
C35 C34 C33 119.5(3) . . ?
C35 C34 H34 120.2 . . ?
C34 C35 O2 117.7(3) . . ?
C34 C35 C36 122.1(3) . . ?
C36 C35 O2 119.7(3) . . ?
C31 C36 C35 116.5(3) . . ?
C31 C36 H36 121.8 . . ?
C35 C36 H36 121.8 . . ?
C38 C37 C29 121.3(2) . . ?
C42 C37 C29 120.5(2) . . ?
C42 C37 C38 118.2(2) . . ?
C37 C38 H38 119.4 . . ?
C37 C38 C39 121.1(3) . . ?
C39 C38 H38 119.4 . . ?
C38 C39 H39 120.1 . . ?
C40 C39 C38 119.8(2) . . ?
C40 C39 H39 120.1 . . ?
C39 C40 N8 118.9(2) . . ?
C41 C40 N8 121.4(2) . . ?
C41 C40 C39 119.7(2) . . ?
C40 C41 H41 120.0 . . ?
C40 C41 C42 120.0(2) . . ?
C42 C41 H41 120.0 . . ?
C37 C42 C41 121.2(2) . . ?
C37 C42 H42 119.4 . . ?
C41 C42 H42 119.4 . . ?
C44 C43 N8 123.9(2) . . ?
C44 C43 C48 117.4(3) . . ?
C48 C43 N8 118.7(3) . . ?
C43 C44 H44 119.2 . . ?
C43 C44 C45 121.7(3) . . ?
C45 C44 H44 119.2 . . ?
C44 C45 H45 119.9 . . ?
C46 C45 C44 120.2(4) . . ?
C46 C45 H45 119.9 . . ?
C45 C46 H46 120.3 . . ?
C45 C46 C47 119.5(3) . . ?
C47 C46 H46 120.3 . . ?
C46 C47 H47 119.7 . . ?
C46 C47 C48 120.6(3) . . ?
C48 C47 H47 119.7 . . ?
O6 C48 C43 121.4(3) . . ?
C47 C48 O6 118.1(3) . . ?
C47 C48 C43 120.6(3) . . ?
O6 C49 C50 121.4(3) . . ?
C54 C49 O6 117.4(3) . . ?
C54 C49 C50 121.2(3) . . ?
N8 C50 C49 119.3(3) . . ?
C51 C50 N8 122.6(2) . . ?
C51 C50 C49 118.1(3) . . ?
C50 C51 H51 119.5 . . ?
C52 C51 C50 121.0(3) . . ?
C52 C51 H51 119.5 . . ?
C51 C52 H52 120.2 . . ?
C51 C52 C53 119.5(4) . . ?
C53 C52 H52 120.2 . . ?
C52 C53 H53 119.8 . . ?
C54 C53 C52 120.3(4) . . ?
C54 C53 H53 119.8 . . ?
C49 C54 C53 119.9(3) . . ?
C49 C54 H54 120.0 . . ?
C53 C54 H54 120.0 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
