# Supplementary Information (SI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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_1_DCM_pentane
_database_code_depnum_ccdc_archive 'CCDC 2373363'
loop_
_audit_author_name
_audit_author_address
'Nicholas White'
;Australian National University
Australia
;
_audit_update_record             
;
2024-07-25 deposited with the CCDC.	2025-02-05 downloaded from the CCDC.
;
#==============================================================================
_audit_creation_date             2023-05-25
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C52 H46 N12, 2(C H2 Cl2)'
_chemical_formula_sum            'C54 H50 Cl4 N12'
_chemical_formula_weight         1008.86
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C60 H60 N12 Cl1 '
_chemical_oxdiff_usercomment     'jns261 nbu4cl'
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'
Cl Cl 0.3639 0.7018 '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'

_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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   11.57630(10)
_cell_length_b                   18.4127(2)
_cell_length_c                   24.1317(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.2280(10)
_cell_angle_gamma                90
_cell_volume                     5007.22(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9449
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      70.7310
_cell_measurement_theta_min      4.5870
_shelx_estimated_absorpt_T_max   0.785
_shelx_estimated_absorpt_T_min   0.568
_exptl_absorpt_coefficient_mu    2.550
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.689
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2104
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 -15 0.0642
1 0 15 0.0313
5 8 3 0.0447
4 -10 -1 0.0636
-7 -10 4 0.1119
-7 2 -1 0.1022
1 12 2 0.0524

_exptl_crystal_preparation       
'Crystals grown by vapour diffusion of n-pentane into dichloromethane solution.'
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.0000 0.0001 -15.0000 0.6378 0.6456 -0.4739
1.0000 -0.0001 15.0000 -0.6378 -0.6456 0.4739
4.9999 7.7001 3.0005 -0.3693 0.3083 0.8666
4.0001 -10.0000 -1.0004 0.6863 -0.6381 0.3299
-7.0999 -10.1001 3.8993 0.1171 -0.7299 -1.0300
-7.0000 2.0000 -1.0001 -0.2822 0.2465 -0.9142
0.9999 12.0001 2.0006 -0.6735 0.6682 0.3903

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0131
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            13491
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.594
_diffrn_reflns_theta_max         66.594
_diffrn_reflns_theta_min         3.763
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -55.00  33.00   1.00    4.00    --  -36.03  38.00   0.00   88
  2  ω    -98.00  19.00   1.00    4.00    --  -36.03   0.00 150.00  117
  3  ω    -84.00 -26.00   1.00    4.00    --  -36.03 125.00-180.00   58
  4  ω     27.00  87.00   1.00    4.00    --   36.03-125.00  90.00   60
  5  ω     -6.00  63.00   1.00    4.00    --   36.03 -77.00 120.00   69
  6  ω    110.00 153.00   1.00   16.00    --  105.15  61.00 -90.00   43
  7  ω     41.00  98.00   1.00   16.00    --  105.15 -45.00  60.00   57
  8  ω     47.00 163.00   1.00   16.00    --  105.15   0.00 -90.00  116
  9  ω     37.00 119.00   1.00   16.00    --  105.15 -45.00-150.00   82
 10  ω     39.00 122.00   1.00   16.00    --  105.15 -45.00 120.00   83
 11  ω     60.00 109.00   1.00   16.00    --  105.15-111.00-150.00   49
 12  ω     39.00 121.00   1.00   16.00    --  105.15 -45.00 -30.00   82
 13  ω     40.00 109.00   1.00   16.00    --  105.15-111.00  30.00   69
 14  ω     51.00 104.00   1.00   16.00    --  105.15 -95.00  90.00   53
 15  ω    107.00 169.00   1.00   16.00    --  105.15  77.00 120.00   62
 16  ω     52.00 132.00   1.00   16.00    --  105.15 -77.00-150.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0320241000
_diffrn_orient_matrix_UB_12      -0.0513492000
_diffrn_orient_matrix_UB_13      -0.0446562000
_diffrn_orient_matrix_UB_21      -0.0109823000
_diffrn_orient_matrix_UB_22      0.0636528000
_diffrn_orient_matrix_UB_23      -0.0423047000
_diffrn_orient_matrix_UB_31      0.1324027000
_diffrn_orient_matrix_UB_32      0.0176988000
_diffrn_orient_matrix_UB_33      0.0227695000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4156
_reflns_number_total             4415
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4415
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0343
_refine_ls_restrained_S_all      1.061
_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)+(0.0452P)²+4.8747P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0914
_refine_special_details          
'The main molecule is generally well behaved, but shows a high Ueq(max)/Ueq(min) ratio for carbon atoms due to minor disorder of the benzyl rings. This behaviour could not be adequately modelled.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C13(H13A,H13B), C20(H20A,H20B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C10(H10), C12(H12), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19),
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_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
Cl1 Cl 0.56481(4) 0.05906(3) 1.06033(2) 0.04808(14) Uani 1 1 d . . . . .
Cl2 Cl 0.73637(5) 0.09647(3) 0.99356(3) 0.05764(16) Uani 1 1 d . . . . .
C27 C 0.69539(16) 0.03231(10) 1.03978(8) 0.0434(4) Uani 1 1 d . . . . .
H27A H 0.760669 0.026930 1.074093 0.052 Uiso 1 1 calc R U . . .
H27B H 0.682379 -0.015441 1.020505 0.052 Uiso 1 1 calc R U . . .
N1 N 0.78768(11) 0.25643(6) 0.85078(5) 0.0255(3) Uani 1 1 d . . . . .
N2 N 0.72354(11) 0.22576(7) 0.88288(6) 0.0280(3) Uani 1 1 d . . . . .
N3 N 0.63544(10) 0.27196(6) 0.88569(5) 0.0229(3) Uani 1 1 d . . . . .
N4 N 0.52465(10) 0.48124(6) 0.67299(5) 0.0207(2) Uani 1 1 d . . . . .
N5 N 0.45147(10) 0.52806(6) 0.64211(5) 0.0224(3) Uani 1 1 d . . . . .
N6 N 0.51597(10) 0.58692(6) 0.63588(5) 0.0195(2) Uani 1 1 d . . . . .
C1 C 0.93644(11) 0.42588(7) 0.75288(5) 0.0174(3) Uani 1 1 d . . . . .
C2 C 0.90413(11) 0.37554(7) 0.79046(5) 0.0178(3) Uani 1 1 d . . . . .
C3 C 0.78465(11) 0.37233(7) 0.79436(5) 0.0175(3) Uani 1 1 d . . . . .
C4 C 0.70236(11) 0.41815(7) 0.76042(6) 0.0176(3) Uani 1 1 d . . . . .
H4 H 0.621759 0.415558 0.762944 0.021 Uiso 1 1 calc R U . . .
C5 C 0.73396(11) 0.46775(7) 0.72283(5) 0.0172(3) Uani 1 1 d . . . . .
C6 C 0.85331(11) 0.47297(7) 0.71931(5) 0.0181(3) Uani 1 1 d . . . . .
C7 C 0.99611(12) 0.32575(8) 0.82520(6) 0.0245(3) Uani 1 1 d . . . . .
H7A H 0.991169 0.278022 0.806834 0.037 Uiso 1 1 calc R U . . .
H7B H 0.981720 0.320522 0.863476 0.037 Uiso 1 1 calc R U . . .
H7C H 1.075300 0.346302 0.827908 0.037 Uiso 1 1 calc R U . . .
C8 C 0.89227(12) 0.52647(8) 0.67994(7) 0.0268(3) Uani 1 1 d . . . . .
H8A H 0.832305 0.528836 0.643997 0.040 Uiso 1 1 calc R U . . .
H8B H 0.968148 0.510757 0.672452 0.040 Uiso 1 1 calc R U . . .
H8C H 0.901691 0.574584 0.697761 0.040 Uiso 1 1 calc R U . . .
C9 C 0.73997(12) 0.32268(7) 0.83287(6) 0.0188(3) Uani 1 1 d . . . . .
C10 C 0.64166(12) 0.33227(7) 0.85515(6) 0.0217(3) Uani 1 1 d . . . . .
H10 H 0.589483 0.372791 0.850042 0.026 Uiso 1 1 calc R U . . .
C11 C 0.63668(11) 0.51008(7) 0.68684(5) 0.0171(3) Uani 1 1 d . . . . .
C12 C 0.63089(12) 0.57812(7) 0.66263(6) 0.0207(3) Uani 1 1 d . . . . .
H12 H 0.694095 0.611575 0.664381 0.025 Uiso 1 1 calc R U . . .
C13 C 0.54378(13) 0.25136(8) 0.91597(7) 0.0273(3) Uani 1 1 d . . . . .
H13A H 0.514341 0.295513 0.931693 0.033 Uiso 1 1 calc R U . . .
H13B H 0.579180 0.219129 0.948230 0.033 Uiso 1 1 calc R U . . .
C14 C 0.44099(13) 0.21290(8) 0.87742(6) 0.0254(3) Uani 1 1 d . . . . .
C15 C 0.42575(14) 0.13835(8) 0.88211(7) 0.0291(3) Uani 1 1 d . . . . .
H15 H 0.479999 0.111460 0.910139 0.035 Uiso 1 1 calc R U . . .
C16 C 0.33196(15) 0.10306(9) 0.84617(7) 0.0352(4) Uani 1 1 d . . . . .
H16 H 0.322193 0.052168 0.849712 0.042 Uiso 1 1 calc R U . . .
C17 C 0.25280(15) 0.14159(10) 0.80531(7) 0.0363(4) Uani 1 1 d . . . . .
H17 H 0.188630 0.117264 0.780734 0.044 Uiso 1 1 calc R U . . .
C18 C 0.26693(15) 0.21570(10) 0.80013(7) 0.0395(4) Uani 1 1 d . . . . .
H18 H 0.212631 0.242206 0.771863 0.047 Uiso 1 1 calc R U . . .
C19 C 0.36024(15) 0.25137(9) 0.83615(7) 0.0350(4) Uani 1 1 d . . . . .
H19 H 0.369138 0.302346 0.832669 0.042 Uiso 1 1 calc R U . . .
C20 C 0.45916(13) 0.65084(7) 0.60494(6) 0.0229(3) Uani 1 1 d . . . . .
H20A H 0.520337 0.688213 0.604343 0.027 Uiso 1 1 calc R U . . .
H20B H 0.401745 0.671382 0.625443 0.027 Uiso 1 1 calc R U . . .
C21 C 0.39536(12) 0.63357(7) 0.54462(6) 0.0212(3) Uani 1 1 d . . . . .
C22 C 0.28216(14) 0.66066(8) 0.52353(7) 0.0306(3) Uani 1 1 d . . . . .
H22 H 0.243787 0.687988 0.547493 0.037 Uiso 1 1 calc R U . . .
C23 C 0.22481(17) 0.64768(10) 0.46707(8) 0.0466(5) Uani 1 1 d . . . . .
H23 H 0.147603 0.666733 0.452396 0.056 Uiso 1 1 calc R U . . .
C24 C 0.2798(2) 0.60727(10) 0.43243(8) 0.0537(6) Uani 1 1 d . . . . .
H24 H 0.240564 0.598620 0.393905 0.064 Uiso 1 1 calc R U . . .
C25 C 0.3908(2) 0.57965(10) 0.45362(8) 0.0503(5) Uani 1 1 d . . . . .
H25 H 0.428234 0.551313 0.429840 0.060 Uiso 1 1 calc R U . . .
C26 C 0.44894(16) 0.59276(9) 0.50947(7) 0.0344(4) Uani 1 1 d . . . . .
H26 H 0.526203 0.573589 0.523770 0.041 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C27 1.7654(19) . ?
Cl2 C27 1.763(2) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
N1 N2 1.3165(17) . ?
N1 C9 1.3678(18) . ?
N2 N3 1.3417(17) . ?
N3 C10 1.3438(18) . ?
N3 C13 1.4693(18) . ?
N4 N5 1.3142(16) . ?
N4 C11 1.3702(17) . ?
N5 N6 1.3439(16) . ?
N6 C12 1.3490(18) . ?
N6 C20 1.4663(17) . ?
C1 C1 1.509(2) 2_756 ?
C1 C2 1.4060(19) . ?
C1 C6 1.4062(19) . ?
C2 C3 1.4088(18) . ?
C2 C7 1.5063(18) . ?
C3 C4 1.3903(18) . ?
C3 C9 1.4788(18) . ?
C4 H4 0.9500 . ?
C4 C5 1.3939(19) . ?
C5 C6 1.4068(18) . ?
C5 C11 1.4772(18) . ?
C6 C8 1.5075(19) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.3769(19) . ?
C10 H10 0.9500 . ?
C11 C12 1.3774(19) . ?
C12 H12 0.9500 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.509(2) . ?
C14 C15 1.392(2) . ?
C14 C19 1.393(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.386(2) . ?
C16 H16 0.9500 . ?
C16 C17 1.379(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.383(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.387(3) . ?
C19 H19 0.9500 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.5078(19) . ?
C21 C22 1.386(2) . ?
C21 C26 1.382(2) . ?
C22 H22 0.9500 . ?
C22 C23 1.393(2) . ?
C23 H23 0.9500 . ?
C23 C24 1.378(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.369(3) . ?
C25 H25 0.9500 . ?
C25 C26 1.383(3) . ?
C26 H26 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 C27 H27A 109.4 . . ?
Cl1 C27 H27B 109.4 . . ?
Cl2 C27 Cl1 111.26(10) . . ?
Cl2 C27 H27A 109.4 . . ?
Cl2 C27 H27B 109.4 . . ?
H27A C27 H27B 108.0 . . ?
N2 N1 C9 109.09(11) . . ?
N1 N2 N3 107.19(11) . . ?
N2 N3 C10 111.07(11) . . ?
N2 N3 C13 120.36(11) . . ?
C10 N3 C13 128.43(12) . . ?
N5 N4 C11 109.60(11) . . ?
N4 N5 N6 106.85(10) . . ?
N5 N6 C12 111.22(11) . . ?
N5 N6 C20 120.55(11) . . ?
C12 N6 C20 128.19(12) . . ?
C2 C1 C1 117.92(11) . 2_756 ?
C2 C1 C6 122.01(12) . . ?
C6 C1 C1 120.00(11) . 2_756 ?
C1 C2 C3 118.74(12) . . ?
C1 C2 C7 120.12(12) . . ?
C3 C2 C7 121.14(12) . . ?
C2 C3 C9 123.90(12) . . ?
C4 C3 C2 119.09(12) . . ?
C4 C3 C9 117.01(12) . . ?
C3 C4 H4 118.8 . . ?
C3 C4 C5 122.31(12) . . ?
C5 C4 H4 118.8 . . ?
C4 C5 C6 119.45(12) . . ?
C4 C5 C11 116.74(12) . . ?
C6 C5 C11 123.75(12) . . ?
C1 C6 C5 118.37(12) . . ?
C1 C6 C8 120.13(12) . . ?
C5 C6 C8 121.49(12) . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 C3 125.17(12) . . ?
N1 C9 C10 107.52(12) . . ?
C10 C9 C3 127.25(12) . . ?
N3 C10 C9 105.12(12) . . ?
N3 C10 H10 127.4 . . ?
C9 C10 H10 127.4 . . ?
N4 C11 C5 119.38(11) . . ?
N4 C11 C12 107.31(11) . . ?
C12 C11 C5 133.30(12) . . ?
N6 C12 C11 105.02(12) . . ?
N6 C12 H12 127.5 . . ?
C11 C12 H12 127.5 . . ?
N3 C13 H13A 109.3 . . ?
N3 C13 H13B 109.3 . . ?
N3 C13 C14 111.83(12) . . ?
H13A C13 H13B 107.9 . . ?
C14 C13 H13A 109.3 . . ?
C14 C13 H13B 109.3 . . ?
C15 C14 C13 120.62(14) . . ?
C15 C14 C19 118.87(15) . . ?
C19 C14 C13 120.50(14) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 C14 120.46(15) . . ?
C16 C15 H15 119.8 . . ?
C15 C16 H16 119.9 . . ?
C17 C16 C15 120.22(16) . . ?
C17 C16 H16 119.9 . . ?
C16 C17 H17 120.0 . . ?
C16 C17 C18 119.94(16) . . ?
C18 C17 H17 120.0 . . ?
C17 C18 H18 119.9 . . ?
C17 C18 C19 120.12(16) . . ?
C19 C18 H18 119.9 . . ?
C14 C19 H19 119.8 . . ?
C18 C19 C14 120.40(15) . . ?
C18 C19 H19 119.8 . . ?
N6 C20 H20A 109.1 . . ?
N6 C20 H20B 109.1 . . ?
N6 C20 C21 112.70(11) . . ?
H20A C20 H20B 107.8 . . ?
C21 C20 H20A 109.1 . . ?
C21 C20 H20B 109.1 . . ?
C22 C21 C20 119.47(13) . . ?
C26 C21 C20 121.18(13) . . ?
C26 C21 C22 119.33(14) . . ?
C21 C22 H22 120.1 . . ?
C21 C22 C23 119.77(17) . . ?
C23 C22 H22 120.1 . . ?
C22 C23 H23 119.9 . . ?
C24 C23 C22 120.20(17) . . ?
C24 C23 H23 119.9 . . ?
C23 C24 H24 120.0 . . ?
C25 C24 C23 119.90(16) . . ?
C25 C24 H24 120.0 . . ?
C24 C25 H25 119.8 . . ?
C24 C25 C26 120.33(18) . . ?
C26 C25 H25 119.8 . . ?
C21 C26 C25 120.45(17) . . ?
C21 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 N2 N3 C10 0.48(17) . . . . ?
N1 N2 N3 C13 176.40(12) . . . . ?
N1 C9 C10 N3 0.53(16) . . . . ?
N2 N1 C9 C3 -177.71(13) . . . . ?
N2 N1 C9 C10 -0.26(16) . . . . ?
N2 N3 C10 C9 -0.63(16) . . . . ?
N2 N3 C13 C14 -88.90(16) . . . . ?
N3 C13 C14 C15 106.37(15) . . . . ?
N3 C13 C14 C19 -73.09(17) . . . . ?
N4 N5 N6 C12 0.14(15) . . . . ?
N4 N5 N6 C20 -177.78(12) . . . . ?
N4 C11 C12 N6 0.41(15) . . . . ?
N5 N4 C11 C5 178.50(11) . . . . ?
N5 N4 C11 C12 -0.35(15) . . . . ?
N5 N6 C12 C11 -0.34(15) . . . . ?
N5 N6 C20 C21 -58.08(17) . . . . ?
N6 C20 C21 C22 134.44(14) . . . . ?
N6 C20 C21 C26 -47.26(18) . . . . ?
C1 C1 C2 C3 -176.97(12) 2_756 . . . ?
C1 C1 C2 C7 2.40(19) 2_756 . . . ?
C1 C1 C6 C5 175.44(11) 2_756 . . . ?
C1 C1 C6 C8 -3.45(19) 2_756 . . . ?
C1 C2 C3 C4 0.93(19) . . . . ?
C1 C2 C3 C9 -178.98(12) . . . . ?
C2 C1 C6 C5 -1.57(19) . . . . ?
C2 C1 C6 C8 179.53(13) . . . . ?
C2 C3 C4 C5 -0.5(2) . . . . ?
C2 C3 C9 N1 -28.8(2) . . . . ?
C2 C3 C9 C10 154.22(14) . . . . ?
C3 C4 C5 C6 -1.0(2) . . . . ?
C3 C4 C5 C11 176.48(12) . . . . ?
C3 C9 C10 N3 177.91(13) . . . . ?
C4 C3 C9 N1 151.25(13) . . . . ?
C4 C3 C9 C10 -25.7(2) . . . . ?
C4 C5 C6 C1 1.98(19) . . . . ?
C4 C5 C6 C8 -179.13(13) . . . . ?
C4 C5 C11 N4 -27.42(18) . . . . ?
C4 C5 C11 C12 151.08(15) . . . . ?
C5 C11 C12 N6 -178.22(14) . . . . ?
C6 C1 C2 C3 0.11(19) . . . . ?
C6 C1 C2 C7 179.47(12) . . . . ?
C6 C5 C11 N4 149.94(13) . . . . ?
C6 C5 C11 C12 -31.6(2) . . . . ?
C7 C2 C3 C4 -178.43(12) . . . . ?
C7 C2 C3 C9 1.7(2) . . . . ?
C9 N1 N2 N3 -0.12(16) . . . . ?
C9 C3 C4 C5 179.42(12) . . . . ?
C10 N3 C13 C14 86.24(18) . . . . ?
C11 N4 N5 N6 0.14(15) . . . . ?
C11 C5 C6 C1 -175.31(12) . . . . ?
C11 C5 C6 C8 3.6(2) . . . . ?
C12 N6 C20 C21 124.39(15) . . . . ?
C13 N3 C10 C9 -176.14(13) . . . . ?
C13 C14 C15 C16 -179.26(14) . . . . ?
C13 C14 C19 C18 178.94(15) . . . . ?
C14 C15 C16 C17 0.1(2) . . . . ?
C15 C14 C19 C18 -0.5(2) . . . . ?
C15 C16 C17 C18 0.0(2) . . . . ?
C16 C17 C18 C19 -0.3(3) . . . . ?
C17 C18 C19 C14 0.6(3) . . . . ?
C19 C14 C15 C16 0.2(2) . . . . ?
C20 N6 C12 C11 177.37(13) . . . . ?
C20 C21 C22 C23 177.11(14) . . . . ?
C20 C21 C26 C25 -177.64(16) . . . . ?
C21 C22 C23 C24 0.8(3) . . . . ?
C22 C21 C26 C25 0.7(2) . . . . ?
C22 C23 C24 C25 0.2(3) . . . . ?
C23 C24 C25 C26 -0.8(3) . . . . ?
C24 C25 C26 C21 0.3(3) . . . . ?
C26 C21 C22 C23 -1.2(2) . . . . ?


_ins_header                      
;
TITL jns2203 in C2/c 
REM C2/c (#15 in standard setting)
CELL 1.54184  11.576268  18.412665  24.131717  90.0000 103.2284  90.0000
ZERR    4.00   0.000112   0.000177   0.000254   0.0000   0.0010   0.0000
LATT  7
SYMM -x, y,-z+1/2 
SFAC C H N Cl
UNIT 240.00 240.00 48.00 4.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
SIZE 0.10 0.18 0.25
TREF
HKLF 4
END
;
_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 1.273
_oxdiff_exptl_absorpt_empirical_full_min 0.854
####################################################################### 
# 
# 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_1_workup
_database_code_depnum_ccdc_archive 'CCDC 2373364'
loop_
_audit_author_name
_audit_author_address
'Nicholas White'
;Australian National University
Australia
;
_audit_update_record             
;
2024-07-25 deposited with the CCDC.	2025-02-05 downloaded from the CCDC.
;
#==============================================================================
_audit_creation_date             2023-06-01
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C52 H46 N12'
_chemical_formula_sum            'C52 H46 N12'
_chemical_formula_weight         839.01
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C60 H75 N8'
_chemical_oxdiff_usercomment     jns261
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'

_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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   11.4546(5)
_cell_length_b                   18.6173(7)
_cell_length_c                   24.6098(12)
_cell_angle_alpha                90
_cell_angle_beta                 100.265(4)
_cell_angle_gamma                90
_cell_volume                     5164.1(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1858
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      63.5380
_cell_measurement_theta_min      4.6520
_shelx_estimated_absorpt_T_max   0.984
_shelx_estimated_absorpt_T_min   0.921
_exptl_absorpt_coefficient_mu    0.525
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99373
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.079
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1768
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 -11 0 0.0445
-2 11 0 0.0445
6 3 6 0.0329
-6 -5 -6 0.0766
0 -2 -15 0.0140
0 2 15 0.0140

_exptl_crystal_preparation       
'Crystals collected from crude reaction mixture following rotary evaporation.'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.9975 -10.9923 -0.0068 0.0826 0.4274 0.8445
-1.9975 10.9923 0.0068 -0.0826 -0.4274 -0.8445
5.9908 3.0001 6.0173 0.1984 0.8700 -0.4400
-5.9909 -4.9989 -6.0195 -0.2109 -0.8330 0.6007
0.0105 -1.9967 -14.9966 0.6720 -0.5962 0.3600
-0.0105 1.9967 14.9966 -0.6720 0.5962 -0.3600

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            7145
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        65.128
_diffrn_reflns_theta_max         65.128
_diffrn_reflns_theta_min         3.651
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -102.00 -19.00   1.00   10.00    --  -36.03 -57.00   0.00   83
  2  ω    -55.00  33.00   1.00   10.00    --  -36.03  38.00 150.00   88
  3  ω     55.00 162.00   1.00   40.00    --   93.63  15.00 120.00  107
  4  ω     80.00 157.00   1.00   40.00    --   93.63  45.00   0.00   77
  5  ω     24.00  92.00   1.00   40.00    --   93.63 -95.00 120.00   68
  6  ω     63.00 104.00   1.00   40.00    --   93.63 -95.00-180.00   41
  7  ω     26.00 111.00   1.00   40.00    --   93.63 -45.00  90.00   85
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0757646000
_diffrn_orient_matrix_UB_12      0.0062859000
_diffrn_orient_matrix_UB_13      -0.0455967000
_diffrn_orient_matrix_UB_21      0.1120167000
_diffrn_orient_matrix_UB_22      -0.0185519000
_diffrn_orient_matrix_UB_23      0.0423014000
_diffrn_orient_matrix_UB_31      -0.0198010000
_diffrn_orient_matrix_UB_32      -0.0804138000
_diffrn_orient_matrix_UB_33      -0.0133130000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3200
_reflns_number_total             4281
_reflns_odcompleteness_completeness 95.24
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     65.87
_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 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.169
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         4281
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0549
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0870P)²+0.7431P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1469
_refine_ls_wR_factor_ref         0.1584
_refine_special_details          
'Regions of electron density could not be adequately modelled and were accounted for using a solvent mask,SQUEEZE'
_olex2_refinement_description    
;
1.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C13(H13A,H13B)
1.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C12(H12), C10(H10), C19(H19), C22(H22), C26(H26), C17(H17), C24(H24),
 C18(H18), C15(H15), C16(H16), C25(H25), C23(H23)
1.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_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
N6 N 0.38107(16) 0.16616(9) 0.63533(8) 0.0302(4) Uani 1 1 d . . . . .
N4 N 0.40518(16) 0.27235(10) 0.66846(8) 0.0325(4) Uani 1 1 d . . . . .
N5 N 0.44899(17) 0.22557(10) 0.63752(8) 0.0349(5) Uani 1 1 d . . . . .
N3 N 0.48015(17) 0.48582(10) 0.87627(9) 0.0378(5) Uani 1 1 d . . . . .
N1 N 0.29680(17) 0.49774(10) 0.84069(9) 0.0392(5) Uani 1 1 d . . . . .
N2 N 0.38733(18) 0.53054(10) 0.87100(10) 0.0424(5) Uani 1 1 d . . . . .
C5 C 0.24408(19) 0.28564(11) 0.72174(9) 0.0278(5) Uani 1 1 d . . . . .
C2 C 0.13148(19) 0.37568(11) 0.78852(9) 0.0294(5) Uani 1 1 d . . . . .
C4 C 0.30820(18) 0.33522(11) 0.75719(9) 0.0291(5) Uani 1 1 d . . . . .
H4 H 0.391461 0.338532 0.758637 0.035 Uiso 1 1 calc R U . . .
C11 C 0.30873(19) 0.24330(11) 0.68573(9) 0.0286(5) Uani 1 1 d . . . . .
C1 C 0.06662(19) 0.32646(12) 0.75235(9) 0.0300(5) Uani 1 1 d . . . . .
C3 C 0.25481(19) 0.38034(11) 0.79078(9) 0.0292(5) Uani 1 1 d . . . . .
C9 C 0.33182(19) 0.43121(12) 0.82635(10) 0.0313(5) Uani 1 1 d . . . . .
C6 C 0.12062(19) 0.28009(12) 0.71900(9) 0.0299(5) Uani 1 1 d . . . . .
C12 C 0.2929(2) 0.17505(12) 0.66433(9) 0.0315(5) Uani 1 1 d . . . . .
H12 H 0.232929 0.141524 0.668988 0.038 Uiso 1 1 calc R U . . .
C20 C 0.4047(2) 0.10387(12) 0.60294(10) 0.0342(5) Uani 1 1 d . . . . .
H20A H 0.356841 0.062844 0.612141 0.041 Uiso 1 1 calc R U . . .
H20B H 0.489442 0.090588 0.613522 0.041 Uiso 1 1 calc R U . . .
C10 C 0.4501(2) 0.42377(12) 0.84913(10) 0.0344(5) Uani 1 1 d . . . . .
H10 H 0.499752 0.383572 0.846327 0.041 Uiso 1 1 calc R U . . .
C21 C 0.3772(2) 0.11639(12) 0.54162(10) 0.0355(5) Uani 1 1 d . . . . .
C7 C 0.0685(2) 0.42294(14) 0.82425(10) 0.0390(6) Uani 1 1 d . . . . .
H7A H 0.048561 0.469024 0.805654 0.059 Uiso 1 1 calc R U . . .
H7B H 0.120653 0.431256 0.859822 0.059 Uiso 1 1 calc R U . . .
H7C H -0.004296 0.399143 0.830389 0.059 Uiso 1 1 calc R U . . .
C8 C 0.0465(2) 0.22786(14) 0.68095(11) 0.0427(6) Uani 1 1 d . . . . .
H8A H 0.074642 0.226282 0.645625 0.064 Uiso 1 1 calc R U . . .
H8B H -0.036619 0.243290 0.674691 0.064 Uiso 1 1 calc R U . . .
H8C H 0.053142 0.179956 0.697726 0.064 Uiso 1 1 calc R U . . .
C14 C 0.6692(2) 0.54680(14) 0.87137(11) 0.0414(6) Uani 1 1 d . . . . .
C13 C 0.5954(2) 0.50835(15) 0.90696(11) 0.0442(6) Uani 1 1 d . . . . .
H13A H 0.639248 0.465527 0.923477 0.053 Uiso 1 1 calc R U . . .
H13B H 0.582972 0.540468 0.937477 0.053 Uiso 1 1 calc R U . . .
C19 C 0.7033(3) 0.61690(15) 0.88291(14) 0.0547(7) Uani 1 1 d . . . . .
H19 H 0.679596 0.640770 0.913284 0.066 Uiso 1 1 calc R U . . .
C22 C 0.4525(3) 0.09077(19) 0.50858(12) 0.0596(8) Uani 1 1 d . . . . .
H22 H 0.524189 0.067640 0.524858 0.072 Uiso 1 1 calc R U . . .
C26 C 0.2760(3) 0.15155(17) 0.51660(13) 0.0604(8) Uani 1 1 d . . . . .
H26 H 0.222084 0.169449 0.538535 0.072 Uiso 1 1 calc R U . . .
C17 C 0.8074(3) 0.61945(18) 0.80708(14) 0.0591(8) Uani 1 1 d . . . . .
H17 H 0.853923 0.644537 0.784948 0.071 Uiso 1 1 calc R U . . .
C24 C 0.3266(3) 0.13428(17) 0.42775(13) 0.0601(8) Uani 1 1 d . . . . .
H24 H 0.309991 0.140677 0.388841 0.072 Uiso 1 1 calc R U . . .
C18 C 0.7720(3) 0.65300(17) 0.85062(16) 0.0625(8) Uani 1 1 d . . . . .
H18 H 0.794598 0.701426 0.858930 0.075 Uiso 1 1 calc R U . . .
C15 C 0.7073(3) 0.51336(17) 0.82732(13) 0.0602(8) Uani 1 1 d . . . . .
H15 H 0.685805 0.464756 0.819092 0.072 Uiso 1 1 calc R U . . .
C16 C 0.7755(3) 0.5490(2) 0.79522(13) 0.0652(9) Uani 1 1 d . . . . .
H16 H 0.800376 0.525236 0.765098 0.078 Uiso 1 1 calc R U . . .
C25 C 0.2518(3) 0.16115(18) 0.45990(13) 0.0672(9) Uani 1 1 d . . . . .
H25 H 0.182596 0.186595 0.443369 0.081 Uiso 1 1 calc R U . . .
C23 C 0.4252(3) 0.0983(2) 0.45187(14) 0.0731(10) Uani 1 1 d . . . . .
H23 H 0.476206 0.077956 0.429492 0.088 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N6 N5 1.348(3) . ?
N6 C12 1.347(3) . ?
N6 C20 1.460(3) . ?
N4 N5 1.314(3) . ?
N4 C11 1.364(3) . ?
N3 N2 1.338(3) . ?
N3 C10 1.348(3) . ?
N3 C13 1.461(3) . ?
N1 N2 1.315(3) . ?
N1 C9 1.368(3) . ?
C5 C4 1.387(3) . ?
C5 C11 1.479(3) . ?
C5 C6 1.407(3) . ?
C2 C1 1.396(3) . ?
C2 C3 1.407(3) . ?
C2 C7 1.514(3) . ?
C4 H4 0.9500 . ?
C4 C3 1.394(3) . ?
C11 C12 1.375(3) . ?
C1 C1 1.510(4) 2_556 ?
C1 C6 1.408(3) . ?
C3 C9 1.472(3) . ?
C9 C10 1.378(3) . ?
C6 C8 1.503(3) . ?
C12 H12 0.9500 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.504(4) . ?
C10 H10 0.9500 . ?
C21 C22 1.372(4) . ?
C21 C26 1.377(4) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C14 C13 1.502(4) . ?
C14 C19 1.377(4) . ?
C14 C15 1.386(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C19 H19 0.9500 . ?
C19 C18 1.388(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.382(5) . ?
C26 H26 0.9500 . ?
C26 C25 1.385(5) . ?
C17 H17 0.9500 . ?
C17 C18 1.363(5) . ?
C17 C16 1.378(5) . ?
C24 H24 0.9500 . ?
C24 C25 1.362(5) . ?
C24 C23 1.355(5) . ?
C18 H18 0.9500 . ?
C15 H15 0.9500 . ?
C15 C16 1.376(5) . ?
C16 H16 0.9500 . ?
C25 H25 0.9500 . ?
C23 H23 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 N6 C20 120.78(17) . . ?
C12 N6 N5 111.10(17) . . ?
C12 N6 C20 128.09(18) . . ?
N5 N4 C11 109.40(17) . . ?
N4 N5 N6 106.85(16) . . ?
N2 N3 C10 110.90(19) . . ?
N2 N3 C13 120.05(19) . . ?
C10 N3 C13 129.0(2) . . ?
N2 N1 C9 109.22(19) . . ?
N1 N2 N3 107.38(18) . . ?
C4 C5 C11 117.76(19) . . ?
C4 C5 C6 119.60(19) . . ?
C6 C5 C11 122.5(2) . . ?
C1 C2 C3 118.84(19) . . ?
C1 C2 C7 119.83(19) . . ?
C3 C2 C7 121.3(2) . . ?
C5 C4 H4 118.8 . . ?
C5 C4 C3 122.33(19) . . ?
C3 C4 H4 118.8 . . ?
N4 C11 C5 119.68(19) . . ?
N4 C11 C12 107.80(18) . . ?
C12 C11 C5 132.51(19) . . ?
C2 C1 C1 117.68(18) . 2_556 ?
C2 C1 C6 122.35(19) . . ?
C6 C1 C1 119.9(2) . 2_556 ?
C2 C3 C9 123.67(19) . . ?
C4 C3 C2 118.9(2) . . ?
C4 C3 C9 117.43(19) . . ?
N1 C9 C3 124.3(2) . . ?
N1 C9 C10 107.4(2) . . ?
C10 C9 C3 128.2(2) . . ?
C5 C6 C1 118.0(2) . . ?
C5 C6 C8 121.91(19) . . ?
C1 C6 C8 120.1(2) . . ?
N6 C12 C11 104.85(19) . . ?
N6 C12 H12 127.6 . . ?
C11 C12 H12 127.6 . . ?
N6 C20 H20A 108.9 . . ?
N6 C20 H20B 108.9 . . ?
N6 C20 C21 113.49(19) . . ?
H20A C20 H20B 107.7 . . ?
C21 C20 H20A 108.9 . . ?
C21 C20 H20B 108.9 . . ?
N3 C10 C9 105.15(19) . . ?
N3 C10 H10 127.4 . . ?
C9 C10 H10 127.4 . . ?
C22 C21 C20 119.9(2) . . ?
C22 C21 C26 117.9(3) . . ?
C26 C21 C20 122.1(2) . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C19 C14 C13 120.0(2) . . ?
C19 C14 C15 118.0(3) . . ?
C15 C14 C13 122.0(2) . . ?
N3 C13 C14 112.7(2) . . ?
N3 C13 H13A 109.1 . . ?
N3 C13 H13B 109.1 . . ?
C14 C13 H13A 109.1 . . ?
C14 C13 H13B 109.1 . . ?
H13A C13 H13B 107.8 . . ?
C14 C19 H19 119.7 . . ?
C14 C19 C18 120.7(3) . . ?
C18 C19 H19 119.7 . . ?
C21 C22 H22 119.7 . . ?
C21 C22 C23 120.7(3) . . ?
C23 C22 H22 119.7 . . ?
C21 C26 H26 119.6 . . ?
C21 C26 C25 120.9(3) . . ?
C25 C26 H26 119.6 . . ?
C18 C17 H17 120.1 . . ?
C18 C17 C16 119.8(3) . . ?
C16 C17 H17 120.1 . . ?
C25 C24 H24 120.4 . . ?
C23 C24 H24 120.4 . . ?
C23 C24 C25 119.3(3) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 C19 120.4(3) . . ?
C17 C18 H18 119.8 . . ?
C14 C15 H15 119.3 . . ?
C16 C15 C14 121.5(3) . . ?
C16 C15 H15 119.3 . . ?
C17 C16 H16 120.2 . . ?
C15 C16 C17 119.6(3) . . ?
C15 C16 H16 120.2 . . ?
C26 C25 H25 119.9 . . ?
C24 C25 C26 120.3(3) . . ?
C24 C25 H25 119.9 . . ?
C22 C23 H23 119.6 . . ?
C24 C23 C22 120.9(3) . . ?
C24 C23 H23 119.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N6 C20 C21 C22 138.8(3) . . . . ?
N6 C20 C21 C26 -42.9(3) . . . . ?
N4 C11 C12 N6 0.2(3) . . . . ?
N5 N6 C12 C11 -0.6(3) . . . . ?
N5 N6 C20 C21 -69.6(3) . . . . ?
N5 N4 C11 C5 179.50(19) . . . . ?
N5 N4 C11 C12 0.2(3) . . . . ?
N1 C9 C10 N3 0.4(3) . . . . ?
N2 N3 C10 C9 -0.4(3) . . . . ?
N2 N3 C13 C14 -88.1(3) . . . . ?
N2 N1 C9 C3 -177.7(2) . . . . ?
N2 N1 C9 C10 -0.2(3) . . . . ?
C5 C4 C3 C2 -0.3(3) . . . . ?
C5 C4 C3 C9 -179.5(2) . . . . ?
C5 C11 C12 N6 -179.0(2) . . . . ?
C2 C1 C6 C5 -1.7(3) . . . . ?
C2 C1 C6 C8 179.7(2) . . . . ?
C2 C3 C9 N1 -31.6(4) . . . . ?
C2 C3 C9 C10 151.5(2) . . . . ?
C4 C5 C11 N4 -30.0(3) . . . . ?
C4 C5 C11 C12 149.1(3) . . . . ?
C4 C5 C6 C1 0.8(3) . . . . ?
C4 C5 C6 C8 179.4(2) . . . . ?
C4 C3 C9 N1 147.6(2) . . . . ?
C4 C3 C9 C10 -29.3(4) . . . . ?
C11 N4 N5 N6 -0.5(2) . . . . ?
C11 C5 C4 C3 176.7(2) . . . . ?
C11 C5 C6 C1 -175.6(2) . . . . ?
C11 C5 C6 C8 3.0(3) . . . . ?
C1 C2 C3 C4 -0.6(3) . . . . ?
C1 C2 C3 C9 178.6(2) . . . . ?
C1 C1 C6 C5 175.3(2) 2_556 . . . ?
C1 C1 C6 C8 -3.2(3) 2_556 . . . ?
C3 C2 C1 C1 -175.5(2) . . . 2_556 ?
C3 C2 C1 C6 1.6(3) . . . . ?
C3 C9 C10 N3 177.7(2) . . . . ?
C9 N1 N2 N3 0.0(3) . . . . ?
C6 C5 C4 C3 0.1(3) . . . . ?
C6 C5 C11 N4 146.4(2) . . . . ?
C6 C5 C11 C12 -34.4(4) . . . . ?
C12 N6 N5 N4 0.7(3) . . . . ?
C12 N6 C20 C21 108.1(3) . . . . ?
C20 N6 N5 N4 178.7(2) . . . . ?
C20 N6 C12 C11 -178.4(2) . . . . ?
C20 C21 C22 C23 176.4(3) . . . . ?
C20 C21 C26 C25 -178.8(3) . . . . ?
C10 N3 N2 N1 0.2(3) . . . . ?
C10 N3 C13 C14 89.8(3) . . . . ?
C21 C22 C23 C24 3.4(6) . . . . ?
C21 C26 C25 C24 1.6(5) . . . . ?
C7 C2 C1 C1 4.3(3) . . . 2_556 ?
C7 C2 C1 C6 -178.6(2) . . . . ?
C7 C2 C3 C4 179.6(2) . . . . ?
C7 C2 C3 C9 -1.2(3) . . . . ?
C14 C19 C18 C17 -0.3(5) . . . . ?
C14 C15 C16 C17 0.3(5) . . . . ?
C13 N3 N2 N1 178.5(2) . . . . ?
C13 N3 C10 C9 -178.4(2) . . . . ?
C13 C14 C19 C18 179.6(3) . . . . ?
C13 C14 C15 C16 -179.6(3) . . . . ?
C19 C14 C13 N3 118.7(3) . . . . ?
C19 C14 C15 C16 -1.1(5) . . . . ?
C22 C21 C26 C25 -0.5(5) . . . . ?
C26 C21 C22 C23 -2.0(5) . . . . ?
C18 C17 C16 C15 0.5(5) . . . . ?
C15 C14 C13 N3 -62.9(3) . . . . ?
C15 C14 C19 C18 1.1(4) . . . . ?
C16 C17 C18 C19 -0.5(5) . . . . ?
C25 C24 C23 C22 -2.3(6) . . . . ?
C23 C24 C25 C26 -0.2(5) . . . . ?

_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 0.000 0.000 0.000 0.0 0.0 ?
2 0.000 0.000 0.500 0.0 0.0 ?
3 -0.687 -0.687 0.000 543.7 146.2 ?
4 -0.647 0.647 0.500 543.7 146.2 ?
5 0.000 0.072 0.750 12.9 0.0 ?
6 0.000 0.428 0.250 8.0 0.0 ?
7 0.000 0.572 0.750 8.0 0.0 ?
8 0.000 0.928 0.250 12.9 0.0 ?
9 0.500 0.428 0.250 12.9 0.0 ?
10 0.500 0.572 0.750 12.9 0.0 ?
11 0.500 0.072 0.750 8.0 0.0 ?
12 0.500 0.928 0.250 8.0 0.0 ?
13 0.500 0.500 0.000 0.0 0.0 ?
14 0.500 0.500 0.500 0.0 0.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2

_ins_header                      
;
TITL JNS-261 in C2/c 
REM C2/c (#15 in standard setting)
CELL 1.54184  11.454571  18.617256  24.609810  90.0000 100.2645  90.0000
ZERR    4.00   0.000486   0.000694   0.001171   0.0000   0.0044   0.0000
LATT  7
SYMM -x, y,-z+1/2 
SFAC C H N
UNIT 240.00 300.00 32.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
SIZE 0.03 0.09 0.16
TREF
HKLF 4
END
;
_olex2_submission_original_sample_id JNS-261
_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 1.111
_oxdiff_exptl_absorpt_empirical_full_min 0.891
####################################################################### 
# 
# 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_1_DCM_ether
_database_code_depnum_ccdc_archive 'CCDC 2373366'
loop_
_audit_author_name
_audit_author_address
'Nicholas White'
;Australian National University
Australia
;
_audit_update_record             
;
2024-07-25 deposited with the CCDC.	2025-02-05 downloaded from the CCDC.
;
#==============================================================================
_audit_creation_date             2024-07-23
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C52 H46 N12'
_chemical_formula_sum            'C52 H46 N12'
_chemical_formula_weight         839.01
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C40 H60 N1 O4'
_chemical_oxdiff_usercomment     jns_283+4-carboxylate
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_H-M_alt        'P 1'
_space_group_name_Hall           'P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'

_cell_length_a                   10.8323(7)
_cell_length_b                   10.8523(10)
_cell_length_c                   13.3670(10)
_cell_angle_alpha                68.942(8)
_cell_angle_beta                 77.748(6)
_cell_angle_gamma                63.780(8)
_cell_volume                     1312.8(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    3104
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      70.2550
_cell_measurement_theta_min      4.5670
_shelx_estimated_absorpt_T_max   0.970
_shelx_estimated_absorpt_T_min   0.865
_exptl_absorpt_coefficient_mu    0.517
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             442
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 -8 0.0152
0 0 8 0.0375
-7 -3 -1 0.1120
7 3 1 0.1610
1 6 5 0.1397
0 -8 -5 0.0788

_exptl_crystal_preparation       
'Crystals were grown by vapour diffusion of diethyl ether into a dichloromethane solution.'
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.06
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0195 0.6049 -7.7972 0.1710 0.1842 -0.9679
0.3146 -0.4699 7.8698 -0.1391 -0.1505 0.9788
-7.0123 -2.8542 -1.2320 -0.6752 -0.7123 -0.1918
7.0123 2.8542 1.2320 0.6752 0.7123 0.1918
0.6789 6.3038 5.0185 -0.7095 0.6711 0.2151
-0.0775 -8.1177 -5.4383 0.9979 -0.8327 -0.1289

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            6788
_diffrn_reflns_point_group_measured_fraction_full 0.538
_diffrn_reflns_point_group_measured_fraction_max 0.538
_diffrn_reflns_theta_full        66.572
_diffrn_reflns_theta_max         66.572
_diffrn_reflns_theta_min         3.550
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -106.00 -15.00   1.00    5.00    --  -36.03 -19.00-180.00   91
  2  ω    -52.00  26.00   1.00    5.00    --  -36.03  57.00  90.00   78
  3  ω   -107.00  -7.00   1.00    5.00    --  -36.03 -19.00 -90.00  100
  4  ω     33.00  88.00   1.00    5.00    --   36.03-125.00   0.00   55
  5  ω      6.00  75.00   1.00    5.00    --   36.03 -99.00 150.00   69
  6  ω     74.00 101.00   1.00   20.00    --  105.15-111.00 -30.00   27
  7  ω     38.00 123.00   1.00   20.00    --  105.15 -61.00-150.00   85
  8  ω     36.00 109.00   1.00   20.00    --  105.15-111.00-120.00   73
  9  ω     45.00 130.00   1.00   20.00    --  105.15 -77.00  60.00   85
 10  ω     83.00 126.00   1.00   20.00    --  105.15 -30.00 120.00   43
 11  ω     84.00 175.00   1.00   20.00    --  105.15  30.00   0.00   91
 12  ω    116.00 160.00   1.00   20.00    --  105.15  77.00-150.00   44
 13  ω     53.00 106.00   1.00   20.00    --  105.15 -95.00   0.00   53
 14  ω     45.00 126.00   1.00   20.00    --  105.15 -30.00  30.00   81
 15  ω     37.00  68.00   1.00   20.00    --  105.15 -30.00 120.00   31
 16  ω     84.00 150.00   1.00   20.00    --  105.15  30.00 -60.00   66
 17  ω     39.00 115.00   1.00   20.00    --  105.15 -45.00 -60.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1440057000
_diffrn_orient_matrix_UB_12      -0.1044324000
_diffrn_orient_matrix_UB_13      -0.0296708000
_diffrn_orient_matrix_UB_21      0.0586183000
_diffrn_orient_matrix_UB_22      0.1119259000
_diffrn_orient_matrix_UB_23      -0.0147894000
_diffrn_orient_matrix_UB_31      0.0325775000
_diffrn_orient_matrix_UB_32      -0.0643081000
_diffrn_orient_matrix_UB_33      0.1192281000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.089
_reflns_Friedel_fraction_full    0.088
_reflns_Friedel_fraction_max     0.088
_reflns_number_gt                4741
_reflns_number_total             4990
_reflns_odcompleteness_completeness 98.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.230
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.2(4)
_refine_ls_extinction_coef       0.0073(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         4990
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0441
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0777P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1185
_refine_ls_wR_factor_ref         0.1208
_refine_special_details          
'One phenyl ring of the main molecule is disordered over two sites and was modelled with the use of DFIX restraints. Regions of disordered solvent could not be adequately modelled and were accounted for with the use of a solvent mask.,SQUEEZE'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C40-C41 = C41-C42 = C42-C43 = C43-C44 = C44-C45 = C45-C40
 1.395 with sigma of 0.01
 C40-C53 = C40-C56 = C43-C55 = C43-C54 = C53-C54 = C55-C56
 1.395 with sigma of 0.01
3. Others
 Fixed Sof: C41(0.6) H41(0.6) C42(0.6) H42(0.6) H43(0.6) H43A(0.4) C44(0.6)
 H44(0.6) C45(0.6) H45(0.6) C53(0.4) H53(0.4) C55(0.4) H55(0.4) C56(0.4)
 H56(0.4) C54(0.4) H54(0.4)
4.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C20(H20A,H20B), C39(H39A,H39B), C46(H46A,H46B)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C10(H10), C12(H12), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19),
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C30(H30), C36(H36), C38(H38),
  C41(H41), C42(H42), C43(H43), C43(H43A), C44(H44), C45(H45), C48(H48),
 C49(H49), C50(H50), C51(H51), C52(H52), C53(H53), C55(H55), C56(H56), C54(H54)
4.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
;
_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
N1 N 1.1865(3) 0.3029(3) 0.3345(2) 0.0357(6) Uani 1 1 d . . . . .
N2 N 1.2947(3) 0.3176(3) 0.2746(2) 0.0389(6) Uani 1 1 d . . . . .
N3 N 1.2901(2) 0.4442(3) 0.2717(2) 0.0293(5) Uani 1 1 d . . . . .
N4 N 0.7726(3) 0.1017(3) 0.6785(2) 0.0318(5) Uani 1 1 d . . . . .
N5 N 0.8164(3) -0.0358(3) 0.7348(2) 0.0337(6) Uani 1 1 d . . . . .
N6 N 0.9533(2) -0.0850(3) 0.7425(2) 0.0317(5) Uani 1 1 d . . . . .
N7 N 0.2959(2) 1.0256(3) 0.6798(2) 0.0315(5) Uani 1 1 d . . . . .
N8 N 0.2829(2) 1.1079(3) 0.7371(2) 0.0320(5) Uani 1 1 d . . . . .
N9 N 0.4085(2) 1.1041(3) 0.7358(2) 0.0286(5) Uani 1 1 d . . . . .
N10 N 0.2629(3) 0.7797(3) 0.3307(2) 0.0345(6) Uani 1 1 d . . . . .
N11 N 0.1530(3) 0.8543(3) 0.2738(2) 0.0367(6) Uani 1 1 d . . . . .
N12 N 0.1048(3) 0.9929(3) 0.2740(2) 0.0325(5) Uani 1 1 d . . . . .
C1 C 0.7552(3) 0.5459(3) 0.5105(3) 0.0297(6) Uani 1 1 d . . . . .
C2 C 0.8703(3) 0.5538(3) 0.4423(3) 0.0314(6) Uani 1 1 d . . . . .
C3 C 0.9882(3) 0.4246(3) 0.4442(2) 0.0276(6) Uani 1 1 d . . . . .
C4 C 0.9854(3) 0.2956(3) 0.5123(2) 0.0274(6) Uani 1 1 d . . . . .
H4 H 1.064424 0.209325 0.512003 0.033 Uiso 1 1 calc R U . . .
C5 C 0.8719(3) 0.2859(3) 0.5815(2) 0.0270(6) Uani 1 1 d . . . . .
C6 C 0.7543(3) 0.4144(3) 0.5817(2) 0.0291(6) Uani 1 1 d . . . . .
C7 C 0.8661(4) 0.6976(4) 0.3681(3) 0.0468(9) Uani 1 1 d . . . . .
H7A H 0.770000 0.766789 0.358860 0.070 Uiso 1 1 calc R U . . .
H7B H 0.911562 0.687196 0.298158 0.070 Uiso 1 1 calc R U . . .
H7C H 0.914123 0.732413 0.398983 0.070 Uiso 1 1 calc R U . . .
C8 C 0.6295(3) 0.4139(3) 0.6567(3) 0.0379(7) Uani 1 1 d . . . . .
H8A H 0.562990 0.408579 0.620586 0.057 Uiso 1 1 calc R U . . .
H8B H 0.587025 0.502438 0.677554 0.057 Uiso 1 1 calc R U . . .
H8C H 0.657247 0.330188 0.720992 0.057 Uiso 1 1 calc R U . . .
C9 C 1.1116(3) 0.4199(3) 0.3699(2) 0.0279(6) Uani 1 1 d . . . . .
C10 C 1.1792(3) 0.5108(3) 0.3293(3) 0.0330(6) Uani 1 1 d . . . . .
H10 H 1.153042 0.601318 0.339901 0.040 Uiso 1 1 calc R U . . .
C11 C 0.8812(3) 0.1414(3) 0.6500(2) 0.0273(6) Uani 1 1 d . . . . .
C12 C 0.9968(3) 0.0219(3) 0.6914(2) 0.0303(6) Uani 1 1 d . . . . .
H12 H 1.088047 0.016255 0.685267 0.036 Uiso 1 1 calc R U . . .
C13 C 1.4014(3) 0.4905(4) 0.2129(3) 0.0344(6) Uani 1 1 d . . . . .
H13A H 1.490983 0.407415 0.229938 0.041 Uiso 1 1 calc R U . . .
H13B H 1.399233 0.565973 0.239059 0.041 Uiso 1 1 calc R U . . .
C14 C 1.3935(3) 0.5483(4) 0.0929(3) 0.0343(6) Uani 1 1 d . . . . .
C15 C 1.4043(5) 0.4647(4) 0.0322(3) 0.0548(10) Uani 1 1 d . . . . .
H15 H 1.413098 0.368239 0.067308 0.066 Uiso 1 1 calc R U . . .
C16 C 1.4028(6) 0.5164(6) -0.0776(4) 0.0694(13) Uani 1 1 d . . . . .
H16 H 1.409817 0.456051 -0.117210 0.083 Uiso 1 1 calc R U . . .
C17 C 1.3912(5) 0.6552(5) -0.1306(3) 0.0578(10) Uani 1 1 d . . . . .
H17 H 1.386550 0.692559 -0.206451 0.069 Uiso 1 1 calc R U . . .
C18 C 1.3864(7) 0.7394(6) -0.0721(4) 0.0794(16) Uani 1 1 d . . . . .
H18 H 1.384001 0.833399 -0.107992 0.095 Uiso 1 1 calc R U . . .
C19 C 1.3850(6) 0.6865(5) 0.0399(4) 0.0652(12) Uani 1 1 d . . . . .
H19 H 1.378071 0.746289 0.079913 0.078 Uiso 1 1 calc R U . . .
C20 C 1.0318(3) -0.2356(3) 0.8017(3) 0.0353(7) Uani 1 1 d . . . . .
H20A H 0.973786 -0.267520 0.864612 0.042 Uiso 1 1 calc R U . . .
H20B H 1.113674 -0.242558 0.828704 0.042 Uiso 1 1 calc R U . . .
C21 C 1.0780(3) -0.3343(3) 0.7339(3) 0.0339(6) Uani 1 1 d . . . . .
C22 C 1.1761(5) -0.3266(5) 0.6491(3) 0.0548(10) Uani 1 1 d . . . . .
H22 H 1.213848 -0.256965 0.632940 0.066 Uiso 1 1 calc R U . . .
C23 C 1.2201(5) -0.4200(5) 0.5869(3) 0.0571(10) Uani 1 1 d . . . . .
H23 H 1.284899 -0.411586 0.527303 0.069 Uiso 1 1 calc R U . . .
C24 C 1.1691(4) -0.5242(4) 0.6126(3) 0.0530(10) Uani 1 1 d . . . . .
H24 H 1.198439 -0.587576 0.570330 0.064 Uiso 1 1 calc R U . . .
C25 C 1.0749(4) -0.5371(4) 0.7002(4) 0.0529(10) Uani 1 1 d . . . . .
H25 H 1.041814 -0.610866 0.719106 0.064 Uiso 1 1 calc R U . . .
C26 C 1.0293(3) -0.4414(4) 0.7599(3) 0.0444(8) Uani 1 1 d . . . . .
H26 H 0.964126 -0.449544 0.819239 0.053 Uiso 1 1 calc R U . . .
C27 C 0.6238(3) 0.6787(3) 0.5049(2) 0.0294(6) Uani 1 1 d . . . . .
C28 C 0.5988(3) 0.7611(3) 0.5726(2) 0.0295(6) Uani 1 1 d . . . . .
C29 C 0.4694(3) 0.8777(3) 0.5715(2) 0.0268(6) Uani 1 1 d . . . . .
C30 C 0.3719(3) 0.9080(3) 0.5051(2) 0.0269(5) Uani 1 1 d . . . . .
H30 H 0.285144 0.986319 0.505787 0.032 Uiso 1 1 calc R U . . .
C31 C 0.3971(3) 0.8261(3) 0.4361(2) 0.0272(6) Uani 1 1 d . . . . .
C32 C 0.5261(3) 0.7094(3) 0.4354(3) 0.0295(6) Uani 1 1 d . . . . .
C33 C 0.7064(3) 0.7235(4) 0.6453(3) 0.0438(8) Uani 1 1 d . . . . .
H33A H 0.749443 0.792956 0.616692 0.066 Uiso 1 1 calc R U . . .
H33B H 0.776713 0.626359 0.649628 0.066 Uiso 1 1 calc R U . . .
H33C H 0.663258 0.726556 0.717152 0.066 Uiso 1 1 calc R U . . .
C34 C 0.5608(3) 0.6209(4) 0.3609(3) 0.0391(7) Uani 1 1 d . . . . .
H34A H 0.527331 0.543928 0.394506 0.059 Uiso 1 1 calc R U . . .
H34B H 0.660968 0.578520 0.346496 0.059 Uiso 1 1 calc R U . . .
H34C H 0.516624 0.682754 0.293293 0.059 Uiso 1 1 calc R U . . .
C35 C 0.4298(3) 0.9686(3) 0.6424(2) 0.0263(6) Uani 1 1 d . . . . .
C36 C 0.5027(3) 1.0184(3) 0.6789(2) 0.0296(6) Uani 1 1 d . . . . .
H36 H 0.598565 0.997291 0.666693 0.036 Uiso 1 1 calc R U . . .
C37 C 0.2851(3) 0.8706(3) 0.3685(2) 0.0288(6) Uani 1 1 d . . . . .
C38 C 0.1841(3) 1.0068(3) 0.3313(2) 0.0294(6) Uani 1 1 d . . . . .
H38 H 0.172597 1.092339 0.343529 0.035 Uiso 1 1 calc R U . . .
C39 C 0.4296(3) 1.1890(3) 0.7894(3) 0.0340(6) Uani 1 1 d . . . . .
H39A H 0.350101 1.283513 0.777956 0.041 Uiso 1 1 calc R U . . .
H39B H 0.513081 1.207019 0.755565 0.041 Uiso 1 1 calc R U . . .
C40 C 0.4457(3) 1.1180(3) 0.9084(2) 0.0331(6) Uani 1 1 d D . . . .
C41 C 0.5578(7) 0.9942(8) 0.9502(5) 0.0549(17) Uani 0.6 1 d D . P A 1
H41 H 0.627139 0.948815 0.902868 0.066 Uiso 0.6 1 calc R U P A 1
C42 C 0.5711(8) 0.9348(9) 1.0596(5) 0.0625(19) Uani 0.6 1 d D . P A 1
H42 H 0.648610 0.848880 1.087066 0.075 Uiso 0.6 1 calc R U P A 1
C43 C 0.4745(6) 0.9987(6) 1.1270(3) 0.0756(15) Uani 1 1 d D . . . .
H43 H 0.488239 0.964374 1.201603 0.091 Uiso 0.6 1 calc R U P A 1
H43A H 0.475718 0.975692 1.202490 0.091 Uiso 0.4 1 calc R U P A 2
C44 C 0.3513(9) 1.1180(8) 1.0867(5) 0.068(2) Uani 0.6 1 d D . P A 1
H44 H 0.278528 1.155587 1.135576 0.082 Uiso 0.6 1 calc R U P A 1
C45 C 0.3362(7) 1.1799(8) 0.9776(5) 0.0526(16) Uani 0.6 1 d D . P A 1
H45 H 0.255147 1.261096 0.950125 0.063 Uiso 0.6 1 calc R U P A 1
C46 C -0.0164(4) 1.1047(4) 0.2151(3) 0.0421(8) Uani 1 1 d . . . . .
H46A H -0.017740 1.081371 0.150308 0.051 Uiso 1 1 calc R U . . .
H46B H -0.007667 1.198226 0.190913 0.051 Uiso 1 1 calc R U . . .
C47 C -0.1496(4) 1.1197(4) 0.2800(3) 0.0406(7) Uani 1 1 d . . . . .
C48 C -0.1844(5) 1.1736(6) 0.3663(4) 0.0632(12) Uani 1 1 d . . . . .
H48 H -0.121469 1.199649 0.385114 0.076 Uiso 1 1 calc R U . . .
C49 C -0.3091(5) 1.1902(7) 0.4259(4) 0.0778(17) Uani 1 1 d . . . . .
H49 H -0.331441 1.228341 0.484265 0.093 Uiso 1 1 calc R U . . .
C50 C -0.4008(4) 1.1513(5) 0.4000(3) 0.0553(10) Uani 1 1 d . . . . .
H50 H -0.486255 1.162062 0.440634 0.066 Uiso 1 1 calc R U . . .
C51 C -0.3672(4) 1.0966(4) 0.3149(5) 0.0629(12) Uani 1 1 d . . . . .
H51 H -0.429895 1.069366 0.296886 0.075 Uiso 1 1 calc R U . . .
C52 C -0.2427(4) 1.0810(4) 0.2553(4) 0.0556(10) Uani 1 1 d . . . . .
H52 H -0.220959 1.043239 0.196697 0.067 Uiso 1 1 calc R U . . .
C53 C 0.3581(10) 1.0627(13) 0.9793(6) 0.056(3) Uani 0.4 1 d D . P A 2
H53 H 0.282131 1.067179 0.951197 0.067 Uiso 0.4 1 calc R U P A 2
C55 C 0.5829(12) 1.0294(18) 1.0572(7) 0.076(4) Uani 0.4 1 d D . P A 2
H55 H 0.665958 1.006691 1.086170 0.091 Uiso 0.4 1 calc R U P A 2
C56 C 0.5693(10) 1.0926(16) 0.9467(7) 0.059(3) Uani 0.4 1 d D . P A 2
H56 H 0.639572 1.117222 0.899694 0.071 Uiso 0.4 1 calc R U P A 2
C54 C 0.3714(14) 1.0026(18) 1.0854(8) 0.093(5) Uani 0.4 1 d D . P A 2
H54 H 0.308359 0.963530 1.129938 0.111 Uiso 0.4 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 N2 1.309(4) . ?
N1 C9 1.362(4) . ?
N2 N3 1.339(4) . ?
N3 C10 1.342(4) . ?
N3 C13 1.474(4) . ?
N4 N5 1.318(4) . ?
N4 C11 1.361(4) . ?
N5 N6 1.349(4) . ?
N6 C12 1.347(4) . ?
N6 C20 1.466(4) . ?
N7 N8 1.319(4) . ?
N7 C35 1.363(4) . ?
N8 N9 1.340(4) . ?
N9 C36 1.351(4) . ?
N9 C39 1.464(4) . ?
N10 N11 1.319(4) . ?
N10 C37 1.381(4) . ?
N11 N12 1.357(4) . ?
N12 C38 1.351(4) . ?
N12 C46 1.470(4) . ?
C1 C2 1.395(4) . ?
C1 C6 1.405(4) . ?
C1 C27 1.505(4) . ?
C2 C3 1.415(4) . ?
C2 C7 1.506(4) . ?
C3 C4 1.378(4) . ?
C3 C9 1.480(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.393(4) . ?
C5 C6 1.413(4) . ?
C5 C11 1.475(4) . ?
C6 C8 1.504(4) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.374(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.378(4) . ?
C12 H12 0.9500 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.503(4) . ?
C14 C15 1.375(5) . ?
C14 C19 1.379(6) . ?
C15 H15 0.9500 . ?
C15 C16 1.370(6) . ?
C16 H16 0.9500 . ?
C16 C17 1.375(7) . ?
C17 H17 0.9500 . ?
C17 C18 1.380(8) . ?
C18 H18 0.9500 . ?
C18 C19 1.397(7) . ?
C19 H19 0.9500 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.500(5) . ?
C21 C22 1.387(5) . ?
C21 C26 1.387(5) . ?
C22 H22 0.9500 . ?
C22 C23 1.398(6) . ?
C23 H23 0.9500 . ?
C23 C24 1.377(7) . ?
C24 H24 0.9500 . ?
C24 C25 1.390(6) . ?
C25 H25 0.9500 . ?
C25 C26 1.392(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.398(4) . ?
C27 C32 1.406(4) . ?
C28 C29 1.412(4) . ?
C28 C33 1.498(4) . ?
C29 C30 1.377(4) . ?
C29 C35 1.477(4) . ?
C30 H30 0.9500 . ?
C30 C31 1.408(4) . ?
C31 C32 1.413(4) . ?
C31 C37 1.468(4) . ?
C32 C34 1.504(4) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.372(4) . ?
C36 H36 0.9500 . ?
C37 C38 1.380(4) . ?
C38 H38 0.9500 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.507(4) . ?
C40 C41 1.378(6) . ?
C40 C45 1.411(6) . ?
C40 C53 1.368(8) . ?
C40 C56 1.412(8) . ?
C41 H41 0.9500 . ?
C41 C42 1.380(7) . ?
C42 H42 0.9500 . ?
C42 C43 1.340(8) . ?
C43 H43 0.9500 . ?
C43 H43A 0.9500 . ?
C43 C44 1.423(8) . ?
C43 C55 1.421(9) . ?
C43 C54 1.328(9) . ?
C44 H44 0.9500 . ?
C44 C45 1.381(7) . ?
C45 H45 0.9500 . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C46 C47 1.492(5) . ?
C47 C48 1.386(5) . ?
C47 C52 1.385(6) . ?
C48 H48 0.9500 . ?
C48 C49 1.386(7) . ?
C49 H49 0.9500 . ?
C49 C50 1.380(8) . ?
C50 H50 0.9500 . ?
C50 C51 1.379(7) . ?
C51 H51 0.9500 . ?
C51 C52 1.386(6) . ?
C52 H52 0.9500 . ?
C53 H53 0.9500 . ?
C53 C54 1.341(9) . ?
C55 H55 0.9500 . ?
C55 C56 1.396(9) . ?
C56 H56 0.9500 . ?
C54 H54 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 N1 C9 110.0(3) . . ?
N1 N2 N3 106.6(2) . . ?
N2 N3 C10 111.2(2) . . ?
N2 N3 C13 119.9(2) . . ?
C10 N3 C13 128.8(3) . . ?
N5 N4 C11 109.1(2) . . ?
N4 N5 N6 107.6(2) . . ?
N5 N6 C20 120.4(3) . . ?
C12 N6 N5 110.2(2) . . ?
C12 N6 C20 129.5(3) . . ?
N8 N7 C35 109.7(2) . . ?
N7 N8 N9 106.5(2) . . ?
N8 N9 C36 111.3(2) . . ?
N8 N9 C39 120.6(2) . . ?
C36 N9 C39 128.1(3) . . ?
N11 N10 C37 109.0(3) . . ?
N10 N11 N12 107.3(2) . . ?
N11 N12 C46 120.7(3) . . ?
C38 N12 N11 110.6(2) . . ?
C38 N12 C46 128.6(3) . . ?
C2 C1 C6 121.9(3) . . ?
C2 C1 C27 120.4(3) . . ?
C6 C1 C27 117.5(3) . . ?
C1 C2 C3 118.6(3) . . ?
C1 C2 C7 119.8(3) . . ?
C3 C2 C7 121.6(3) . . ?
C2 C3 C9 122.8(3) . . ?
C4 C3 C2 119.2(3) . . ?
C4 C3 C9 117.9(3) . . ?
C3 C4 H4 118.5 . . ?
C3 C4 C5 123.0(3) . . ?
C5 C4 H4 118.5 . . ?
C4 C5 C6 118.4(3) . . ?
C4 C5 C11 117.8(2) . . ?
C6 C5 C11 123.8(3) . . ?
C1 C6 C5 118.9(3) . . ?
C1 C6 C8 119.4(3) . . ?
C5 C6 C8 121.7(3) . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 C3 120.0(3) . . ?
N1 C9 C10 107.0(3) . . ?
C10 C9 C3 132.9(3) . . ?
N3 C10 C9 105.2(3) . . ?
N3 C10 H10 127.4 . . ?
C9 C10 H10 127.4 . . ?
N4 C11 C5 124.0(2) . . ?
N4 C11 C12 107.6(3) . . ?
C12 C11 C5 128.2(3) . . ?
N6 C12 C11 105.6(2) . . ?
N6 C12 H12 127.2 . . ?
C11 C12 H12 127.2 . . ?
N3 C13 H13A 108.6 . . ?
N3 C13 H13B 108.6 . . ?
N3 C13 C14 114.7(3) . . ?
H13A C13 H13B 107.6 . . ?
C14 C13 H13A 108.6 . . ?
C14 C13 H13B 108.6 . . ?
C15 C14 C13 122.3(3) . . ?
C15 C14 C19 118.0(4) . . ?
C19 C14 C13 119.6(3) . . ?
C14 C15 H15 119.0 . . ?
C16 C15 C14 121.9(4) . . ?
C16 C15 H15 119.0 . . ?
C15 C16 H16 119.9 . . ?
C15 C16 C17 120.3(5) . . ?
C17 C16 H16 119.9 . . ?
C16 C17 H17 120.5 . . ?
C16 C17 C18 119.0(4) . . ?
C18 C17 H17 120.5 . . ?
C17 C18 H18 120.0 . . ?
C17 C18 C19 120.1(5) . . ?
C19 C18 H18 120.0 . . ?
C14 C19 C18 120.6(5) . . ?
C14 C19 H19 119.7 . . ?
C18 C19 H19 119.7 . . ?
N6 C20 H20A 109.1 . . ?
N6 C20 H20B 109.1 . . ?
N6 C20 C21 112.6(3) . . ?
H20A C20 H20B 107.8 . . ?
C21 C20 H20A 109.1 . . ?
C21 C20 H20B 109.1 . . ?
C22 C21 C20 121.0(3) . . ?
C26 C21 C20 120.1(3) . . ?
C26 C21 C22 118.8(3) . . ?
C21 C22 H22 119.6 . . ?
C21 C22 C23 120.8(4) . . ?
C23 C22 H22 119.6 . . ?
C22 C23 H23 120.2 . . ?
C24 C23 C22 119.6(4) . . ?
C24 C23 H23 120.2 . . ?
C23 C24 H24 119.9 . . ?
C23 C24 C25 120.2(4) . . ?
C25 C24 H24 119.9 . . ?
C24 C25 H25 120.2 . . ?
C24 C25 C26 119.6(4) . . ?
C26 C25 H25 120.2 . . ?
C21 C26 C25 120.8(4) . . ?
C21 C26 H26 119.6 . . ?
C25 C26 H26 119.6 . . ?
C28 C27 C1 119.9(3) . . ?
C28 C27 C32 122.4(3) . . ?
C32 C27 C1 117.6(3) . . ?
C27 C28 C29 118.2(3) . . ?
C27 C28 C33 120.2(3) . . ?
C29 C28 C33 121.5(3) . . ?
C28 C29 C35 122.9(3) . . ?
C30 C29 C28 120.1(3) . . ?
C30 C29 C35 117.0(2) . . ?
C29 C30 H30 119.1 . . ?
C29 C30 C31 121.9(3) . . ?
C31 C30 H30 119.1 . . ?
C30 C31 C32 118.9(3) . . ?
C30 C31 C37 116.5(2) . . ?
C32 C31 C37 124.6(3) . . ?
C27 C32 C31 118.5(3) . . ?
C27 C32 C34 120.1(3) . . ?
C31 C32 C34 121.4(3) . . ?
C28 C33 H33A 109.5 . . ?
C28 C33 H33B 109.5 . . ?
C28 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N7 C35 C29 120.0(2) . . ?
N7 C35 C36 107.4(3) . . ?
C36 C35 C29 132.5(3) . . ?
N9 C36 C35 105.0(3) . . ?
N9 C36 H36 127.5 . . ?
C35 C36 H36 127.5 . . ?
N10 C37 C31 124.9(3) . . ?
C38 C37 N10 107.5(3) . . ?
C38 C37 C31 127.6(3) . . ?
N12 C38 C37 105.5(3) . . ?
N12 C38 H38 127.2 . . ?
C37 C38 H38 127.2 . . ?
N9 C39 H39A 108.8 . . ?
N9 C39 H39B 108.8 . . ?
N9 C39 C40 113.9(3) . . ?
H39A C39 H39B 107.7 . . ?
C40 C39 H39A 108.8 . . ?
C40 C39 H39B 108.8 . . ?
C41 C40 C39 122.9(4) . . ?
C41 C40 C45 120.1(4) . . ?
C45 C40 C39 117.0(4) . . ?
C53 C40 C39 125.2(4) . . ?
C53 C40 C56 117.7(6) . . ?
C56 C40 C39 116.7(4) . . ?
C40 C41 H41 119.4 . . ?
C40 C41 C42 121.2(6) . . ?
C42 C41 H41 119.4 . . ?
C41 C42 H42 120.1 . . ?
C43 C42 C41 119.9(6) . . ?
C43 C42 H42 120.1 . . ?
C42 C43 H43 120.0 . . ?
C42 C43 C44 119.9(5) . . ?
C44 C43 H43 120.0 . . ?
C55 C43 H43A 120.4 . . ?
C54 C43 H43A 120.4 . . ?
C54 C43 C55 119.2(7) . . ?
C43 C44 H44 119.6 . . ?
C45 C44 C43 120.8(6) . . ?
C45 C44 H44 119.6 . . ?
C40 C45 H45 121.3 . . ?
C44 C45 C40 117.5(6) . . ?
C44 C45 H45 121.3 . . ?
N12 C46 H46A 108.9 . . ?
N12 C46 H46B 108.9 . . ?
N12 C46 C47 113.5(3) . . ?
H46A C46 H46B 107.7 . . ?
C47 C46 H46A 108.9 . . ?
C47 C46 H46B 108.9 . . ?
C48 C47 C46 121.1(3) . . ?
C52 C47 C46 120.9(4) . . ?
C52 C47 C48 118.0(4) . . ?
C47 C48 H48 119.3 . . ?
C47 C48 C49 121.4(4) . . ?
C49 C48 H48 119.3 . . ?
C48 C49 H49 120.1 . . ?
C50 C49 C48 119.8(5) . . ?
C50 C49 H49 120.1 . . ?
C49 C50 H50 120.3 . . ?
C51 C50 C49 119.5(4) . . ?
C51 C50 H50 120.3 . . ?
C50 C51 H51 119.8 . . ?
C50 C51 C52 120.4(4) . . ?
C52 C51 H51 119.8 . . ?
C47 C52 C51 120.8(4) . . ?
C47 C52 H52 119.6 . . ?
C51 C52 H52 119.6 . . ?
C40 C53 H53 117.6 . . ?
C54 C53 C40 124.9(8) . . ?
C54 C53 H53 117.6 . . ?
C43 C55 H55 119.5 . . ?
C56 C55 C43 121.0(8) . . ?
C56 C55 H55 119.5 . . ?
C40 C56 H56 121.7 . . ?
C55 C56 C40 116.6(8) . . ?
C55 C56 H56 121.7 . . ?
C43 C54 C53 118.7(9) . . ?
C43 C54 H54 120.7 . . ?
C53 C54 H54 120.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 N2 N3 C10 -0.1(4) . . . . ?
N1 N2 N3 C13 178.0(3) . . . . ?
N1 C9 C10 N3 0.3(4) . . . . ?
N2 N1 C9 C3 -176.6(3) . . . . ?
N2 N1 C9 C10 -0.4(4) . . . . ?
N2 N3 C10 C9 -0.1(4) . . . . ?
N2 N3 C13 C14 77.6(4) . . . . ?
N3 C13 C14 C15 -63.1(4) . . . . ?
N3 C13 C14 C19 121.6(4) . . . . ?
N4 N5 N6 C12 0.4(4) . . . . ?
N4 N5 N6 C20 179.6(3) . . . . ?
N4 C11 C12 N6 0.4(3) . . . . ?
N5 N4 C11 C5 176.6(3) . . . . ?
N5 N4 C11 C12 -0.2(3) . . . . ?
N5 N6 C12 C11 -0.5(3) . . . . ?
N5 N6 C20 C21 85.3(4) . . . . ?
N6 C20 C21 C22 67.9(4) . . . . ?
N6 C20 C21 C26 -116.3(3) . . . . ?
N7 N8 N9 C36 -0.7(3) . . . . ?
N7 N8 N9 C39 177.9(3) . . . . ?
N7 C35 C36 N9 -0.5(3) . . . . ?
N8 N7 C35 C29 -177.1(3) . . . . ?
N8 N7 C35 C36 0.1(3) . . . . ?
N8 N9 C36 C35 0.7(3) . . . . ?
N8 N9 C39 C40 82.7(4) . . . . ?
N9 C39 C40 C41 67.4(6) . . . . ?
N9 C39 C40 C45 -109.4(5) . . . . ?
N9 C39 C40 C53 -50.8(8) . . . . ?
N9 C39 C40 C56 121.7(8) . . . . ?
N10 N11 N12 C38 -0.1(4) . . . . ?
N10 N11 N12 C46 178.7(3) . . . . ?
N10 C37 C38 N12 0.5(3) . . . . ?
N11 N10 C37 C31 179.3(3) . . . . ?
N11 N10 C37 C38 -0.6(4) . . . . ?
N11 N12 C38 C37 -0.3(4) . . . . ?
N11 N12 C46 C47 88.7(4) . . . . ?
N12 C46 C47 C48 68.6(5) . . . . ?
N12 C46 C47 C52 -111.9(4) . . . . ?
C1 C2 C3 C4 0.6(4) . . . . ?
C1 C2 C3 C9 175.6(3) . . . . ?
C1 C27 C28 C29 -174.7(3) . . . . ?
C1 C27 C28 C33 4.1(5) . . . . ?
C1 C27 C32 C31 174.5(3) . . . . ?
C1 C27 C32 C34 -6.7(4) . . . . ?
C2 C1 C6 C5 -2.1(4) . . . . ?
C2 C1 C6 C8 177.2(3) . . . . ?
C2 C1 C27 C28 -93.4(4) . . . . ?
C2 C1 C27 C32 90.7(4) . . . . ?
C2 C3 C4 C5 -1.1(4) . . . . ?
C2 C3 C9 N1 -146.3(3) . . . . ?
C2 C3 C9 C10 38.7(5) . . . . ?
C3 C4 C5 C6 0.1(4) . . . . ?
C3 C4 C5 C11 179.6(3) . . . . ?
C3 C9 C10 N3 175.8(3) . . . . ?
C4 C3 C9 N1 28.8(4) . . . . ?
C4 C3 C9 C10 -146.2(3) . . . . ?
C4 C5 C6 C1 1.5(4) . . . . ?
C4 C5 C6 C8 -177.8(3) . . . . ?
C4 C5 C11 N4 -145.8(3) . . . . ?
C4 C5 C11 C12 30.4(4) . . . . ?
C5 C11 C12 N6 -176.2(3) . . . . ?
C6 C1 C2 C3 1.1(5) . . . . ?
C6 C1 C2 C7 -179.6(3) . . . . ?
C6 C1 C27 C28 90.3(4) . . . . ?
C6 C1 C27 C32 -85.6(4) . . . . ?
C6 C5 C11 N4 33.8(5) . . . . ?
C6 C5 C11 C12 -150.1(3) . . . . ?
C7 C2 C3 C4 -178.8(3) . . . . ?
C7 C2 C3 C9 -3.7(5) . . . . ?
C9 N1 N2 N3 0.3(4) . . . . ?
C9 C3 C4 C5 -176.4(3) . . . . ?
C10 N3 C13 C14 -104.6(4) . . . . ?
C11 N4 N5 N6 -0.1(3) . . . . ?
C11 C5 C6 C1 -178.0(3) . . . . ?
C11 C5 C6 C8 2.7(5) . . . . ?
C12 N6 C20 C21 -95.6(4) . . . . ?
C13 N3 C10 C9 -178.0(3) . . . . ?
C13 C14 C15 C16 -177.2(4) . . . . ?
C13 C14 C19 C18 175.9(5) . . . . ?
C14 C15 C16 C17 0.5(8) . . . . ?
C15 C14 C19 C18 0.4(8) . . . . ?
C15 C16 C17 C18 2.4(8) . . . . ?
C16 C17 C18 C19 -3.8(9) . . . . ?
C17 C18 C19 C14 2.4(9) . . . . ?
C19 C14 C15 C16 -1.9(7) . . . . ?
C20 N6 C12 C11 -179.7(3) . . . . ?
C20 C21 C22 C23 179.2(4) . . . . ?
C20 C21 C26 C25 -177.7(3) . . . . ?
C21 C22 C23 C24 -2.3(7) . . . . ?
C22 C21 C26 C25 -1.9(5) . . . . ?
C22 C23 C24 C25 -0.3(6) . . . . ?
C23 C24 C25 C26 1.8(6) . . . . ?
C24 C25 C26 C21 -0.7(6) . . . . ?
C26 C21 C22 C23 3.4(6) . . . . ?
C27 C1 C2 C3 -175.1(3) . . . . ?
C27 C1 C2 C7 4.3(5) . . . . ?
C27 C1 C6 C5 174.1(3) . . . . ?
C27 C1 C6 C8 -6.6(4) . . . . ?
C27 C28 C29 C30 -0.1(4) . . . . ?
C27 C28 C29 C35 177.7(3) . . . . ?
C28 C27 C32 C31 -1.4(4) . . . . ?
C28 C27 C32 C34 177.4(3) . . . . ?
C28 C29 C30 C31 -0.5(4) . . . . ?
C28 C29 C35 N7 -146.8(3) . . . . ?
C28 C29 C35 C36 36.8(5) . . . . ?
C29 C30 C31 C32 0.2(4) . . . . ?
C29 C30 C31 C37 -179.4(3) . . . . ?
C29 C35 C36 N9 176.2(3) . . . . ?
C30 C29 C35 N7 31.0(4) . . . . ?
C30 C29 C35 C36 -145.4(3) . . . . ?
C30 C31 C32 C27 0.8(4) . . . . ?
C30 C31 C32 C34 -178.0(3) . . . . ?
C30 C31 C37 N10 -152.2(3) . . . . ?
C30 C31 C37 C38 27.7(5) . . . . ?
C31 C37 C38 N12 -179.4(3) . . . . ?
C32 C27 C28 C29 1.1(4) . . . . ?
C32 C27 C28 C33 179.9(3) . . . . ?
C32 C31 C37 N10 28.2(5) . . . . ?
C32 C31 C37 C38 -151.9(3) . . . . ?
C33 C28 C29 C30 -178.9(3) . . . . ?
C33 C28 C29 C35 -1.1(5) . . . . ?
C35 N7 N8 N9 0.4(3) . . . . ?
C35 C29 C30 C31 -178.4(3) . . . . ?
C36 N9 C39 C40 -99.0(4) . . . . ?
C37 N10 N11 N12 0.5(4) . . . . ?
C37 C31 C32 C27 -179.7(3) . . . . ?
C37 C31 C32 C34 1.5(5) . . . . ?
C38 N12 C46 C47 -92.7(4) . . . . ?
C39 N9 C36 C35 -177.7(3) . . . . ?
C39 C40 C41 C42 177.9(7) . . . . ?
C39 C40 C45 C44 -178.4(6) . . . . ?
C39 C40 C53 C54 -178.4(11) . . . . ?
C39 C40 C56 C55 178.8(11) . . . . ?
C40 C41 C42 C43 -0.6(13) . . . . ?
C40 C53 C54 C43 2(2) . . . . ?
C41 C40 C45 C44 4.7(10) . . . . ?
C41 C42 C43 C44 6.9(12) . . . . ?
C42 C43 C44 C45 -7.5(12) . . . . ?
C43 C44 C45 C40 1.6(12) . . . . ?
C43 C55 C56 C40 -3(2) . . . . ?
C45 C40 C41 C42 -5.4(11) . . . . ?
C46 N12 C38 C37 -179.0(3) . . . . ?
C46 C47 C48 C49 178.8(5) . . . . ?
C46 C47 C52 C51 -179.2(4) . . . . ?
C47 C48 C49 C50 0.7(8) . . . . ?
C48 C47 C52 C51 0.4(6) . . . . ?
C48 C49 C50 C51 -0.2(8) . . . . ?
C49 C50 C51 C52 -0.2(7) . . . . ?
C50 C51 C52 C47 0.1(7) . . . . ?
C52 C47 C48 C49 -0.7(7) . . . . ?
C53 C40 C56 C55 -8.2(17) . . . . ?
C55 C43 C54 C53 -13(2) . . . . ?
C56 C40 C53 C54 9.2(17) . . . . ?
C54 C43 C55 C56 14(2) . . . . ?

_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 -0.105 -0.709 0.014 275.9 79.4 ?
2 -0.050 0.868 0.499 14.5 0.8 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2

_ins_header                      
;
TITL jns2204 in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  10.832295  10.852309  13.366994  68.9420  77.7476  63.7803
ZERR    2.00   0.000698   0.001046   0.000981   0.0080   0.0059   0.0078
LATT  1
SFAC C H N O
UNIT 80.00 120.00 2.00 8.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
SIZE 0.06 0.24 0.29
TREF
HKLF 4
END
;
_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 1.475
_oxdiff_exptl_absorpt_empirical_full_min 0.736
####################################################################### 
# 
# 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_1_chloroform
_database_code_depnum_ccdc_archive 'CCDC 2373365'
loop_
_audit_author_name
_audit_author_address
'Nicholas White'
;Australian National University
Australia
;
_audit_update_record             
;
2024-07-25 deposited with the CCDC.	2025-02-05 downloaded from the CCDC.
;
#==============================================================================
# start Validation Reply Form
_vrf_THETM01_1_chloroform        
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: Crystals diffracted relatively weakly and it was only possible to
obtain data to a resolution of 0.87 A. Nevertheless, the structure refines 
well. No crystallographic restraints were necessary during refinement.
;
_vrf_PLAT340_1_chloroform        
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01386 Ang.  
RESPONSE: Crystals diffracted relatively weakly and it was only possible to
obtain data to a resolution of 0.87 A. Nevertheless, the structure refines 
well. No crystallographic restraints were necessary during refinement.
;
# end Validation Reply Form

_audit_creation_date             2023-06-01
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C52 H46 N12, 2(C H Cl3)'
_chemical_formula_sum            'C54 H48 Cl6 N12'
_chemical_formula_weight         1077.74
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C60 H80 N12'
_chemical_oxdiff_usercomment     jns_219_261

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'
Cl Cl 0.3639 0.7018 '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'

_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           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   10.6444(3)
_cell_length_b                   49.4450(13)
_cell_length_c                   11.0340(4)
_cell_angle_alpha                90
_cell_angle_beta                 115.695(4)
_cell_angle_gamma                90
_cell_volume                     5233.1(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2781
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      64.8110
_cell_measurement_theta_min      4.4350
_shelx_estimated_absorpt_T_max   0.876
_shelx_estimated_absorpt_T_min   0.648
_exptl_absorpt_coefficient_mu    3.394
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2232
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-7 -2 3 0.0512
2 -31 -1 0.0076
-1 31 1 0.0260
1 -2 -7 0.0364
6 3 -1 0.0409
-4 1 7 0.0756

_exptl_crystal_preparation       
'Crytals were grown by evaporation of a chloroform solution.'
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-6.8798 -2.4500 2.7844 0.3915 -0.4603 0.7968
1.9265 -30.7474 -1.2868 0.7357 0.6289 -0.2515
-1.3620 31.4624 0.6538 -0.7513 -0.6426 0.1506
1.2468 -2.1357 -6.8959 0.4652 -0.5410 -0.7007
6.4913 3.0489 -0.8005 -0.5226 0.6128 -0.5928
-4.1456 0.6832 7.0279 -0.2129 0.2453 0.9458

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0917
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       55
_diffrn_reflns_limit_k_min       -56
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            15475
_diffrn_reflns_point_group_measured_fraction_full 0.692
_diffrn_reflns_point_group_measured_fraction_max 0.692
_diffrn_reflns_theta_full        62.385
_diffrn_reflns_theta_max         62.385
_diffrn_reflns_theta_min         3.576
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -107.00  -7.00   1.00    7.50    --  -36.03 -19.00-150.00  100
  2  ω     32.00  89.00   1.00    7.50    --   36.03-125.00  90.00   57
  3  ω    105.00 154.00   1.00   27.50    --   93.63  77.00  90.00   49
  4  ω     36.00 108.00   1.00   27.50    --   93.63-111.00-180.00   72
  5  ω    121.00 161.00   1.00   27.50    --   93.63  77.00  30.00   40
  6  ω     26.00 106.00   1.00   27.50    --   93.63 -95.00 -60.00   80
  7  ω     27.00  89.00   1.00   27.50    --   93.63 -61.00   0.00   62
  8  ω    103.00 159.00   1.00   27.50    --   93.63  77.00-120.00   56
  9  ω     81.00 141.00   1.00   27.50    --   93.63  30.00-150.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0775017000
_diffrn_orient_matrix_UB_12      -0.0257067000
_diffrn_orient_matrix_UB_13      -0.0735089000
_diffrn_orient_matrix_UB_21      0.1155848000
_diffrn_orient_matrix_UB_22      -0.0175972000
_diffrn_orient_matrix_UB_23      0.1047968000
_diffrn_orient_matrix_UB_31      -0.0803257000
_diffrn_orient_matrix_UB_32      -0.0005051000
_diffrn_orient_matrix_UB_33      0.0872422000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.381
_reflns_Friedel_fraction_full    0.387
_reflns_Friedel_fraction_max     0.387
_reflns_number_gt                9540
_reflns_number_total             11518
_reflns_odcompleteness_completeness 98.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     62.30
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.882
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 
;
 Flack x determined using 2005 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.30(2)
_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     1305
_refine_ls_number_reflns         11518
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0715
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0863P)²+4.2408P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1716
_refine_ls_wR_factor_ref         0.1850
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Ternary CH refined with riding coordinates:
 C101(H101), C104(H104), C102(H102), C103(H103)
1.b Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B), C39(H39A,H39B), C13(H13A,H13B), C98(H98A,H98B), C20(H20A,
 H20B), C65(H65A,H65B), C72(H72A,H72B), C91(H91A,H91B)
1.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C30(H30), C90(H90), C82(H82), C56(H56), C88(H88), C36(H36), C62(H62),
 C12(H12), C10(H10), C38(H38), C64(H64), C67(H67), C52(H52), C94(H94), C93(H93),
  C95(H95), C24(H24), C19(H19), C16(H16), C48(H48), C15(H15), C50(H50),
 C49(H49), C51(H51), C69(H69), C68(H68), C71(H71), C18(H18), C108(H108),
 C70(H70), C25(H25), C78(H78), C17(H17), C45(H45), C100(H100), C23(H23),
 C96(H96), C41(H41), C106(H106), C97(H97), C22(H22), C107(H107), C105(H105),
 C26(H26), C77(H77), C44(H44), C74(H74), C43(H43), C42(H42), C75(H75), C76(H76)
1.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C86(H86A,H86B,H86C), C7(H7A,H7B,H7C), C59(H59A,H59B,
 H59C), C33(H33A,H33B,H33C), C85(H85A,H85B,H85C), C8(H8A,H8B,H8C), 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
Cl1 Cl 0.9705(3) 0.66859(7) 0.6700(3) 0.0473(7) Uani 1 1 d . . . . .
Cl2 Cl 1.2161(3) 0.63615(7) 0.7151(3) 0.0569(8) Uani 1 1 d . . . . .
Cl10 Cl 0.7172(3) 0.36724(6) 0.5545(3) 0.0537(7) Uani 1 1 d . . . . .
Cl4 Cl 0.7429(4) 0.54266(9) 0.8919(4) 0.0718(10) Uani 1 1 d . . . . .
Cl12 Cl 0.5835(4) 0.34113(8) 0.2979(3) 0.0662(9) Uani 1 1 d . . . . .
Cl9 Cl 0.6026(4) 0.48499(7) 0.2102(5) 0.0773(11) Uani 1 1 d . . . . .
Cl11 Cl 0.4495(4) 0.34137(10) 0.4739(4) 0.0821(12) Uani 1 1 d . . . . .
Cl3 Cl 1.0152(6) 0.65010(9) 0.4474(4) 0.1054(19) Uani 1 1 d . . . . .
Cl6 Cl 0.5507(4) 0.49873(9) 0.7866(6) 0.0925(13) Uani 1 1 d . . . . .
Cl7 Cl 0.8148(4) 0.52527(9) 0.3002(5) 0.0943(14) Uani 1 1 d . . . . .
Cl8 Cl 0.8655(5) 0.47622(9) 0.1928(5) 0.0929(14) Uani 1 1 d . . . . .
Cl5 Cl 0.6922(7) 0.51999(9) 0.6363(4) 0.1048(18) Uani 1 1 d . . . . .
N15 N 1.1722(7) 0.55996(16) 1.5917(7) 0.0236(15) Uani 1 1 d . . . . .
N17 N 1.6079(7) 0.67951(16) 1.4527(7) 0.0254(16) Uani 1 1 d . . . . .
N10 N 0.5875(6) 0.41893(16) 0.3158(7) 0.0235(15) Uani 1 1 d . . . . .
N18 N 1.5976(7) 0.68297(15) 1.3281(7) 0.0227(15) Uani 1 1 d . . . . .
N1 N 0.1170(7) 0.41124(16) -0.6081(7) 0.0229(15) Uani 1 1 d . . . . .
N24 N 0.6494(7) 0.57690(16) 0.4538(7) 0.0236(16) Uani 1 1 d . . . . .
N12 N 0.7707(6) 0.43702(15) 0.4681(7) 0.0220(15) Uani 1 1 d . . . . .
N9 N 1.1015(7) 0.31919(15) 0.1567(7) 0.0208(15) Uani 1 1 d . . . . .
N14 N 1.3092(6) 0.56105(16) 1.6258(7) 0.0226(15) Uani 1 1 d . . . . .
N16 N 1.5024(7) 0.66427(16) 1.4412(7) 0.0237(15) Uani 1 1 d . . . . .
N23 N 0.7837(7) 0.57792(16) 0.4762(7) 0.0255(16) Uani 1 1 d . . . . .
N6 N -0.0813(7) 0.30862(15) -0.3845(7) 0.0215(15) Uani 1 1 d . . . . .
N2 N 0.1084(6) 0.42543(16) -0.7102(7) 0.0243(16) Uani 1 1 d . . . . .
N7 N 1.0006(6) 0.33636(15) 0.2696(6) 0.0199(14) Uani 1 1 d . . . . .
N3 N 0.2383(7) 0.42970(15) -0.6961(7) 0.0218(15) Uani 1 1 d . . . . .
N8 N 1.1070(7) 0.32112(16) 0.2811(7) 0.0246(15) Uani 1 1 d . . . . .
N13 N 1.3242(7) 0.57718(16) 1.5368(7) 0.0237(15) Uani 1 1 d . . . . .
N11 N 0.6340(7) 0.43388(16) 0.4275(7) 0.0233(15) Uani 1 1 d . . . . .
N19 N 0.5628(7) 0.67407(16) 0.9590(7) 0.0240(16) Uani 1 1 d . . . . .
N21 N 0.4136(7) 0.69322(15) 0.7823(7) 0.0234(15) Uani 1 1 d . . . . .
N22 N 0.8519(7) 0.59123(17) 0.5893(7) 0.0269(17) Uani 1 1 d . . . . .
N5 N -0.0430(7) 0.31235(16) -0.2517(7) 0.0260(16) Uani 1 1 d . . . . .
N20 N 0.4520(7) 0.68938(17) 0.9131(7) 0.0273(16) Uani 1 1 d . . . . .
N4 N 0.0687(7) 0.32814(16) -0.2065(7) 0.0248(16) Uani 1 1 d . . . . .
C29 C 0.8045(7) 0.36184(17) 0.0997(8) 0.0174(16) Uani 1 1 d . . . . .
C4 C 0.1914(8) 0.37021(18) -0.4078(8) 0.0200(17) Uani 1 1 d . . . . .
H4 H 0.106420 0.368963 -0.487155 0.024 Uiso 1 1 calc R U . . .
C27 C 0.5718(7) 0.37673(17) -0.0496(8) 0.0182(16) Uani 1 1 d . . . . .
C9 C 0.2534(7) 0.40571(17) -0.5244(7) 0.0171(16) Uani 1 1 d . . . . .
C30 C 0.8038(8) 0.37923(17) 0.1966(8) 0.0188(16) Uani 1 1 d . . . . .
H30 H 0.883646 0.380121 0.280777 0.023 Uiso 1 1 calc R U . . .
C90 C 0.6298(8) 0.58921(17) 0.5519(8) 0.0181(16) Uani 1 1 d . . . . .
H90 H 0.544504 0.591044 0.559237 0.022 Uiso 1 1 calc R U . . .
C5 C 0.2118(8) 0.35329(17) -0.2998(7) 0.0169(16) Uani 1 1 d . . . . .
C81 C 0.7122(8) 0.64897(16) 0.8689(8) 0.0155(15) Uani 1 1 d . . . . .
C82 C 0.6918(8) 0.63328(18) 0.7590(7) 0.0184(16) Uani 1 1 d . . . . .
H82 H 0.607603 0.635160 0.679267 0.022 Uiso 1 1 calc R U . . .
C84 C 0.9180(8) 0.61187(18) 0.8811(7) 0.0179(16) Uani 1 1 d . . . . .
C2 C 0.4166(8) 0.39112(17) -0.2873(8) 0.0185(16) Uani 1 1 d . . . . .
C35 C 0.9283(8) 0.34412(17) 0.1375(8) 0.0194(17) Uani 1 1 d . . . . .
C37 C 0.6988(8) 0.41313(18) 0.2887(8) 0.0226(18) Uani 1 1 d . . . . .
C55 C 1.1858(8) 0.60495(17) 1.3404(7) 0.0183(17) Uani 1 1 d . . . . .
C83 C 0.7931(8) 0.61439(18) 0.7615(7) 0.0178(16) Uani 1 1 d . . . . .
C3 C 0.2912(8) 0.38885(16) -0.4035(8) 0.0168(16) Uani 1 1 d . . . . .
C56 C 1.2979(8) 0.62192(16) 1.3639(8) 0.0163(16) Uani 1 1 d . . . . .
H56 H 1.377184 0.620949 1.448495 0.020 Uiso 1 1 calc R U . . .
C28 C 0.6880(8) 0.36056(18) -0.0266(8) 0.0200(17) Uani 1 1 d . . . . .
C79 C 0.9374(8) 0.62871(17) 0.9910(8) 0.0190(16) Uani 1 1 d . . . . .
C80 C 0.8372(8) 0.64727(18) 0.9871(8) 0.0208(17) Uani 1 1 d . . . . .
C57 C 1.2991(7) 0.64031(16) 1.2689(7) 0.0160(16) Uani 1 1 d . . . . .
C1 C 0.4403(8) 0.37416(17) -0.1787(7) 0.0173(16) Uani 1 1 d . . . . .
C88 C 0.4986(8) 0.67975(18) 0.7401(8) 0.0213(17) Uani 1 1 d . . . . .
H88 H 0.492491 0.678947 0.651695 0.026 Uiso 1 1 calc R U . . .
C87 C 0.5961(8) 0.66747(18) 0.8549(8) 0.0207(17) Uani 1 1 d . . . . .
C6 C 0.3395(8) 0.35500(17) -0.1839(8) 0.0200(17) Uani 1 1 d . . . . .
C61 C 1.1969(8) 0.58612(17) 1.4476(8) 0.0184(17) Uani 1 1 d . . . . .
C36 C 0.9932(8) 0.33283(18) 0.0659(8) 0.0212(17) Uani 1 1 d . . . . .
H36 H 0.966899 0.334389 -0.027861 0.025 Uiso 1 1 calc R U . . .
C54 C 1.0655(8) 0.60711(18) 1.2158(8) 0.0191(17) Uani 1 1 d . . . . .
C89 C 0.7586(8) 0.59869(18) 0.6400(8) 0.0201(17) Uani 1 1 d . . . . .
C63 C 1.4236(8) 0.65779(17) 1.3086(8) 0.0196(17) Uani 1 1 d . . . . .
C62 C 1.0991(8) 0.57497(18) 1.4843(9) 0.0230(18) Uani 1 1 d . . . . .
H62 H 1.000959 0.577515 1.441766 0.028 Uiso 1 1 calc R U . . .
C53 C 1.0670(8) 0.62549(18) 1.1198(8) 0.0189(16) Uani 1 1 d . . . . .
C12 C 0.0036(8) 0.32233(19) -0.4259(8) 0.0220(18) Uani 1 1 d . . . . .
H12 H -0.001770 0.323139 -0.514031 0.026 Uiso 1 1 calc R U . . .
C14 C 0.2411(8) 0.4751(2) -0.7885(8) 0.0245(18) Uani 1 1 d . . . . .
C32 C 0.5694(8) 0.39473(18) 0.0490(8) 0.0198(17) Uani 1 1 d . . . . .
C10 C 0.3330(8) 0.41786(19) -0.5809(8) 0.0236(18) Uani 1 1 d . . . . .
H10 H 0.431693 0.417913 -0.546963 0.028 Uiso 1 1 calc R U . . .
C38 C 0.8162(8) 0.42460(19) 0.3852(9) 0.0253(19) Uani 1 1 d . . . . .
H38 H 0.908436 0.424010 0.392552 0.030 Uiso 1 1 calc R U . . .
C92 C 0.2958(8) 0.7373(2) 0.7565(9) 0.0261(19) Uani 1 1 d . . . . .
C58 C 1.1833(8) 0.64201(18) 1.1429(8) 0.0221(18) Uani 1 1 d . . . . .
C11 C 0.0987(8) 0.33476(18) -0.3121(8) 0.0207(17) Uani 1 1 d . . . . .
C31 C 0.6871(7) 0.39593(17) 0.1745(7) 0.0175(16) Uani 1 1 d . . . . .
C47 C 0.8979(8) 0.43507(19) 0.7170(8) 0.0249(18) Uani 1 1 d . . . . .
C34 C 0.4435(8) 0.4120(2) 0.0192(9) 0.028(2) Uani 1 1 d . . . . .
H34A H 0.382108 0.402871 0.051579 0.043 Uiso 1 1 calc R U . . .
H34B H 0.393403 0.414850 -0.078075 0.043 Uiso 1 1 calc R U . . .
H34C H 0.472860 0.429454 0.064619 0.043 Uiso 1 1 calc R U . . .
C64 C 1.4857(8) 0.67000(18) 1.2370(8) 0.0227(17) Uani 1 1 d . . . . .
H64 H 1.455762 0.669402 1.142407 0.027 Uiso 1 1 calc R U . . .
C46 C 0.8524(8) 0.45208(19) 0.5933(8) 0.0253(19) Uani 1 1 d . . . . .
H46A H 0.795369 0.467291 0.600209 0.030 Uiso 1 1 calc R U . . .
H46B H 0.935854 0.459829 0.588470 0.030 Uiso 1 1 calc R U . . .
C86 C 1.0276(9) 0.5915(2) 0.8938(9) 0.028(2) Uani 1 1 d . . . . .
H86A H 0.984968 0.576844 0.828709 0.042 Uiso 1 1 calc R U . . .
H86B H 1.068861 0.583974 0.985027 0.042 Uiso 1 1 calc R U . . .
H86C H 1.100305 0.600229 0.875776 0.042 Uiso 1 1 calc R U . . .
C39 C 1.2073(8) 0.30299(19) 0.1352(9) 0.0258(19) Uani 1 1 d . . . . .
H39A H 1.301347 0.307643 0.205052 0.031 Uiso 1 1 calc R U . . .
H39B H 1.203901 0.307530 0.046402 0.031 Uiso 1 1 calc R U . . .
C40 C 1.1825(8) 0.27313(19) 0.1409(9) 0.0256(19) Uani 1 1 d . . . . .
C99 C 0.5295(8) 0.5737(2) 0.2048(9) 0.0278(19) Uani 1 1 d . . . . .
C7 C 0.5271(8) 0.4117(2) -0.2770(9) 0.028(2) Uani 1 1 d . . . . .
H7A H 0.576507 0.405388 -0.328658 0.042 Uiso 1 1 calc R U . . .
H7B H 0.593655 0.413990 -0.182462 0.042 Uiso 1 1 calc R U . . .
H7C H 0.482385 0.429136 -0.313105 0.042 Uiso 1 1 calc R U . . .
C67 C 1.1536(9) 0.5004(2) 1.5704(8) 0.0284(19) Uani 1 1 d . . . . .
H67 H 1.123338 0.509451 1.486642 0.034 Uiso 1 1 calc R U . . .
C66 C 1.1623(9) 0.51449(19) 1.6822(9) 0.0265(19) Uani 1 1 d . . . . .
C13 C 0.2623(8) 0.44567(19) -0.7967(8) 0.0232(18) Uani 1 1 d . . . . .
H13A H 0.198304 0.439203 -0.887646 0.028 Uiso 1 1 calc R U . . .
H13B H 0.358894 0.442514 -0.784594 0.028 Uiso 1 1 calc R U . . .
C59 C 0.9399(8) 0.5897(2) 1.1865(9) 0.0280(19) Uani 1 1 d . . . . .
H59A H 0.969793 0.571090 1.214798 0.042 Uiso 1 1 calc R U . . .
H59B H 0.878716 0.590051 1.089827 0.042 Uiso 1 1 calc R U . . .
H59C H 0.889203 0.596653 1.235908 0.042 Uiso 1 1 calc R U . . .
C52 C 0.8566(9) 0.4415(2) 0.8175(10) 0.035(2) Uani 1 1 d . . . . .
H52 H 0.798079 0.456646 0.807142 0.042 Uiso 1 1 calc R U . . .
C94 C 0.4151(10) 0.7790(2) 0.8421(10) 0.037(2) Uani 1 1 d . . . . .
H94 H 0.497751 0.789538 0.870830 0.044 Uiso 1 1 calc R U . . .
C33 C 0.6846(8) 0.3416(2) -0.1358(8) 0.028(2) Uani 1 1 d . . . . .
H33A H 0.745780 0.348531 -0.174070 0.042 Uiso 1 1 calc R U . . .
H33B H 0.588995 0.340272 -0.206631 0.042 Uiso 1 1 calc R U . . .
H33C H 0.716697 0.323598 -0.097278 0.042 Uiso 1 1 calc R U . . .
C93 C 0.4145(9) 0.7531(2) 0.7974(9) 0.032(2) Uani 1 1 d . . . . .
H93 H 0.496058 0.745975 0.794582 0.038 Uiso 1 1 calc R U . . .
C95 C 0.2996(11) 0.7900(2) 0.8459(10) 0.038(2) Uani 1 1 d . . . . .
H95 H 0.301401 0.808053 0.875504 0.046 Uiso 1 1 calc R U . . .
C24 C -0.1893(10) 0.2099(2) -0.3285(10) 0.034(2) Uani 1 1 d . . . . .
H24 H -0.185584 0.191495 -0.303076 0.041 Uiso 1 1 calc R U . . .
C73 C 1.6762(10) 0.7294(2) 1.3126(10) 0.033(2) Uani 1 1 d . . . . .
C19 C 0.3160(10) 0.4894(2) -0.6708(9) 0.034(2) Uani 1 1 d . . . . .
H19 H 0.382674 0.480307 -0.594109 0.041 Uiso 1 1 calc R U . . .
C85 C 0.8634(9) 0.6649(2) 1.1048(8) 0.029(2) Uani 1 1 d . . . . .
H85A H 0.825883 0.656280 1.162139 0.044 Uiso 1 1 calc R U . . .
H85B H 0.817524 0.682423 1.073443 0.044 Uiso 1 1 calc R U . . .
H85C H 0.963942 0.667688 1.156489 0.044 Uiso 1 1 calc R U . . .
C98 C 0.5448(9) 0.5628(2) 0.3365(8) 0.029(2) Uani 1 1 d . . . . .
H98A H 0.453503 0.564049 0.339772 0.035 Uiso 1 1 calc R U . . .
H98B H 0.570313 0.543477 0.342128 0.035 Uiso 1 1 calc R U . . .
C16 C 0.1293(11) 0.5166(2) -0.8930(13) 0.048(3) Uani 1 1 d . . . . .
H16 H 0.068461 0.526056 -0.971494 0.058 Uiso 1 1 calc R U . . .
C48 C 0.9852(10) 0.4126(2) 0.7365(10) 0.034(2) Uani 1 1 d . . . . .
H48 H 1.016108 0.408045 0.670165 0.041 Uiso 1 1 calc R U . . .
C15 C 0.1452(10) 0.4890(2) -0.8988(10) 0.035(2) Uani 1 1 d . . . . .
H15 H 0.089827 0.479476 -0.979122 0.042 Uiso 1 1 calc R U . . .
C50 C 0.9839(10) 0.4034(2) 0.9488(10) 0.037(2) Uani 1 1 d . . . . .
H50 H 1.011870 0.392566 1.027166 0.044 Uiso 1 1 calc R U . . .
C8 C 0.3708(9) 0.3365(2) -0.0648(8) 0.0281(19) Uani 1 1 d . . . . .
H8A H 0.471893 0.334194 -0.014823 0.042 Uiso 1 1 calc R U . . .
H8B H 0.327064 0.318856 -0.096870 0.042 Uiso 1 1 calc R U . . .
H8C H 0.333692 0.344490 -0.005743 0.042 Uiso 1 1 calc R U . . .
C20 C -0.2073(9) 0.2926(2) -0.4631(10) 0.033(2) Uani 1 1 d . . . . .
H20A H -0.222393 0.292088 -0.558178 0.040 Uiso 1 1 calc R U . . .
H20B H -0.288889 0.301613 -0.460034 0.040 Uiso 1 1 calc R U . . .
C49 C 1.0263(11) 0.3971(2) 0.8507(10) 0.042(2) Uani 1 1 d . . . . .
H49 H 1.084571 0.381813 0.862080 0.050 Uiso 1 1 calc R U . . .
C51 C 0.9005(10) 0.4258(2) 0.9319(10) 0.040(2) Uani 1 1 d . . . . .
H51 H 0.872773 0.430446 1.000296 0.048 Uiso 1 1 calc R U . . .
C60 C 1.1798(9) 0.6616(2) 1.0380(9) 0.030(2) Uani 1 1 d . . . . .
H60A H 1.223701 0.678662 1.081276 0.045 Uiso 1 1 calc R U . . .
H60B H 1.082824 0.665069 0.974105 0.045 Uiso 1 1 calc R U . . .
H60C H 1.230608 0.654058 0.990129 0.045 Uiso 1 1 calc R U . . .
C69 C 1.2327(10) 0.4599(2) 1.7035(11) 0.039(2) Uani 1 1 d . . . . .
H69 H 1.257643 0.441285 1.711193 0.047 Uiso 1 1 calc R U . . .
C68 C 1.1881(10) 0.4734(2) 1.5787(11) 0.036(2) Uani 1 1 d . . . . .
H68 H 1.182130 0.464007 1.501403 0.043 Uiso 1 1 calc R U . . .
C65 C 1.1215(9) 0.5437(2) 1.6744(10) 0.031(2) Uani 1 1 d . . . . .
H65A H 1.018602 0.545030 1.635520 0.037 Uiso 1 1 calc R U . . .
H65B H 1.159835 0.551315 1.766451 0.037 Uiso 1 1 calc R U . . .
C71 C 1.2083(10) 0.5007(2) 1.8038(9) 0.033(2) Uani 1 1 d . . . . .
H71 H 1.218306 0.510196 1.882407 0.039 Uiso 1 1 calc R U . . .
C18 C 0.2949(12) 0.5166(2) -0.6639(11) 0.044(3) Uani 1 1 d . . . . .
H18 H 0.345647 0.526024 -0.581862 0.052 Uiso 1 1 calc R U . . .
C108 C 0.4755(10) 0.5562(2) 0.0914(9) 0.036(2) Uani 1 1 d . . . . .
H108 H 0.451271 0.538054 0.100616 0.043 Uiso 1 1 calc R U . . .
C70 C 1.2392(11) 0.4739(2) 1.8121(11) 0.040(2) Uani 1 1 d . . . . .
H70 H 1.265897 0.464774 1.895401 0.048 Uiso 1 1 calc R U . . .
C25 C -0.3092(12) 0.2254(2) -0.3593(13) 0.046(3) Uani 1 1 d . . . . .
H25 H -0.387274 0.217724 -0.351534 0.055 Uiso 1 1 calc R U . . .
C78 C 1.7570(11) 0.7445(3) 1.4250(10) 0.045(3) Uani 1 1 d . . . . .
H78 H 1.828904 0.736001 1.500482 0.054 Uiso 1 1 calc R U . . .
C72 C 1.6997(9) 0.7000(2) 1.3037(10) 0.033(2) Uani 1 1 d . . . . .
H72A H 1.795116 0.695357 1.370671 0.039 Uiso 1 1 calc R U . . .
H72B H 1.693014 0.695911 1.213321 0.039 Uiso 1 1 calc R U . . .
C91 C 0.2900(9) 0.7091(2) 0.7003(9) 0.030(2) Uani 1 1 d . . . . .
H91A H 0.205963 0.699729 0.695716 0.036 Uiso 1 1 calc R U . . .
H91B H 0.281820 0.710547 0.607655 0.036 Uiso 1 1 calc R U . . .
C17 C 0.2012(11) 0.5306(2) -0.7741(12) 0.044(3) Uani 1 1 d . . . . .
H17 H 0.186207 0.549404 -0.768688 0.053 Uiso 1 1 calc R U . . .
C45 C 1.2607(11) 0.2580(2) 0.2542(11) 0.042(3) Uani 1 1 d . . . . .
H45 H 1.330104 0.266432 0.331650 0.051 Uiso 1 1 calc R U . . .
C21 C -0.1974(9) 0.2640(2) -0.4116(9) 0.031(2) Uani 1 1 d . . . . .
C100 C 0.5616(11) 0.6001(2) 0.1845(11) 0.040(2) Uani 1 1 d . . . . .
H100 H 0.596994 0.612126 0.258808 0.048 Uiso 1 1 calc R U . . .
C23 C -0.0762(11) 0.2222(2) -0.3360(11) 0.042(3) Uani 1 1 d . . . . .
H23 H 0.007313 0.212096 -0.311292 0.050 Uiso 1 1 calc R U . . .
C96 C 0.1804(12) 0.7747(2) 0.8068(13) 0.049(3) Uani 1 1 d . . . . .
H96 H 0.099510 0.782180 0.809843 0.059 Uiso 1 1 calc R U . . .
C41 C 1.0792(13) 0.2598(3) 0.0323(11) 0.050(3) Uani 1 1 d . . . . .
H41 H 1.021858 0.269826 -0.045685 0.060 Uiso 1 1 calc R U . . .
C106 C 0.4932(12) 0.5916(3) -0.0501(11) 0.046(3) Uani 1 1 d . . . . .
H106 H 0.483272 0.597544 -0.135646 0.055 Uiso 1 1 calc R U . . .
C97 C 0.1791(10) 0.7485(2) 0.7630(11) 0.039(2) Uani 1 1 d . . . . .
H97 H 0.096967 0.737901 0.736816 0.047 Uiso 1 1 calc R U . . .
C22 C -0.0807(10) 0.2481(2) -0.3776(11) 0.042(3) Uani 1 1 d . . . . .
H22 H -0.001134 0.255530 -0.383393 0.050 Uiso 1 1 calc R U . . .
C107 C 0.4586(11) 0.5657(3) -0.0311(10) 0.046(3) Uani 1 1 d . . . . .
H107 H 0.421406 0.553926 -0.106412 0.055 Uiso 1 1 calc R U . . .
C101 C 1.0399(11) 0.6420(2) 0.6081(11) 0.041(2) Uani 1 1 d . . . . .
H101 H 0.986466 0.625112 0.603737 0.049 Uiso 1 1 calc R U . . .
C105 C 0.5439(11) 0.6091(3) 0.0621(11) 0.047(3) Uani 1 1 d . . . . .
H105 H 0.565755 0.627358 0.051860 0.057 Uiso 1 1 calc R U . . .
C26 C -0.3137(11) 0.2525(3) -0.4020(12) 0.047(3) Uani 1 1 d . . . . .
H26 H -0.395629 0.262922 -0.424424 0.056 Uiso 1 1 calc R U . . .
C77 C 1.7330(15) 0.7721(3) 1.4274(14) 0.060(4) Uani 1 1 d . . . . .
H77 H 1.789397 0.782307 1.504957 0.071 Uiso 1 1 calc R U . . .
C44 C 1.2367(15) 0.2299(3) 0.2537(14) 0.056(4) Uani 1 1 d . . . . .
H44 H 1.291253 0.219391 0.330642 0.068 Uiso 1 1 calc R U . . .
C74 C 1.5689(13) 0.7427(3) 1.2035(11) 0.050(3) Uani 1 1 d . . . . .
H74 H 1.511913 0.732734 1.125143 0.060 Uiso 1 1 calc R U . . .
C43 C 1.1393(18) 0.2183(3) 0.1476(16) 0.065(4) Uani 1 1 d . . . . .
H43 H 1.124810 0.199393 0.149353 0.078 Uiso 1 1 calc R U . . .
C42 C 1.0585(18) 0.2326(3) 0.0355(15) 0.071(4) Uani 1 1 d . . . . .
H42 H 0.988472 0.223720 -0.039930 0.086 Uiso 1 1 calc R U . . .
C104 C 0.5560(11) 0.3590(3) 0.4172(13) 0.056(3) Uani 1 1 d . . . . .
H104 H 0.507912 0.376327 0.375374 0.067 Uiso 1 1 calc R U . . .
C75 C 1.5464(19) 0.7697(3) 1.2097(15) 0.072(4) Uani 1 1 d . . . . .
H75 H 1.472208 0.778369 1.136843 0.087 Uiso 1 1 calc R U . . .
C102 C 0.6214(12) 0.5276(3) 0.7449(11) 0.051(3) Uani 1 1 d . . . . .
H102 H 0.543906 0.540797 0.699214 0.061 Uiso 1 1 calc R U . . .
C76 C 1.6315(17) 0.7846(3) 1.3222(16) 0.063(4) Uani 1 1 d . . . . .
H76 H 1.618077 0.803575 1.324925 0.076 Uiso 1 1 calc R U . . .
C103 C 0.7351(12) 0.4997(2) 0.1798(13) 0.051(3) Uani 1 1 d . . . . .
H103 H 0.694121 0.507841 0.087838 0.061 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C101 1.781(11) . ?
Cl2 C101 1.754(11) . ?
Cl10 C104 1.774(12) . ?
Cl4 C102 1.743(12) . ?
Cl12 C104 1.714(14) . ?
Cl9 C103 1.743(12) . ?
Cl11 C104 1.749(13) . ?
Cl3 C101 1.724(11) . ?
Cl6 C102 1.765(14) . ?
Cl7 C103 1.763(13) . ?
Cl8 C103 1.766(12) . ?
Cl5 C102 1.712(12) . ?
N15 N14 1.340(10) . ?
N15 C62 1.327(11) . ?
N15 C65 1.482(11) . ?
N17 N18 1.342(10) . ?
N17 N16 1.312(10) . ?
N10 N11 1.335(10) . ?
N10 C37 1.372(10) . ?
N18 C64 1.343(11) . ?
N18 C72 1.489(11) . ?
N1 N2 1.296(10) . ?
N1 C9 1.369(10) . ?
N24 N23 1.342(10) . ?
N24 C90 1.334(11) . ?
N24 C98 1.466(10) . ?
N12 N11 1.333(9) . ?
N12 C38 1.353(11) . ?
N12 C46 1.475(11) . ?
N9 N8 1.352(10) . ?
N9 C36 1.336(11) . ?
N9 C39 1.483(10) . ?
N14 N13 1.328(10) . ?
N16 C63 1.373(11) . ?
N23 N22 1.316(10) . ?
N6 N5 1.352(10) . ?
N6 C12 1.357(11) . ?
N6 C20 1.473(11) . ?
N2 N3 1.340(9) . ?
N7 N8 1.320(10) . ?
N7 C35 1.376(11) . ?
N3 C10 1.365(11) . ?
N3 C13 1.472(11) . ?
N13 C61 1.358(11) . ?
N19 N20 1.305(10) . ?
N19 C87 1.381(10) . ?
N21 N20 1.332(10) . ?
N21 C88 1.358(11) . ?
N21 C91 1.462(11) . ?
N22 C89 1.385(10) . ?
N5 N4 1.326(10) . ?
N4 C11 1.374(10) . ?
C29 C30 1.375(12) . ?
C29 C35 1.484(11) . ?
C29 C28 1.408(11) . ?
C4 H4 0.9500 . ?
C4 C5 1.394(11) . ?
C4 C3 1.391(11) . ?
C27 C28 1.400(12) . ?
C27 C1 1.509(10) . ?
C27 C32 1.414(12) . ?
C9 C3 1.473(11) . ?
C9 C10 1.388(11) . ?
C30 H30 0.9500 . ?
C30 C31 1.422(11) . ?
C90 H90 0.9500 . ?
C90 C89 1.374(12) . ?
C5 C6 1.408(11) . ?
C5 C11 1.472(11) . ?
C81 C82 1.375(11) . ?
C81 C80 1.405(11) . ?
C81 C87 1.490(11) . ?
C82 H82 0.9500 . ?
C82 C83 1.418(11) . ?
C84 C83 1.416(11) . ?
C84 C79 1.410(12) . ?
C84 C86 1.503(12) . ?
C2 C3 1.398(11) . ?
C2 C1 1.393(11) . ?
C2 C7 1.524(12) . ?
C35 C36 1.374(11) . ?
C37 C38 1.366(12) . ?
C37 C31 1.480(12) . ?
C55 C56 1.388(11) . ?
C55 C61 1.469(11) . ?
C55 C54 1.420(11) . ?
C83 C89 1.452(11) . ?
C56 H56 0.9500 . ?
C56 C57 1.392(11) . ?
C28 C33 1.516(12) . ?
C79 C80 1.393(12) . ?
C79 C53 1.499(11) . ?
C80 C85 1.488(11) . ?
C57 C63 1.481(11) . ?
C57 C58 1.404(11) . ?
C1 C6 1.413(12) . ?
C88 H88 0.9500 . ?
C88 C87 1.382(12) . ?
C6 C8 1.515(12) . ?
C61 C62 1.385(11) . ?
C36 H36 0.9500 . ?
C54 C53 1.401(12) . ?
C54 C59 1.503(12) . ?
C63 C64 1.371(12) . ?
C62 H62 0.9500 . ?
C53 C58 1.411(12) . ?
C12 H12 0.9500 . ?
C12 C11 1.370(12) . ?
C14 C13 1.482(13) . ?
C14 C19 1.388(13) . ?
C14 C15 1.385(13) . ?
C32 C31 1.409(11) . ?
C32 C34 1.500(11) . ?
C10 H10 0.9500 . ?
C38 H38 0.9500 . ?
C92 C93 1.385(14) . ?
C92 C91 1.513(14) . ?
C92 C97 1.390(13) . ?
C58 C60 1.499(12) . ?
C47 C46 1.494(13) . ?
C47 C52 1.395(13) . ?
C47 C48 1.405(14) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C64 H64 0.9500 . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C86 H86A 0.9800 . ?
C86 H86B 0.9800 . ?
C86 H86C 0.9800 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.506(13) . ?
C40 C45 1.384(14) . ?
C40 C41 1.392(15) . ?
C99 C98 1.490(13) . ?
C99 C108 1.421(13) . ?
C99 C100 1.391(15) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C67 H67 0.9500 . ?
C67 C66 1.385(13) . ?
C67 C68 1.373(15) . ?
C66 C65 1.500(13) . ?
C66 C71 1.391(13) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C52 H52 0.9500 . ?
C52 C51 1.379(15) . ?
C94 H94 0.9500 . ?
C94 C93 1.372(15) . ?
C94 C95 1.360(15) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C93 H93 0.9500 . ?
C95 H95 0.9500 . ?
C95 C96 1.374(17) . ?
C24 H24 0.9500 . ?
C24 C25 1.397(15) . ?
C24 C23 1.381(15) . ?
C73 C78 1.382(14) . ?
C73 C72 1.484(15) . ?
C73 C74 1.412(16) . ?
C19 H19 0.9500 . ?
C19 C18 1.371(16) . ?
C85 H85A 0.9800 . ?
C85 H85B 0.9800 . ?
C85 H85C 0.9800 . ?
C98 H98A 0.9900 . ?
C98 H98B 0.9900 . ?
C16 H16 0.9500 . ?
C16 C15 1.377(15) . ?
C16 C17 1.384(17) . ?
C48 H48 0.9500 . ?
C48 C49 1.374(15) . ?
C15 H15 0.9500 . ?
C50 H50 0.9500 . ?
C50 C49 1.378(15) . ?
C50 C51 1.378(16) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.511(15) . ?
C49 H49 0.9500 . ?
C51 H51 0.9500 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C69 H69 0.9500 . ?
C69 C68 1.415(15) . ?
C69 C70 1.360(16) . ?
C68 H68 0.9500 . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C71 H71 0.9500 . ?
C71 C70 1.360(15) . ?
C18 H18 0.9500 . ?
C18 C17 1.378(17) . ?
C108 H108 0.9500 . ?
C108 C107 1.369(15) . ?
C70 H70 0.9500 . ?
C25 H25 0.9500 . ?
C25 C26 1.413(18) . ?
C78 H78 0.9500 . ?
C78 C77 1.39(2) . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
C91 H91A 0.9900 . ?
C91 H91B 0.9900 . ?
C17 H17 0.9500 . ?
C45 H45 0.9500 . ?
C45 C44 1.410(18) . ?
C21 C22 1.378(15) . ?
C21 C26 1.408(14) . ?
C100 H100 0.9500 . ?
C100 C105 1.356(15) . ?
C23 H23 0.9500 . ?
C23 C22 1.356(16) . ?
C96 H96 0.9500 . ?
C96 C97 1.384(17) . ?
C41 H41 0.9500 . ?
C41 C42 1.37(2) . ?
C106 H106 0.9500 . ?
C106 C107 1.372(19) . ?
C106 C105 1.412(17) . ?
C97 H97 0.9500 . ?
C22 H22 0.9500 . ?
C107 H107 0.9500 . ?
C101 H101 1.0000 . ?
C105 H105 0.9500 . ?
C26 H26 0.9500 . ?
C77 H77 0.9500 . ?
C77 C76 1.35(2) . ?
C44 H44 0.9500 . ?
C44 C43 1.31(2) . ?
C74 H74 0.9500 . ?
C74 C75 1.37(2) . ?
C43 H43 0.9500 . ?
C43 C42 1.36(2) . ?
C42 H42 0.9500 . ?
C104 H104 1.0000 . ?
C75 H75 0.9500 . ?
C75 C76 1.39(2) . ?
C102 H102 1.0000 . ?
C76 H76 0.9500 . ?
C103 H103 1.0000 . ?

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
N14 N15 C65 119.5(7) . . ?
C62 N15 N14 111.9(7) . . ?
C62 N15 C65 128.6(7) . . ?
N16 N17 N18 106.7(6) . . ?
N11 N10 C37 107.9(6) . . ?
N17 N18 C64 111.0(7) . . ?
N17 N18 C72 121.0(7) . . ?
C64 N18 C72 128.0(7) . . ?
N2 N1 C9 110.4(6) . . ?
N23 N24 C98 121.4(7) . . ?
C90 N24 N23 111.2(7) . . ?
C90 N24 C98 127.4(7) . . ?
N11 N12 C38 112.2(7) . . ?
N11 N12 C46 119.2(6) . . ?
C38 N12 C46 128.5(6) . . ?
N8 N9 C39 120.0(7) . . ?
C36 N9 N8 111.7(6) . . ?
C36 N9 C39 128.3(7) . . ?
N13 N14 N15 106.4(6) . . ?
N17 N16 C63 109.8(6) . . ?
N22 N23 N24 107.4(6) . . ?
N5 N6 C12 111.4(7) . . ?
N5 N6 C20 118.8(7) . . ?
C12 N6 C20 129.7(7) . . ?
N1 N2 N3 107.7(6) . . ?
N8 N7 C35 108.9(6) . . ?
N2 N3 C10 110.4(6) . . ?
N2 N3 C13 120.3(7) . . ?
C10 N3 C13 129.3(7) . . ?
N7 N8 N9 106.6(6) . . ?
N14 N13 C61 109.2(6) . . ?
N12 N11 N10 106.8(6) . . ?
N20 N19 C87 109.2(7) . . ?
N20 N21 C88 111.4(7) . . ?
N20 N21 C91 121.2(7) . . ?
C88 N21 C91 127.4(7) . . ?
N23 N22 C89 108.6(6) . . ?
N4 N5 N6 106.7(6) . . ?
N19 N20 N21 107.7(6) . . ?
N5 N4 C11 108.7(7) . . ?
C30 C29 C35 117.0(7) . . ?
C30 C29 C28 119.9(7) . . ?
C28 C29 C35 123.0(7) . . ?
C5 C4 H4 118.8 . . ?
C3 C4 H4 118.8 . . ?
C3 C4 C5 122.3(8) . . ?
C28 C27 C1 120.5(7) . . ?
C28 C27 C32 121.9(7) . . ?
C32 C27 C1 117.4(7) . . ?
N1 C9 C3 121.2(6) . . ?
N1 C9 C10 106.6(7) . . ?
C10 C9 C3 132.2(7) . . ?
C29 C30 H30 119.0 . . ?
C29 C30 C31 121.9(7) . . ?
C31 C30 H30 119.0 . . ?
N24 C90 H90 127.2 . . ?
N24 C90 C89 105.7(7) . . ?
C89 C90 H90 127.2 . . ?
C4 C5 C6 118.1(7) . . ?
C4 C5 C11 118.5(7) . . ?
C6 C5 C11 123.4(7) . . ?
C82 C81 C80 120.5(7) . . ?
C82 C81 C87 116.6(7) . . ?
C80 C81 C87 122.8(7) . . ?
C81 C82 H82 119.1 . . ?
C81 C82 C83 121.8(7) . . ?
C83 C82 H82 119.1 . . ?
C83 C84 C86 121.5(7) . . ?
C79 C84 C83 118.6(7) . . ?
C79 C84 C86 119.9(7) . . ?
C3 C2 C7 121.4(7) . . ?
C1 C2 C3 119.0(7) . . ?
C1 C2 C7 119.5(7) . . ?
N7 C35 C29 118.9(6) . . ?
C36 C35 N7 107.8(7) . . ?
C36 C35 C29 133.3(7) . . ?
N10 C37 C31 123.0(7) . . ?
C38 C37 N10 109.1(7) . . ?
C38 C37 C31 127.8(7) . . ?
C56 C55 C61 118.0(7) . . ?
C56 C55 C54 118.5(7) . . ?
C54 C55 C61 123.5(7) . . ?
C82 C83 C89 116.7(7) . . ?
C84 C83 C82 118.4(7) . . ?
C84 C83 C89 125.0(7) . . ?
C4 C3 C9 116.1(7) . . ?
C4 C3 C2 119.7(7) . . ?
C2 C3 C9 124.2(7) . . ?
C55 C56 H56 118.6 . . ?
C55 C56 C57 122.8(7) . . ?
C57 C56 H56 118.6 . . ?
C29 C28 C33 121.4(7) . . ?
C27 C28 C29 118.9(7) . . ?
C27 C28 C33 119.7(7) . . ?
C84 C79 C53 118.9(7) . . ?
C80 C79 C84 122.5(7) . . ?
C80 C79 C53 118.5(7) . . ?
C81 C80 C85 121.2(7) . . ?
C79 C80 C81 118.2(7) . . ?
C79 C80 C85 120.6(7) . . ?
C56 C57 C63 117.2(7) . . ?
C56 C57 C58 119.6(7) . . ?
C58 C57 C63 123.1(7) . . ?
C2 C1 C27 120.6(7) . . ?
C2 C1 C6 121.2(7) . . ?
C6 C1 C27 118.2(7) . . ?
N21 C88 H88 127.8 . . ?
N21 C88 C87 104.4(7) . . ?
C87 C88 H88 127.8 . . ?
N19 C87 C81 124.0(7) . . ?
N19 C87 C88 107.3(7) . . ?
C88 C87 C81 128.6(7) . . ?
C5 C6 C1 119.6(7) . . ?
C5 C6 C8 120.9(7) . . ?
C1 C6 C8 119.5(7) . . ?
N13 C61 C55 119.8(7) . . ?
N13 C61 C62 107.4(7) . . ?
C62 C61 C55 132.8(7) . . ?
N9 C36 C35 105.0(7) . . ?
N9 C36 H36 127.5 . . ?
C35 C36 H36 127.5 . . ?
C55 C54 C59 120.6(7) . . ?
C53 C54 C55 118.7(7) . . ?
C53 C54 C59 120.6(7) . . ?
N22 C89 C83 125.2(7) . . ?
C90 C89 N22 107.1(7) . . ?
C90 C89 C83 127.7(7) . . ?
N16 C63 C57 120.4(7) . . ?
C64 C63 N16 106.7(7) . . ?
C64 C63 C57 132.9(8) . . ?
N15 C62 C61 105.1(7) . . ?
N15 C62 H62 127.5 . . ?
C61 C62 H62 127.5 . . ?
C54 C53 C79 118.6(7) . . ?
C54 C53 C58 122.4(7) . . ?
C58 C53 C79 119.0(7) . . ?
N6 C12 H12 127.7 . . ?
N6 C12 C11 104.5(7) . . ?
C11 C12 H12 127.7 . . ?
C19 C14 C13 121.2(8) . . ?
C15 C14 C13 120.5(8) . . ?
C15 C14 C19 118.3(9) . . ?
C27 C32 C34 120.1(7) . . ?
C31 C32 C27 118.5(7) . . ?
C31 C32 C34 121.4(7) . . ?
N3 C10 C9 104.8(7) . . ?
N3 C10 H10 127.6 . . ?
C9 C10 H10 127.6 . . ?
N12 C38 C37 103.9(7) . . ?
N12 C38 H38 128.0 . . ?
C37 C38 H38 128.0 . . ?
C93 C92 C91 121.5(7) . . ?
C93 C92 C97 117.8(9) . . ?
C97 C92 C91 120.6(8) . . ?
C57 C58 C53 118.0(7) . . ?
C57 C58 C60 121.4(8) . . ?
C53 C58 C60 120.6(7) . . ?
N4 C11 C5 123.5(7) . . ?
C12 C11 N4 108.6(7) . . ?
C12 C11 C5 127.8(7) . . ?
C30 C31 C37 116.3(7) . . ?
C32 C31 C30 118.8(7) . . ?
C32 C31 C37 124.8(7) . . ?
C52 C47 C46 120.6(8) . . ?
C52 C47 C48 118.2(9) . . ?
C48 C47 C46 121.1(7) . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N18 C64 C63 105.8(7) . . ?
N18 C64 H64 127.1 . . ?
C63 C64 H64 127.1 . . ?
N12 C46 C47 113.4(7) . . ?
N12 C46 H46A 108.9 . . ?
N12 C46 H46B 108.9 . . ?
C47 C46 H46A 108.9 . . ?
C47 C46 H46B 108.9 . . ?
H46A C46 H46B 107.7 . . ?
C84 C86 H86A 109.5 . . ?
C84 C86 H86B 109.5 . . ?
C84 C86 H86C 109.5 . . ?
H86A C86 H86B 109.5 . . ?
H86A C86 H86C 109.5 . . ?
H86B C86 H86C 109.5 . . ?
N9 C39 H39A 109.4 . . ?
N9 C39 H39B 109.4 . . ?
N9 C39 C40 111.3(6) . . ?
H39A C39 H39B 108.0 . . ?
C40 C39 H39A 109.4 . . ?
C40 C39 H39B 109.4 . . ?
C45 C40 C39 121.3(9) . . ?
C45 C40 C41 117.6(10) . . ?
C41 C40 C39 121.0(9) . . ?
C108 C99 C98 118.1(9) . . ?
C100 C99 C98 124.3(9) . . ?
C100 C99 C108 117.6(9) . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C66 C67 H67 119.4 . . ?
C68 C67 H67 119.4 . . ?
C68 C67 C66 121.1(8) . . ?
C67 C66 C65 121.9(8) . . ?
C67 C66 C71 118.1(8) . . ?
C71 C66 C65 119.9(8) . . ?
N3 C13 C14 113.6(7) . . ?
N3 C13 H13A 108.8 . . ?
N3 C13 H13B 108.8 . . ?
C14 C13 H13A 108.8 . . ?
C14 C13 H13B 108.8 . . ?
H13A C13 H13B 107.7 . . ?
C54 C59 H59A 109.5 . . ?
C54 C59 H59B 109.5 . . ?
C54 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C47 C52 H52 119.9 . . ?
C51 C52 C47 120.1(10) . . ?
C51 C52 H52 119.9 . . ?
C93 C94 H94 119.4 . . ?
C95 C94 H94 119.4 . . ?
C95 C94 C93 121.2(9) . . ?
C28 C33 H33A 109.5 . . ?
C28 C33 H33B 109.5 . . ?
C28 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C92 C93 H93 119.8 . . ?
C94 C93 C92 120.4(8) . . ?
C94 C93 H93 119.8 . . ?
C94 C95 H95 120.1 . . ?
C94 C95 C96 119.8(10) . . ?
C96 C95 H95 120.1 . . ?
C25 C24 H24 120.8 . . ?
C23 C24 H24 120.8 . . ?
C23 C24 C25 118.3(10) . . ?
C78 C73 C72 122.0(10) . . ?
C78 C73 C74 118.2(10) . . ?
C74 C73 C72 119.8(10) . . ?
C14 C19 H19 119.6 . . ?
C18 C19 C14 120.7(9) . . ?
C18 C19 H19 119.6 . . ?
C80 C85 H85A 109.5 . . ?
C80 C85 H85B 109.5 . . ?
C80 C85 H85C 109.5 . . ?
H85A C85 H85B 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
N24 C98 C99 114.3(7) . . ?
N24 C98 H98A 108.7 . . ?
N24 C98 H98B 108.7 . . ?
C99 C98 H98A 108.7 . . ?
C99 C98 H98B 108.7 . . ?
H98A C98 H98B 107.6 . . ?
C15 C16 H16 119.7 . . ?
C15 C16 C17 120.7(11) . . ?
C17 C16 H16 119.7 . . ?
C47 C48 H48 119.7 . . ?
C49 C48 C47 120.6(9) . . ?
C49 C48 H48 119.7 . . ?
C14 C15 H15 119.7 . . ?
C16 C15 C14 120.6(10) . . ?
C16 C15 H15 119.7 . . ?
C49 C50 H50 120.4 . . ?
C51 C50 H50 120.4 . . ?
C51 C50 C49 119.2(10) . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N6 C20 H20A 109.1 . . ?
N6 C20 H20B 109.1 . . ?
N6 C20 C21 112.6(8) . . ?
H20A C20 H20B 107.8 . . ?
C21 C20 H20A 109.1 . . ?
C21 C20 H20B 109.1 . . ?
C48 C49 C50 120.7(10) . . ?
C48 C49 H49 119.6 . . ?
C50 C49 H49 119.6 . . ?
C52 C51 H51 119.4 . . ?
C50 C51 C52 121.1(9) . . ?
C50 C51 H51 119.4 . . ?
C58 C60 H60A 109.5 . . ?
C58 C60 H60B 109.5 . . ?
C58 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C68 C69 H69 120.6 . . ?
C70 C69 H69 120.6 . . ?
C70 C69 C68 118.9(9) . . ?
C67 C68 C69 119.4(9) . . ?
C67 C68 H68 120.3 . . ?
C69 C68 H68 120.3 . . ?
N15 C65 C66 112.6(7) . . ?
N15 C65 H65A 109.1 . . ?
N15 C65 H65B 109.1 . . ?
C66 C65 H65A 109.1 . . ?
C66 C65 H65B 109.1 . . ?
H65A C65 H65B 107.8 . . ?
C66 C71 H71 119.5 . . ?
C70 C71 C66 121.1(9) . . ?
C70 C71 H71 119.5 . . ?
C19 C18 H18 119.5 . . ?
C19 C18 C17 121.0(10) . . ?
C17 C18 H18 119.5 . . ?
C99 C108 H108 120.4 . . ?
C107 C108 C99 119.3(11) . . ?
C107 C108 H108 120.4 . . ?
C69 C70 H70 119.3 . . ?
C71 C70 C69 121.3(9) . . ?
C71 C70 H70 119.3 . . ?
C24 C25 H25 120.2 . . ?
C24 C25 C26 119.6(9) . . ?
C26 C25 H25 120.2 . . ?
C73 C78 H78 120.0 . . ?
C73 C78 C77 119.9(12) . . ?
C77 C78 H78 120.0 . . ?
N18 C72 H72A 109.1 . . ?
N18 C72 H72B 109.1 . . ?
C73 C72 N18 112.7(7) . . ?
C73 C72 H72A 109.1 . . ?
C73 C72 H72B 109.1 . . ?
H72A C72 H72B 107.8 . . ?
N21 C91 C92 112.1(7) . . ?
N21 C91 H91A 109.2 . . ?
N21 C91 H91B 109.2 . . ?
C92 C91 H91A 109.2 . . ?
C92 C91 H91B 109.2 . . ?
H91A C91 H91B 107.9 . . ?
C16 C17 H17 120.8 . . ?
C18 C17 C16 118.5(10) . . ?
C18 C17 H17 120.8 . . ?
C40 C45 H45 120.3 . . ?
C40 C45 C44 119.4(11) . . ?
C44 C45 H45 120.3 . . ?
C22 C21 C20 122.9(8) . . ?
C22 C21 C26 117.8(10) . . ?
C26 C21 C20 119.2(9) . . ?
C99 C100 H100 118.9 . . ?
C105 C100 C99 122.2(10) . . ?
C105 C100 H100 118.9 . . ?
C24 C23 H23 119.0 . . ?
C22 C23 C24 122.1(10) . . ?
C22 C23 H23 119.0 . . ?
C95 C96 H96 120.3 . . ?
C95 C96 C97 119.4(9) . . ?
C97 C96 H96 120.3 . . ?
C40 C41 H41 119.3 . . ?
C42 C41 C40 121.3(13) . . ?
C42 C41 H41 119.3 . . ?
C107 C106 H106 121.2 . . ?
C107 C106 C105 117.7(9) . . ?
C105 C106 H106 121.2 . . ?
C92 C97 H97 119.4 . . ?
C96 C97 C92 121.2(10) . . ?
C96 C97 H97 119.4 . . ?
C21 C22 H22 119.1 . . ?
C23 C22 C21 121.8(9) . . ?
C23 C22 H22 119.1 . . ?
C108 C107 C106 122.9(10) . . ?
C108 C107 H107 118.5 . . ?
C106 C107 H107 118.5 . . ?
Cl1 C101 H101 108.3 . . ?
Cl2 C101 Cl1 111.4(6) . . ?
Cl2 C101 H101 108.3 . . ?
Cl3 C101 Cl1 108.6(6) . . ?
Cl3 C101 Cl2 111.8(6) . . ?
Cl3 C101 H101 108.3 . . ?
C100 C105 C106 120.4(11) . . ?
C100 C105 H105 119.8 . . ?
C106 C105 H105 119.8 . . ?
C25 C26 H26 119.8 . . ?
C21 C26 C25 120.4(10) . . ?
C21 C26 H26 119.8 . . ?
C78 C77 H77 119.3 . . ?
C76 C77 C78 121.4(12) . . ?
C76 C77 H77 119.3 . . ?
C45 C44 H44 119.8 . . ?
C43 C44 C45 120.4(12) . . ?
C43 C44 H44 119.8 . . ?
C73 C74 H74 119.7 . . ?
C75 C74 C73 120.5(12) . . ?
C75 C74 H74 119.7 . . ?
C44 C43 H43 119.1 . . ?
C44 C43 C42 121.9(13) . . ?
C42 C43 H43 119.1 . . ?
C41 C42 H42 120.3 . . ?
C43 C42 C41 119.3(14) . . ?
C43 C42 H42 120.3 . . ?
Cl10 C104 H104 108.1 . . ?
Cl12 C104 Cl10 110.5(6) . . ?
Cl12 C104 Cl11 111.7(7) . . ?
Cl12 C104 H104 108.1 . . ?
Cl11 C104 Cl10 110.2(7) . . ?
Cl11 C104 H104 108.1 . . ?
C74 C75 H75 119.9 . . ?
C74 C75 C76 120.3(14) . . ?
C76 C75 H75 119.9 . . ?
Cl4 C102 Cl6 109.4(7) . . ?
Cl4 C102 H102 107.9 . . ?
Cl6 C102 H102 107.9 . . ?
Cl5 C102 Cl4 111.8(7) . . ?
Cl5 C102 Cl6 111.8(7) . . ?
Cl5 C102 H102 107.9 . . ?
C77 C76 C75 119.6(13) . . ?
C77 C76 H76 120.2 . . ?
C75 C76 H76 120.2 . . ?
Cl9 C103 Cl7 108.6(7) . . ?
Cl9 C103 Cl8 112.6(7) . . ?
Cl9 C103 H103 109.3 . . ?
Cl7 C103 Cl8 107.8(7) . . ?
Cl7 C103 H103 109.3 . . ?
Cl8 C103 H103 109.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N15 N14 N13 C61 0.0(9) . . . . ?
N17 N18 C64 C63 -0.2(10) . . . . ?
N17 N18 C72 C73 -75.4(11) . . . . ?
N17 N16 C63 C57 179.1(7) . . . . ?
N17 N16 C63 C64 -0.2(10) . . . . ?
N10 C37 C38 N12 0.1(10) . . . . ?
N10 C37 C31 C30 -144.9(8) . . . . ?
N10 C37 C31 C32 33.9(13) . . . . ?
N18 N17 N16 C63 0.1(9) . . . . ?
N1 N2 N3 C10 -0.1(10) . . . . ?
N1 N2 N3 C13 -179.2(7) . . . . ?
N1 C9 C3 C4 26.4(11) . . . . ?
N1 C9 C3 C2 -151.8(8) . . . . ?
N1 C9 C10 N3 -0.5(9) . . . . ?
N24 N23 N22 C89 0.3(10) . . . . ?
N24 C90 C89 N22 -0.4(10) . . . . ?
N24 C90 C89 C83 177.7(8) . . . . ?
N9 C39 C40 C45 -101.6(9) . . . . ?
N9 C39 C40 C41 78.1(10) . . . . ?
N14 N15 C62 C61 0.5(10) . . . . ?
N14 N15 C65 C66 -58.6(11) . . . . ?
N14 N13 C61 C55 178.4(7) . . . . ?
N14 N13 C61 C62 0.3(10) . . . . ?
N16 N17 N18 C64 0.1(9) . . . . ?
N16 N17 N18 C72 178.4(8) . . . . ?
N16 C63 C64 N18 0.3(9) . . . . ?
N23 N24 C90 C89 0.6(10) . . . . ?
N23 N24 C98 C99 -59.9(12) . . . . ?
N23 N22 C89 C90 0.0(10) . . . . ?
N23 N22 C89 C83 -178.1(8) . . . . ?
N6 N5 N4 C11 1.2(9) . . . . ?
N6 C12 C11 N4 0.2(10) . . . . ?
N6 C12 C11 C5 -177.1(8) . . . . ?
N6 C20 C21 C22 -45.1(13) . . . . ?
N6 C20 C21 C26 137.2(9) . . . . ?
N2 N1 C9 C3 -177.4(7) . . . . ?
N2 N1 C9 C10 0.5(10) . . . . ?
N2 N3 C10 C9 0.4(10) . . . . ?
N2 N3 C13 C14 74.1(10) . . . . ?
N7 C35 C36 N9 -0.7(9) . . . . ?
N8 N9 C36 C35 0.6(10) . . . . ?
N8 N9 C39 C40 73.9(10) . . . . ?
N8 N7 C35 C29 -179.1(7) . . . . ?
N8 N7 C35 C36 0.6(9) . . . . ?
N13 C61 C62 N15 -0.4(9) . . . . ?
N11 N10 C37 C38 0.2(10) . . . . ?
N11 N10 C37 C31 177.6(8) . . . . ?
N11 N12 C38 C37 -0.3(10) . . . . ?
N11 N12 C46 C47 84.4(9) . . . . ?
N21 C88 C87 N19 0.7(9) . . . . ?
N21 C88 C87 C81 177.0(8) . . . . ?
N5 N6 C12 C11 0.6(9) . . . . ?
N5 N6 C20 C21 -60.1(10) . . . . ?
N5 N4 C11 C5 176.5(8) . . . . ?
N5 N4 C11 C12 -0.9(10) . . . . ?
N20 N19 C87 C81 -176.4(8) . . . . ?
N20 N19 C87 C88 0.1(10) . . . . ?
N20 N21 C88 C87 -1.2(10) . . . . ?
N20 N21 C91 C92 55.7(11) . . . . ?
C29 C30 C31 C37 178.3(7) . . . . ?
C29 C30 C31 C32 -0.6(12) . . . . ?
C29 C35 C36 N9 179.0(9) . . . . ?
C4 C5 C6 C1 2.0(11) . . . . ?
C4 C5 C6 C8 -177.7(7) . . . . ?
C4 C5 C11 N4 -144.6(8) . . . . ?
C4 C5 C11 C12 32.3(13) . . . . ?
C27 C1 C6 C5 175.9(7) . . . . ?
C27 C1 C6 C8 -4.3(11) . . . . ?
C27 C32 C31 C30 0.6(11) . . . . ?
C27 C32 C31 C37 -178.2(7) . . . . ?
C9 N1 N2 N3 -0.3(10) . . . . ?
C30 C29 C35 N7 29.3(11) . . . . ?
C30 C29 C35 C36 -150.4(9) . . . . ?
C30 C29 C28 C27 -1.5(12) . . . . ?
C30 C29 C28 C33 -179.7(8) . . . . ?
C90 N24 N23 N22 -0.6(10) . . . . ?
C90 N24 C98 C99 122.4(9) . . . . ?
C5 C4 C3 C9 -178.7(7) . . . . ?
C5 C4 C3 C2 -0.4(12) . . . . ?
C81 C82 C83 C84 0.0(12) . . . . ?
C81 C82 C83 C89 179.0(7) . . . . ?
C82 C81 C80 C79 -2.0(12) . . . . ?
C82 C81 C80 C85 177.4(8) . . . . ?
C82 C81 C87 N19 146.4(8) . . . . ?
C82 C81 C87 C88 -29.4(13) . . . . ?
C82 C83 C89 N22 142.8(9) . . . . ?
C82 C83 C89 C90 -34.9(13) . . . . ?
C84 C83 C89 N22 -38.2(14) . . . . ?
C84 C83 C89 C90 144.0(9) . . . . ?
C84 C79 C80 C81 0.4(12) . . . . ?
C84 C79 C80 C85 -179.0(8) . . . . ?
C84 C79 C53 C54 -89.3(9) . . . . ?
C84 C79 C53 C58 93.9(10) . . . . ?
C2 C1 C6 C5 -1.1(12) . . . . ?
C2 C1 C6 C8 178.6(7) . . . . ?
C35 N7 N8 N9 -0.3(9) . . . . ?
C35 C29 C30 C31 -176.0(7) . . . . ?
C35 C29 C28 C27 175.4(7) . . . . ?
C35 C29 C28 C33 -2.8(12) . . . . ?
C37 N10 N11 N12 -0.3(9) . . . . ?
C55 C56 C57 C63 178.2(7) . . . . ?
C55 C56 C57 C58 -0.3(12) . . . . ?
C55 C61 C62 N15 -178.3(9) . . . . ?
C55 C54 C53 C79 -177.0(7) . . . . ?
C55 C54 C53 C58 -0.3(12) . . . . ?
C83 C84 C79 C80 1.3(12) . . . . ?
C83 C84 C79 C53 177.8(7) . . . . ?
C3 C4 C5 C6 -1.3(12) . . . . ?
C3 C4 C5 C11 178.2(7) . . . . ?
C3 C9 C10 N3 177.1(9) . . . . ?
C3 C2 C1 C27 -177.6(7) . . . . ?
C3 C2 C1 C6 -0.6(11) . . . . ?
C56 C55 C61 N13 -27.6(11) . . . . ?
C56 C55 C61 C62 150.0(9) . . . . ?
C56 C55 C54 C53 2.5(11) . . . . ?
C56 C55 C54 C59 -178.5(7) . . . . ?
C56 C57 C63 N16 -27.2(11) . . . . ?
C56 C57 C63 C64 151.9(9) . . . . ?
C56 C57 C58 C53 2.5(11) . . . . ?
C56 C57 C58 C60 179.6(8) . . . . ?
C28 C29 C30 C31 1.1(12) . . . . ?
C28 C29 C35 N7 -147.7(8) . . . . ?
C28 C29 C35 C36 32.6(14) . . . . ?
C28 C27 C1 C2 -94.4(10) . . . . ?
C28 C27 C1 C6 88.5(9) . . . . ?
C28 C27 C32 C31 -1.1(11) . . . . ?
C28 C27 C32 C34 179.1(8) . . . . ?
C79 C84 C83 C82 -1.5(12) . . . . ?
C79 C84 C83 C89 179.5(8) . . . . ?
C79 C53 C58 C57 174.6(7) . . . . ?
C79 C53 C58 C60 -2.6(12) . . . . ?
C80 C81 C82 C83 1.9(12) . . . . ?
C80 C81 C87 N19 -33.7(13) . . . . ?
C80 C81 C87 C88 150.5(9) . . . . ?
C80 C79 C53 C54 87.3(10) . . . . ?
C80 C79 C53 C58 -89.5(9) . . . . ?
C57 C63 C64 N18 -178.9(8) . . . . ?
C1 C27 C28 C29 -174.5(7) . . . . ?
C1 C27 C28 C33 3.8(11) . . . . ?
C1 C27 C32 C31 175.1(7) . . . . ?
C1 C27 C32 C34 -4.7(11) . . . . ?
C1 C2 C3 C4 1.4(11) . . . . ?
C1 C2 C3 C9 179.5(7) . . . . ?
C88 N21 N20 N19 1.4(10) . . . . ?
C88 N21 C91 C92 -127.5(9) . . . . ?
C87 N19 N20 N21 -0.9(10) . . . . ?
C87 C81 C82 C83 -178.3(7) . . . . ?
C87 C81 C80 C79 178.1(7) . . . . ?
C87 C81 C80 C85 -2.5(13) . . . . ?
C6 C5 C11 N4 34.9(12) . . . . ?
C6 C5 C11 C12 -148.2(9) . . . . ?
C61 C55 C56 C57 179.3(7) . . . . ?
C61 C55 C54 C53 -179.0(7) . . . . ?
C61 C55 C54 C59 0.0(12) . . . . ?
C36 N9 N8 N7 -0.2(9) . . . . ?
C36 N9 C39 C40 -105.1(10) . . . . ?
C54 C55 C56 C57 -2.2(12) . . . . ?
C54 C55 C61 N13 153.9(8) . . . . ?
C54 C55 C61 C62 -28.5(14) . . . . ?
C54 C53 C58 C57 -2.1(12) . . . . ?
C54 C53 C58 C60 -179.3(8) . . . . ?
C63 C57 C58 C53 -176.0(7) . . . . ?
C63 C57 C58 C60 1.1(12) . . . . ?
C62 N15 N14 N13 -0.3(10) . . . . ?
C62 N15 C65 C66 123.0(10) . . . . ?
C53 C79 C80 C81 -176.0(7) . . . . ?
C53 C79 C80 C85 4.5(12) . . . . ?
C12 N6 N5 N4 -1.2(9) . . . . ?
C12 N6 C20 C21 124.4(10) . . . . ?
C14 C19 C18 C17 -1.4(15) . . . . ?
C32 C27 C28 C29 1.5(12) . . . . ?
C32 C27 C28 C33 179.8(8) . . . . ?
C32 C27 C1 C2 89.3(9) . . . . ?
C32 C27 C1 C6 -87.8(10) . . . . ?
C10 N3 C13 C14 -104.9(10) . . . . ?
C10 C9 C3 C4 -151.0(9) . . . . ?
C10 C9 C3 C2 30.9(14) . . . . ?
C38 N12 N11 N10 0.4(10) . . . . ?
C38 N12 C46 C47 -93.6(10) . . . . ?
C38 C37 C31 C30 32.0(13) . . . . ?
C38 C37 C31 C32 -149.2(9) . . . . ?
C58 C57 C63 N16 151.3(8) . . . . ?
C58 C57 C63 C64 -29.7(14) . . . . ?
C11 C5 C6 C1 -177.4(7) . . . . ?
C11 C5 C6 C8 2.8(12) . . . . ?
C31 C37 C38 N12 -177.2(8) . . . . ?
C47 C52 C51 C50 -0.8(15) . . . . ?
C47 C48 C49 C50 -0.7(16) . . . . ?
C34 C32 C31 C30 -179.6(7) . . . . ?
C34 C32 C31 C37 1.6(13) . . . . ?
C64 N18 C72 C73 102.7(11) . . . . ?
C46 N12 N11 N10 -177.9(7) . . . . ?
C46 N12 C38 C37 177.8(8) . . . . ?
C46 C47 C52 C51 -179.3(9) . . . . ?
C46 C47 C48 C49 -180.0(9) . . . . ?
C86 C84 C83 C82 177.3(8) . . . . ?
C86 C84 C83 C89 -1.7(13) . . . . ?
C86 C84 C79 C80 -177.5(8) . . . . ?
C86 C84 C79 C53 -1.0(11) . . . . ?
C39 N9 N8 N7 -179.4(7) . . . . ?
C39 N9 C36 C35 179.7(8) . . . . ?
C39 C40 C45 C44 -178.2(8) . . . . ?
C39 C40 C41 C42 178.3(11) . . . . ?
C40 C45 C44 C43 -1.2(16) . . . . ?
C40 C41 C42 C43 1(2) . . . . ?
C99 C108 C107 C106 0.7(16) . . . . ?
C99 C100 C105 C106 -0.8(17) . . . . ?
C7 C2 C3 C4 -178.5(7) . . . . ?
C7 C2 C3 C9 -0.3(12) . . . . ?
C7 C2 C1 C27 2.2(11) . . . . ?
C7 C2 C1 C6 179.2(7) . . . . ?
C67 C66 C65 N15 -42.7(11) . . . . ?
C67 C66 C71 C70 -2.4(13) . . . . ?
C66 C67 C68 C69 0.3(13) . . . . ?
C66 C71 C70 C69 3.2(15) . . . . ?
C13 N3 C10 C9 179.5(8) . . . . ?
C13 C14 C19 C18 -179.5(8) . . . . ?
C13 C14 C15 C16 -177.4(9) . . . . ?
C59 C54 C53 C79 3.9(11) . . . . ?
C59 C54 C53 C58 -179.4(8) . . . . ?
C52 C47 C46 N12 -120.0(9) . . . . ?
C52 C47 C48 C49 1.2(14) . . . . ?
C94 C95 C96 C97 -0.5(18) . . . . ?
C93 C92 C91 N21 46.6(12) . . . . ?
C93 C92 C97 C96 1.0(16) . . . . ?
C93 C94 C95 C96 1.2(17) . . . . ?
C95 C94 C93 C92 -0.8(16) . . . . ?
C95 C96 C97 C92 -0.6(18) . . . . ?
C24 C25 C26 C21 -1.0(18) . . . . ?
C24 C23 C22 C21 1.6(18) . . . . ?
C73 C78 C77 C76 0.3(17) . . . . ?
C73 C74 C75 C76 2(2) . . . . ?
C19 C14 C13 N3 57.4(10) . . . . ?
C19 C14 C15 C16 2.8(13) . . . . ?
C19 C18 C17 C16 -0.6(15) . . . . ?
C98 N24 N23 N22 -178.7(8) . . . . ?
C98 N24 C90 C89 178.5(9) . . . . ?
C98 C99 C108 C107 179.2(9) . . . . ?
C98 C99 C100 C105 -179.0(9) . . . . ?
C48 C47 C46 N12 61.2(10) . . . . ?
C48 C47 C52 C51 -0.5(14) . . . . ?
C15 C14 C13 N3 -122.4(8) . . . . ?
C15 C14 C19 C18 0.3(13) . . . . ?
C15 C16 C17 C18 3.7(15) . . . . ?
C20 N6 N5 N4 -177.5(8) . . . . ?
C20 N6 C12 C11 176.4(9) . . . . ?
C20 C21 C22 C23 -177.7(10) . . . . ?
C20 C21 C26 C25 177.5(10) . . . . ?
C49 C50 C51 C52 1.4(15) . . . . ?
C51 C50 C49 C48 -0.6(15) . . . . ?
C68 C67 C66 C65 -178.4(8) . . . . ?
C68 C67 C66 C71 0.6(13) . . . . ?
C68 C69 C70 C71 -2.2(15) . . . . ?
C65 N15 N14 N13 -179.0(7) . . . . ?
C65 N15 C62 C61 179.0(8) . . . . ?
C65 C66 C71 C70 176.7(9) . . . . ?
C71 C66 C65 N15 138.3(8) . . . . ?
C108 C99 C98 N24 156.1(8) . . . . ?
C108 C99 C100 C105 -0.6(15) . . . . ?
C70 C69 C68 C67 0.5(14) . . . . ?
C25 C24 C23 C22 -2.9(17) . . . . ?
C78 C73 C72 N18 101.7(10) . . . . ?
C78 C73 C74 C75 0.0(17) . . . . ?
C78 C77 C76 C75 1.5(19) . . . . ?
C72 N18 C64 C63 -178.4(8) . . . . ?
C72 C73 C78 C77 178.6(9) . . . . ?
C72 C73 C74 C75 -179.7(11) . . . . ?
C91 N21 N20 N19 178.6(8) . . . . ?
C91 N21 C88 C87 -178.3(8) . . . . ?
C91 C92 C93 C94 176.9(9) . . . . ?
C91 C92 C97 C96 -176.2(10) . . . . ?
C17 C16 C15 C14 -4.9(15) . . . . ?
C45 C40 C41 C42 -2.1(16) . . . . ?
C45 C44 C43 C42 0(2) . . . . ?
C100 C99 C98 N24 -25.5(13) . . . . ?
C100 C99 C108 C107 0.7(14) . . . . ?
C23 C24 C25 C26 2.5(17) . . . . ?
C41 C40 C45 C44 2.2(13) . . . . ?
C97 C92 C93 C94 -0.3(14) . . . . ?
C97 C92 C91 N21 -136.3(9) . . . . ?
C22 C21 C26 C25 -0.3(16) . . . . ?
C107 C106 C105 C100 2.1(17) . . . . ?
C105 C106 C107 C108 -2.1(17) . . . . ?
C26 C21 C22 C23 0.0(16) . . . . ?
C44 C43 C42 C41 0(2) . . . . ?
C74 C73 C78 C77 -1.1(14) . . . . ?
C74 C73 C72 N18 -78.6(11) . . . . ?
C74 C75 C76 C77 -3(2) . . . . ?


_ins_header                      
;
TITL jns2202 in P2(1) 
REM P2(1) (#4 in standard setting)
CELL 1.54184  10.644399  49.444959  11.034046  90.0000 115.6949  90.0000
ZERR    4.00   0.000333   0.001294   0.000395   0.0000   0.0042   0.0000
LATT -1
SYMM -x, y+1/2,-z 
SFAC C H N
UNIT 240.00 320.00 48.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
SIZE 0.04 0.11 0.14
TREF
HKLF 4
END
;
_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 1.367
_oxdiff_exptl_absorpt_empirical_full_min 0.808
