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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1-rac_100K_publ
_database_code_depnum_ccdc_archive 'CCDC 2073633'
loop_
_audit_author_name
_audit_author_address
'Marc Little'
;University of Liverpool
United Kingdom
;
_audit_update_record             
;
2021-03-27 deposited with the CCDC.	2021-05-14 downloaded from the CCDC.
;
_audit_creation_date             2019-11-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H48 N6'
_chemical_formula_sum            'C42 H48 N6'
_chemical_formula_weight         636.86
_chemical_melting_point          ?
_chemical_oxdiff_formula         C48H120N6
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 '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        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   24.7909(8)
_cell_length_b                   14.7339(4)
_cell_length_c                   22.7185(8)
_cell_angle_alpha                90
_cell_angle_beta                 101.230(3)
_cell_angle_gamma                90
_cell_volume                     8139.4(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    14662
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.9640
_cell_measurement_theta_min      2.1980
_shelx_estimated_absorpt_T_max   0.993
_shelx_estimated_absorpt_T_min   0.982
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84356
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     ?
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.039
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2736
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.297
_exptl_crystal_size_mid          0.206
_exptl_crystal_size_min          0.112
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            52053
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.616
_diffrn_ambient_temperature      100
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 1.000
_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   -100.00  25.00   1.00   20.00    --  -10.00 -68.00   0.00  125
  2  ω   -100.00  25.00   1.00   20.00    --  -10.00 -68.00 120.00  125
  3  ω   -100.00  25.00   1.00   20.00    --  -10.00 -68.00 240.00  125
  4  ω   -100.00  25.00   1.00   20.00    --  -10.00 -30.00  90.00  125
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0285835000
_diffrn_orient_matrix_UB_12      0.0002857000
_diffrn_orient_matrix_UB_13      -0.0122316000
_diffrn_orient_matrix_UB_21      0.0057383000
_diffrn_orient_matrix_UB_22      -0.0036810000
_diffrn_orient_matrix_UB_23      -0.0293120000
_diffrn_orient_matrix_UB_31      -0.0006018000
_diffrn_orient_matrix_UB_32      -0.0480209000
_diffrn_orient_matrix_UB_33      0.0020653000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5734
_reflns_number_total             8312
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.213
_refine_diff_density_min         -0.196
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         8312
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1002
_refine_ls_R_factor_gt           0.0628
_refine_ls_restrained_S_all      1.042
_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)+(0.0617P)²+6.8642P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1503
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C4(H4), C5(H5), C15(H15), C16(H16), C29(H29), C34(H34)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B), C17(H17A,H17B), C18(H18A,
 H18B), C19(H19A,H19B), C20(H20A,H20B), C30(H30A,H30B), C31(H31A,H31B),
 C32(H32A,H32B), C33(H33A,H33B)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C11(H11), C12(H12), C13(H13), C14(H14), C21(H21), C23(H23),
 C24(H24), C25(H25), C27(H27), C28(H28), C35(H35), C37(H37), C39(H39), C40(H40),
  C41(H41), C42(H42)
;
_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 0.02950(7) 0.28760(11) 0.19285(8) 0.0336(4) Uani 1 1 d . . . . .
N2 N 0.07368(7) 0.10925(12) 0.17124(8) 0.0349(4) Uani 1 1 d . . . . .
N3 N 0.29590(7) -0.07887(11) 0.31326(8) 0.0347(4) Uani 1 1 d . . . . .
N4 N 0.37616(7) 0.02973(11) 0.39109(8) 0.0361(4) Uani 1 1 d . . . . .
N5 N 0.31144(7) 0.43514(11) 0.44791(8) 0.0343(4) Uani 1 1 d . . . . .
N6 N 0.21006(7) 0.50974(11) 0.37427(7) 0.0326(4) Uani 1 1 d . . . . .
C1 C 0.35834(8) 0.66169(14) 0.39587(10) 0.0371(5) Uani 1 1 d . . . . .
H1A H 0.390630 0.699281 0.413229 0.045 Uiso 1 1 calc R . . . .
H1B H 0.360315 0.647975 0.353680 0.045 Uiso 1 1 calc R . . . .
C2 C 0.30582(8) 0.71393(14) 0.39782(10) 0.0386(5) Uani 1 1 d . . . . .
H2A H 0.305053 0.770564 0.374222 0.046 Uiso 1 1 calc R . . . .
H2B H 0.304750 0.730541 0.439804 0.046 Uiso 1 1 calc R . . . .
C3 C 0.25589(8) 0.65572(14) 0.37202(10) 0.0359(5) Uani 1 1 d . . . . .
H3A H 0.255746 0.643275 0.329167 0.043 Uiso 1 1 calc R . . . .
H3B H 0.221940 0.689728 0.374411 0.043 Uiso 1 1 calc R . . . .
C4 C 0.25589(8) 0.56553(13) 0.40563(9) 0.0315(5) Uani 1 1 d . . . . .
H4 H 0.250764 0.577633 0.447508 0.038 Uiso 1 1 calc R . . . .
C5 C 0.30978(8) 0.51355(13) 0.40769(9) 0.0319(5) Uani 1 1 d . . . . .
H5 H 0.311678 0.491857 0.366436 0.038 Uiso 1 1 calc R . . . .
C6 C 0.35955(8) 0.57327(14) 0.43126(10) 0.0361(5) Uani 1 1 d . . . . .
H6A H 0.393539 0.539443 0.428776 0.043 Uiso 1 1 calc R . . . .
H6B H 0.360411 0.587597 0.474010 0.043 Uiso 1 1 calc R . . . .
C7 C 0.17053(8) 0.49491(13) 0.40052(9) 0.0309(5) Uani 1 1 d . . . . .
H7 H 0.172404 0.517556 0.440024 0.037 Uiso 1 1 calc R . . . .
C8 C 0.12139(8) 0.44331(13) 0.37154(9) 0.0290(4) Uani 1 1 d . . . . .
C9 C 0.12002(8) 0.40152(13) 0.31611(9) 0.0300(5) Uani 1 1 d . . . . .
H9 H 0.151910 0.403002 0.298740 0.036 Uiso 1 1 calc R . . . .
C10 C 0.07297(8) 0.35771(13) 0.28569(9) 0.0295(4) Uani 1 1 d . . . . .
C11 C 0.02639(8) 0.35445(14) 0.31251(10) 0.0356(5) Uani 1 1 d . . . . .
H11 H -0.006150 0.325186 0.292352 0.043 Uiso 1 1 calc R . . . .
C12 C 0.02781(9) 0.39351(15) 0.36784(10) 0.0409(5) Uani 1 1 d . . . . .
H12 H -0.003576 0.390196 0.385974 0.049 Uiso 1 1 calc R . . . .
C13 C 0.07517(9) 0.43803(15) 0.39748(10) 0.0375(5) Uani 1 1 d . . . . .
H13 H 0.075744 0.464848 0.435627 0.045 Uiso 1 1 calc R . . . .
C14 C 0.07236(8) 0.32019(13) 0.22586(9) 0.0311(5) Uani 1 1 d . . . . .
H14 H 0.105643 0.320235 0.211042 0.037 Uiso 1 1 calc R . . . .
C15 C 0.03417(8) 0.25548(14) 0.13324(9) 0.0343(5) Uani 1 1 d . . . . .
H15 H 0.071408 0.271509 0.125642 0.041 Uiso 1 1 calc R . . . .
C16 C 0.02730(8) 0.15178(14) 0.13044(9) 0.0328(5) Uani 1 1 d . . . . .
H16 H -0.007913 0.134710 0.142819 0.039 Uiso 1 1 calc R . . . .
C17 C 0.02657(9) 0.11786(15) 0.06674(10) 0.0395(5) Uani 1 1 d . . . . .
H17A H 0.062979 0.128844 0.056316 0.047 Uiso 1 1 calc R . . . .
H17B H 0.019787 0.051604 0.065047 0.047 Uiso 1 1 calc R . . . .
C18 C -0.01764(9) 0.16514(16) 0.02095(10) 0.0439(6) Uani 1 1 d . . . . .
H18A H -0.016286 0.142617 -0.019797 0.053 Uiso 1 1 calc R . . . .
H18B H -0.054354 0.150613 0.029466 0.053 Uiso 1 1 calc R . . . .
C19 C -0.00914(10) 0.26754(17) 0.02321(10) 0.0468(6) Uani 1 1 d . . . . .
H19A H -0.038849 0.297394 -0.005751 0.056 Uiso 1 1 calc R . . . .
H19B H 0.026406 0.282598 0.011901 0.056 Uiso 1 1 calc R . . . .
C20 C -0.00947(9) 0.30212(15) 0.08639(10) 0.0414(5) Uani 1 1 d . . . . .
H20A H -0.046164 0.291269 0.096099 0.050 Uiso 1 1 calc R . . . .
H20B H -0.002755 0.368392 0.087842 0.050 Uiso 1 1 calc R . . . .
C21 C 0.06276(8) 0.05959(15) 0.21303(9) 0.0345(5) Uani 1 1 d . . . . .
H21 H 0.025561 0.054542 0.217487 0.041 Uiso 1 1 calc R . . . .
C22 C 0.10537(8) 0.00921(15) 0.25511(9) 0.0350(5) Uani 1 1 d . . . . .
C23 C 0.08961(9) -0.05283(18) 0.29474(11) 0.0476(6) Uani 1 1 d . . . . .
H23 H 0.051833 -0.059675 0.296399 0.057 Uiso 1 1 calc R . . . .
C24 C 0.12905(10) -0.10490(19) 0.33198(12) 0.0557(7) Uani 1 1 d . . . . .
H24 H 0.118098 -0.146738 0.359229 0.067 Uiso 1 1 calc R . . . .
C25 C 0.18416(9) -0.09603(17) 0.32948(11) 0.0477(6) Uani 1 1 d . . . . .
H25 H 0.210759 -0.132502 0.354592 0.057 Uiso 1 1 calc R . . . .
C26 C 0.20088(8) -0.03377(14) 0.29027(9) 0.0334(5) Uani 1 1 d . . . . .
C27 C 0.16122(8) 0.01884(14) 0.25394(9) 0.0321(5) Uani 1 1 d . . . . .
H27 H 0.172324 0.062249 0.227757 0.038 Uiso 1 1 calc R . . . .
C28 C 0.25930(8) -0.02598(14) 0.28563(9) 0.0322(5) Uani 1 1 d . . . . .
H28 H 0.269783 0.020365 0.261035 0.039 Uiso 1 1 calc R . . . .
C29 C 0.35225(8) -0.06791(14) 0.30420(10) 0.0329(5) Uani 1 1 d . . . . .
H29 H 0.354272 -0.012436 0.279358 0.039 Uiso 1 1 calc R . . . .
C30 C 0.36870(8) -0.15094(14) 0.27075(10) 0.0362(5) Uani 1 1 d . . . . .
H30A H 0.363091 -0.206794 0.293025 0.043 Uiso 1 1 calc R . . . .
H30B H 0.344808 -0.154588 0.230467 0.043 Uiso 1 1 calc R . . . .
C31 C 0.42855(9) -0.14530(15) 0.26421(10) 0.0399(5) Uani 1 1 d . . . . .
H31A H 0.438390 -0.200675 0.243984 0.048 Uiso 1 1 calc R . . . .
H31B H 0.433516 -0.092395 0.238930 0.048 Uiso 1 1 calc R . . . .
C32 C 0.46640(8) -0.13599(14) 0.32519(11) 0.0399(5) Uani 1 1 d . . . . .
H32A H 0.504926 -0.130242 0.319785 0.048 Uiso 1 1 calc R . . . .
H32B H 0.463684 -0.191169 0.349307 0.048 Uiso 1 1 calc R . . . .
C33 C 0.45094(8) -0.05265(14) 0.35861(11) 0.0402(5) Uani 1 1 d . . . . .
H33A H 0.457436 0.002930 0.336510 0.048 Uiso 1 1 calc R . . . .
H33B H 0.474770 -0.049846 0.398961 0.048 Uiso 1 1 calc R . . . .
C34 C 0.39047(8) -0.05571(13) 0.36504(10) 0.0333(5) Uani 1 1 d . . . . .
H34 H 0.385018 -0.107129 0.392010 0.040 Uiso 1 1 calc R . . . .
C35 C 0.36081(9) 0.02820(14) 0.44082(11) 0.0389(5) Uani 1 1 d . . . . .
H35 H 0.359471 -0.028254 0.460691 0.047 Uiso 1 1 calc R . . . .
C36 C 0.34482(9) 0.11199(14) 0.46914(10) 0.0387(5) Uani 1 1 d . . . . .
C37 C 0.33682(8) 0.19288(13) 0.43664(10) 0.0337(5) Uani 1 1 d . . . . .
H37 H 0.340313 0.192961 0.395739 0.040 Uiso 1 1 calc R . . . .
C38 C 0.32386(8) 0.27331(13) 0.46267(10) 0.0335(5) Uani 1 1 d . . . . .
C39 C 0.31761(10) 0.27235(15) 0.52251(10) 0.0428(6) Uani 1 1 d . . . . .
H39 H 0.308484 0.326687 0.540846 0.051 Uiso 1 1 calc R . . . .
C40 C 0.32469(12) 0.19256(16) 0.55503(12) 0.0543(7) Uani 1 1 d . . . . .
H40 H 0.320258 0.192190 0.595634 0.065 Uiso 1 1 calc R . . . .
C41 C 0.33832(11) 0.11245(16) 0.52849(12) 0.0511(6) Uani 1 1 d . . . . .
H41 H 0.343177 0.057895 0.551197 0.061 Uiso 1 1 calc R . . . .
C42 C 0.31826(8) 0.35722(13) 0.42652(10) 0.0325(5) Uani 1 1 d . . . . .
H42 H 0.319836 0.352767 0.385171 0.039 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C14 1.269(2) . ?
N1 C15 1.460(3) . ?
N2 C16 1.469(3) . ?
N2 C21 1.269(3) . ?
N3 C28 1.266(3) . ?
N3 C29 1.460(2) . ?
N4 C34 1.464(2) . ?
N4 C35 1.261(3) . ?
N5 C5 1.469(3) . ?
N5 C42 1.271(2) . ?
N6 C4 1.469(2) . ?
N6 C7 1.262(2) . ?
C1 C2 1.521(3) . ?
C1 C6 1.528(3) . ?
C2 C3 1.526(3) . ?
C3 C4 1.533(3) . ?
C4 C5 1.533(3) . ?
C5 C6 1.525(3) . ?
C7 C8 1.478(3) . ?
C8 C9 1.396(3) . ?
C8 C13 1.389(3) . ?
C9 C10 1.393(3) . ?
C10 C11 1.408(3) . ?
C10 C14 1.465(3) . ?
C11 C12 1.377(3) . ?
C12 C13 1.398(3) . ?
C15 C16 1.537(3) . ?
C15 C20 1.525(3) . ?
C16 C17 1.528(3) . ?
C17 C18 1.525(3) . ?
C18 C19 1.523(3) . ?
C19 C20 1.525(3) . ?
C21 C22 1.479(3) . ?
C22 C23 1.391(3) . ?
C22 C27 1.397(3) . ?
C23 C24 1.392(3) . ?
C24 C25 1.385(3) . ?
C25 C26 1.397(3) . ?
C26 C27 1.390(3) . ?
C26 C28 1.477(3) . ?
C29 C30 1.537(3) . ?
C29 C34 1.526(3) . ?
C30 C31 1.522(3) . ?
C31 C32 1.521(3) . ?
C32 C33 1.531(3) . ?
C33 C34 1.535(3) . ?
C35 C36 1.481(3) . ?
C36 C37 1.396(3) . ?
C36 C41 1.389(3) . ?
C37 C38 1.390(3) . ?
C38 C39 1.398(3) . ?
C38 C42 1.476(3) . ?
C39 C40 1.381(3) . ?
C40 C41 1.397(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C14 N1 C15 117.53(17) . . ?
C21 N2 C16 117.59(17) . . ?
C28 N3 C29 118.36(17) . . ?
C35 N4 C34 119.09(17) . . ?
C42 N5 C5 117.54(17) . . ?
C7 N6 C4 117.78(17) . . ?
C2 C1 C6 110.20(17) . . ?
C1 C2 C3 109.84(17) . . ?
C2 C3 C4 112.00(17) . . ?
N6 C4 C3 108.57(16) . . ?
N6 C4 C5 108.81(16) . . ?
C3 C4 C5 111.34(16) . . ?
N5 C5 C4 109.31(16) . . ?
N5 C5 C6 108.22(16) . . ?
C6 C5 C4 111.30(16) . . ?
C5 C6 C1 112.05(17) . . ?
N6 C7 C8 121.83(18) . . ?
C9 C8 C7 120.12(17) . . ?
C13 C8 C7 121.10(18) . . ?
C13 C8 C9 118.75(18) . . ?
C10 C9 C8 121.51(18) . . ?
C9 C10 C11 118.64(18) . . ?
C9 C10 C14 119.45(17) . . ?
C11 C10 C14 121.85(18) . . ?
C12 C11 C10 120.25(19) . . ?
C11 C12 C13 120.38(19) . . ?
C8 C13 C12 120.44(19) . . ?
N1 C14 C10 123.18(18) . . ?
N1 C15 C16 109.41(17) . . ?
N1 C15 C20 109.13(17) . . ?
C20 C15 C16 111.17(17) . . ?
N2 C16 C15 109.33(16) . . ?
N2 C16 C17 108.75(16) . . ?
C17 C16 C15 110.19(17) . . ?
C18 C17 C16 111.78(17) . . ?
C19 C18 C17 110.68(18) . . ?
C18 C19 C20 109.69(19) . . ?
C19 C20 C15 111.92(18) . . ?
N2 C21 C22 122.92(18) . . ?
C23 C22 C21 119.53(18) . . ?
C23 C22 C27 118.90(19) . . ?
C27 C22 C21 121.49(19) . . ?
C22 C23 C24 120.2(2) . . ?
C25 C24 C23 120.3(2) . . ?
C24 C25 C26 120.4(2) . . ?
C25 C26 C28 120.90(19) . . ?
C27 C26 C25 118.79(19) . . ?
C27 C26 C28 120.28(18) . . ?
C26 C27 C22 121.39(19) . . ?
N3 C28 C26 122.33(19) . . ?
N3 C29 C30 109.57(16) . . ?
N3 C29 C34 109.11(16) . . ?
C34 C29 C30 111.34(16) . . ?
C31 C30 C29 111.25(17) . . ?
C32 C31 C30 110.88(18) . . ?
C31 C32 C33 110.76(18) . . ?
C32 C33 C34 111.54(17) . . ?
N4 C34 C29 108.11(16) . . ?
N4 C34 C33 109.35(16) . . ?
C29 C34 C33 111.27(17) . . ?
N4 C35 C36 121.82(19) . . ?
C37 C36 C35 120.3(2) . . ?
C41 C36 C35 121.1(2) . . ?
C41 C36 C37 118.6(2) . . ?
C38 C37 C36 121.6(2) . . ?
C37 C38 C39 118.93(19) . . ?
C37 C38 C42 118.83(19) . . ?
C39 C38 C42 122.24(18) . . ?
C40 C39 C38 120.1(2) . . ?
C39 C40 C41 120.3(2) . . ?
C36 C41 C40 120.5(2) . . ?
N5 C42 C38 123.31(19) . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.215
_oxdiff_exptl_absorpt_empirical_full_min 0.785
####################################################################### 
# 
# 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_2oX_1-rac_100K_publ
_database_code_depnum_ccdc_archive 'CCDC 2073636'
loop_
_audit_author_name
_audit_author_address
'Marc Little'
;University of Liverpool
United Kingdom
;
_audit_update_record             
;
2021-03-27 deposited with the CCDC.	2021-05-14 downloaded from the CCDC.
;
_audit_creation_date             2019-10-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H48 N6, 2(C8 H10)'
_chemical_formula_sum            'C58 H68 N6'
_chemical_formula_weight         849.18
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0028 0.0015 '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 0.0056 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.19190(7)
_cell_length_b                   15.18470(8)
_cell_length_c                   15.73550(8)
_cell_angle_alpha                104.5050(4)
_cell_angle_beta                 91.5770(5)
_cell_angle_gamma                105.6390(5)
_cell_volume                     2480.11(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    31076
_cell_measurement_temperature    100
_cell_measurement_theta_max      35.7188703978
_cell_measurement_theta_min      1.40837131993
_shelx_estimated_absorpt_T_max   0.999
_shelx_estimated_absorpt_T_min   0.994
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
CCP4 7.0.040: AIMLESS, version 0.5.32 : 29/03/17
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.023
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1264
_diffrn_reflns_av_unetI/netI     0.0826
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32622
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         25.847
_diffrn_reflns_theta_min         1.302
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_area_resol_mean PILATUS_2M_S_N_24_0107_Diamond
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'Fixed χ 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_collimation    '0.3 x 1.5 Double Pinhole'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_source                   Synchrotron
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9404
_reflns_number_total             10349
_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       
'DIALS 2theta refinement, DIALS 1.6.4-g47a579eb-release'
_computing_data_collection       'Diamond I19 GDA, (Diamond, RAL, Didcot, UK)'
_computing_data_reduction        
;
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
DIALS 1.6.4-g47a579eb-release
pointless (Evans, P., 2006)
XIA2 0.5.340-g5578c4a7-dials-1.6 (Winter, G., 2010)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         10349
_refine_ls_number_restraints     112
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0674
_refine_ls_restrained_S_all      1.079
_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)+(0.1218P)²+0.5184P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1899
_refine_ls_wR_factor_ref         0.1955
_refine_special_details          ?
_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
 C57-C53 = C58-C54
 1.49 with sigma of 0.01
 C62-C65 = C66-C61
 1.49 with sigma of 0.01
3. Rigid body (RIGU) restrains
 C63, C62, C60, C59, C64, C61, C66, C65
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C50, C43, C44, C48, C49, C45, C47, C46
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(C62)=Sof(C61)=Sof(C60)=Sof(H1ca)=Sof(C59)=Sof(H2ca)=Sof(C64)=Sof(H3ca)=
 Sof(C63)=Sof(H4ca)=Sof(C66)=Sof(H5ca)=Sof(H6ca)=Sof(H7ca)=Sof(C65)=Sof(H8ca)=
 Sof(H9ca)=Sof(H0da)=1-FVAR(1)
 Sof(C53)=Sof(C54)=Sof(C55)=Sof(H1da)=Sof(C56)=Sof(H2da)=Sof(C51)=Sof(H3da)=
 Sof(C52)=Sof(H4da)=Sof(C57)=Sof(H5da)=Sof(H6da)=Sof(H7da)=Sof(C58)=Sof(H8da)=
 Sof(H9da)=Sof(H0ea)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C5(Hb), C15(Hd), C4(Hg), C34(Hi), C29(Hn), C20(Hu)
5.b Secondary CH2 refined with riding coordinates:
 C16(Hj,Hk), C17(Hs,Ht), C19(Hv,Hw), C30(Hx,Hy), C2(Hz,H0aa), C32(H1aa,H2aa),
 C3(H5aa,H6aa), C18(H0ba,H1ba), C6(H2ba,H3ba), C33(H4ba,H5ba), C1(H7ba,H8ba),
 C31(H9ba,H0ca)
5.c Aromatic/amide H refined with riding coordinates:
 C42(H), C21(Ha), C37(Hc), C14(He), C9(Hf), C39(Hh), C27(Hl), C35(Hm), C28(Ho),
  C11(Hp), C38(Hq), C41(Hr), C7(H3aa), C13(H4aa), C23(H7aa), C25(H8aa),
 C10(H9aa), C24(H6ba), C48(H48), C45(H45), C46(H46), C47(H47), C60(H1ca),
 C59(H2ca), C64(H3ca), C63(H4ca), C55(H1da), C56(H2da), C51(H3da), C52(H4da)
5.d Fitted hexagon refined as free rotating group:
 C62(C61,C60,C59,C64,C63), C53(C54,C55,C56,C51,C52)
5.e Idealised Me refined as rotating group:
 C49(H49a,H49b,H49c), C50(H50a,H50b,H50c), C66(H5ca,H6ca,H7ca), C65(H8ca,H9ca,
 H0da), C57(H5da,H6da,H7da), C58(H8da,H9da,H0ea)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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 0.05885(10) 0.85494(8) 0.53041(7) 0.0239(2) Uani 1 1 d . . . . .
N5 N 0.30089(11) 0.87585(8) 0.62785(8) 0.0264(3) Uani 1 1 d . . . . .
N4 N 0.71681(10) 0.67208(8) 0.50206(7) 0.0256(2) Uani 1 1 d . . . . .
N2 N 0.08800(11) 0.42497(8) 0.10396(8) 0.0271(3) Uani 1 1 d . . . . .
N3 N 0.60400(10) 0.51080(8) 0.34962(8) 0.0280(3) Uani 1 1 d . . . . .
N1 N -0.09019(10) 0.52451(8) 0.17303(7) 0.0253(2) Uani 1 1 d . . . . .
C12 C -0.04561(12) 0.69360(9) 0.21908(8) 0.0242(3) Uani 1 1 d . . . . .
C42 C 0.39566(13) 0.94057(9) 0.62145(8) 0.0259(3) Uani 1 1 d . . . . .
H H 0.393968 1.004802 0.637781 0.031 Uiso 1 1 calc R . . . .
C21 C 0.17145(13) 0.44324(9) 0.16671(9) 0.0268(3) Uani 1 1 d . . . . .
HA H 0.148590 0.424472 0.218609 0.032 Uiso 1 1 calc R . . . .
C22 C 0.30346(12) 0.49281(9) 0.16222(9) 0.0264(3) Uani 1 1 d . . . . .
C36 C 0.62613(13) 0.80255(9) 0.54612(9) 0.0275(3) Uani 1 1 d . . . . .
C5 C 0.07325(12) 0.83739(9) 0.61701(8) 0.0234(3) Uani 1 1 d . . . . .
HB H 0.075272 0.770262 0.608070 0.028 Uiso 1 1 calc R . . . .
C37 C 0.72270(12) 0.87206(10) 0.52527(9) 0.0277(3) Uani 1 1 d . . . . .
HC H 0.794818 0.856650 0.503288 0.033 Uiso 1 1 calc R . . . .
C15 C -0.12483(12) 0.43633(9) 0.10252(8) 0.0236(3) Uani 1 1 d . . . . .
HD H -0.115230 0.451057 0.044166 0.028 Uiso 1 1 calc R . . . .
C14 C -0.07526(12) 0.60157(9) 0.15139(8) 0.0247(3) Uani 1 1 d . . . . .
HE H -0.083276 0.600059 0.090744 0.030 Uiso 1 1 calc R . . . .
C9 C 0.00434(12) 0.86684(9) 0.34903(9) 0.0255(3) Uani 1 1 d . . . . .
HF H 0.019340 0.925414 0.392979 0.031 Uiso 1 1 calc R . . . .
C4 C 0.19603(12) 0.90369(9) 0.66896(8) 0.0246(3) Uani 1 1 d . . . . .
HG H 0.202509 0.970981 0.670161 0.030 Uiso 1 1 calc R . . . .
C39 C 0.60742(13) 0.98646(9) 0.56980(9) 0.0277(3) Uani 1 1 d . . . . .
HH H 0.602519 1.049643 0.579383 0.033 Uiso 1 1 calc R . . . .
C26 C 0.52122(13) 0.54084(9) 0.21960(9) 0.0266(3) Uani 1 1 d . . . . .
C34 C 0.70740(12) 0.57354(9) 0.50018(9) 0.0254(3) Uani 1 1 d . . . . .
HI H 0.625848 0.544352 0.520446 0.030 Uiso 1 1 calc R . . . .
C16 C -0.26153(12) 0.38376(10) 0.10663(9) 0.0267(3) Uani 1 1 d . . . . .
HJ H -0.272143 0.374399 0.166311 0.032 Uiso 1 1 calc R . . . .
HK H -0.315244 0.423013 0.096231 0.032 Uiso 1 1 calc R . . . .
C40 C 0.50931(12) 0.91758(9) 0.58883(9) 0.0256(3) Uani 1 1 d . . . . .
C27 C 0.39545(12) 0.49723(9) 0.22561(9) 0.0263(3) Uani 1 1 d . . . . .
HL H 0.372899 0.470475 0.273405 0.032 Uiso 1 1 calc R . . . .
C35 C 0.63077(13) 0.70415(10) 0.53576(10) 0.0285(3) Uani 1 1 d . . . . .
HM H 0.564996 0.662390 0.555652 0.034 Uiso 1 1 calc R . . . .
C29 C 0.71472(12) 0.51785(9) 0.40570(9) 0.0259(3) Uani 1 1 d . . . . .
HN H 0.791261 0.551440 0.382626 0.031 Uiso 1 1 calc R . . . .
C28 C 0.62242(12) 0.54543(9) 0.28406(9) 0.0270(3) Uani 1 1 d . . . . .
HO H 0.705726 0.575923 0.276059 0.032 Uiso 1 1 calc R . . . .
C11 C -0.04332(13) 0.77658(10) 0.19603(9) 0.0277(3) Uani 1 1 d . . . . .
HP H -0.058951 0.774639 0.135843 0.033 Uiso 1 1 calc R . . . .
C38 C 0.71277(13) 0.96333(10) 0.53680(9) 0.0288(3) Uani 1 1 d . . . . .
HQ H 0.777863 1.010244 0.522191 0.035 Uiso 1 1 calc R . . . .
C41 C 0.52019(13) 0.82585(9) 0.57689(9) 0.0268(3) Uani 1 1 d . . . . .
HR H 0.454095 0.778521 0.590016 0.032 Uiso 1 1 calc R . . . .
C17 C -0.30290(13) 0.28733(10) 0.03810(9) 0.0282(3) Uani 1 1 d . . . . .
HS H -0.389860 0.253993 0.044646 0.034 Uiso 1 1 calc R . . . .
HT H -0.300370 0.296709 -0.021936 0.034 Uiso 1 1 calc R . . . .
C20 C -0.03968(12) 0.37556(9) 0.11487(8) 0.0252(3) Uani 1 1 d . . . . .
HU H -0.043187 0.365977 0.175457 0.030 Uiso 1 1 calc R . . . .
C19 C -0.08130(13) 0.27895(10) 0.04610(9) 0.0284(3) Uani 1 1 d . . . . .
HV H -0.070169 0.288348 -0.013531 0.034 Uiso 1 1 calc R . . . .
HW H -0.028014 0.239462 0.056653 0.034 Uiso 1 1 calc R . . . .
C30 C 0.71853(13) 0.41717(10) 0.40276(11) 0.0333(3) Uani 1 1 d . . . . .
HX H 0.637115 0.381192 0.416749 0.040 Uiso 1 1 calc R . . . .
HY H 0.731237 0.384925 0.342168 0.040 Uiso 1 1 calc R . . . .
C2 C 0.09146(16) 0.90563(11) 0.81108(9) 0.0346(3) Uani 1 1 d . . . . .
HZ H 0.087226 0.971548 0.819766 0.041 Uiso 1 1 calc R . . . .
H0AA H 0.099653 0.894163 0.869898 0.041 Uiso 1 1 calc R . . . .
C32 C 0.81354(15) 0.47181(11) 0.56051(11) 0.0362(3) Uani 1 1 d . . . . .
H1AA H 0.885097 0.473518 0.599926 0.043 Uiso 1 1 calc R . . . .
H2AA H 0.735964 0.440017 0.582455 0.043 Uiso 1 1 calc R . . . .
C7 C 0.03078(12) 0.78236(9) 0.46490(8) 0.0233(3) Uani 1 1 d . . . . .
H3AA H 0.026135 0.722765 0.475684 0.028 Uiso 1 1 calc R . . . .
C8 C 0.00483(11) 0.78395(9) 0.37307(8) 0.0230(3) Uani 1 1 d . . . . .
C13 C -0.02019(12) 0.69838(9) 0.30798(8) 0.0236(3) Uani 1 1 d . . . . .
H4AA H -0.020007 0.642198 0.324176 0.028 Uiso 1 1 calc R . . . .
C3 C 0.20461(14) 0.89344(10) 0.76334(9) 0.0312(3) Uani 1 1 d . . . . .
H5AA H 0.213801 0.829904 0.761217 0.037 Uiso 1 1 calc R . . . .
H6AA H 0.280195 0.941398 0.797346 0.037 Uiso 1 1 calc R . . . .
C23 C 0.33747(13) 0.53458(10) 0.09304(9) 0.0299(3) Uani 1 1 d . . . . .
H7AA H 0.275039 0.532221 0.049710 0.036 Uiso 1 1 calc R . . . .
C25 C 0.55295(13) 0.58126(10) 0.15016(9) 0.0296(3) Uani 1 1 d . . . . .
H8AA H 0.638048 0.610571 0.145461 0.035 Uiso 1 1 calc R . . . .
C10 C -0.01813(13) 0.86286(10) 0.26092(9) 0.0294(3) Uani 1 1 d . . . . .
H9AA H -0.016395 0.919244 0.244484 0.035 Uiso 1 1 calc R . . . .
C18 C -0.21772(13) 0.22694(9) 0.04979(9) 0.0287(3) Uani 1 1 d . . . . .
H0BA H -0.242411 0.166480 0.002662 0.034 Uiso 1 1 calc R . . . .
H1BA H -0.227421 0.211740 0.107288 0.034 Uiso 1 1 calc R . . . .
C6 C -0.03971(13) 0.85035(10) 0.66579(9) 0.0287(3) Uani 1 1 d . . . . .
H2BA H -0.047176 0.914816 0.670251 0.034 Uiso 1 1 calc R . . . .
H3BA H -0.116416 0.803816 0.631858 0.034 Uiso 1 1 calc R . . . .
C33 C 0.81423(13) 0.57307(10) 0.56287(9) 0.0293(3) Uani 1 1 d . . . . .
H4BA H 0.894812 0.606557 0.545688 0.035 Uiso 1 1 calc R . . . .
H5BA H 0.805840 0.607488 0.623747 0.035 Uiso 1 1 calc R . . . .
C24 C 0.46112(14) 0.57914(10) 0.08747(10) 0.0322(3) Uani 1 1 d . . . . .
H6BA H 0.483365 0.608208 0.041051 0.039 Uiso 1 1 calc R . . . .
C1 C -0.02766(15) 0.83670(12) 0.75825(10) 0.0370(3) Uani 1 1 d . . . . .
H7BA H -0.100586 0.847350 0.789001 0.044 Uiso 1 1 calc R . . . .
H8BA H -0.026532 0.770739 0.753815 0.044 Uiso 1 1 calc R . . . .
C31 C 0.82177(14) 0.41547(11) 0.46726(11) 0.0355(3) Uani 1 1 d . . . . .
H9BA H 0.814834 0.348950 0.466758 0.043 Uiso 1 1 calc R . . . .
H0CA H 0.903969 0.442683 0.448150 0.043 Uiso 1 1 calc R . . . .
C43 C 0.43373(15) 0.77204(10) 0.29822(10) 0.0345(3) Uani 1 1 d . U . . .
C44 C 0.41019(14) 0.80759(10) 0.22797(10) 0.0339(3) Uani 1 1 d . U . . .
C48 C 0.55371(17) 0.77199(12) 0.32140(12) 0.0452(4) Uani 1 1 d . U . . .
H48 H 0.568699 0.747445 0.369298 0.054 Uiso 1 1 calc R . . . .
C45 C 0.50923(18) 0.84198(11) 0.18236(11) 0.0451(4) Uani 1 1 d . U . . .
H45 H 0.494842 0.866142 0.134076 0.054 Uiso 1 1 calc R . . . .
C46 C 0.63106(17) 0.84120(12) 0.20740(14) 0.0541(5) Uani 1 1 d . U . . .
H46 H 0.698511 0.864656 0.176108 0.065 Uiso 1 1 calc R . . . .
C49 C 0.3300(2) 0.73240(13) 0.34965(13) 0.0518(5) Uani 1 1 d . U . . .
H49A H 0.288426 0.780944 0.374066 0.078 Uiso 1 1 calc GR . . . .
H49B H 0.364892 0.713680 0.397865 0.078 Uiso 1 1 calc GR . . . .
H49C H 0.269420 0.676863 0.310372 0.078 Uiso 1 1 calc GR . . . .
C47 C 0.65118(17) 0.80632(14) 0.27723(14) 0.0537(5) Uani 1 1 d . U . . .
H47 H 0.732935 0.806058 0.294829 0.064 Uiso 1 1 calc R . . . .
C50 C 0.27806(19) 0.80471(16) 0.20301(13) 0.0536(5) Uani 1 1 d . U . . .
H50A H 0.225877 0.738640 0.185098 0.080 Uiso 1 1 calc GR . . . .
H50B H 0.276165 0.833412 0.153904 0.080 Uiso 1 1 calc GR . . . .
H50C H 0.246143 0.840196 0.253800 0.080 Uiso 1 1 calc GR . . . .
C62 C 0.3405(5) 0.1551(4) 0.0628(4) 0.0379(19) Uani 0.175(2) 1 d D U P A 2
C61 C 0.4166(6) 0.1756(4) 0.1406(3) 0.0409(19) Uani 0.175(2) 1 d DG U P A 2
C60 C 0.4963(6) 0.1210(4) 0.1477(3) 0.0405(19) Uani 0.175(2) 1 d G U P A 2
H1CA H 0.548330 0.135056 0.200897 0.049 Uiso 0.175(2) 1 calc R . P A 2
C59 C 0.4998(6) 0.0460(4) 0.0769(4) 0.045(2) Uani 0.175(2) 1 d G U P A 2
H2CA H 0.554230 0.008684 0.081728 0.054 Uiso 0.175(2) 1 calc R . P A 2
C64 C 0.4236(6) 0.0255(4) -0.0009(3) 0.045(2) Uani 0.175(2) 1 d G U P A 2
H3CA H 0.426043 -0.025844 -0.049322 0.054 Uiso 0.175(2) 1 calc R . P A 2
C63 C 0.3440(6) 0.0800(4) -0.0080(3) 0.043(2) Uani 0.175(2) 1 d G U P A 2
H4CA H 0.291955 0.066000 -0.061203 0.052 Uiso 0.175(2) 1 calc R . P A 2
C66 C 0.4145(14) 0.2578(8) 0.2153(8) 0.050(3) Uani 0.175(2) 1 d D U P A 2
H5CA H 0.466659 0.316568 0.204887 0.076 Uiso 0.175(2) 1 calc GR . P A 2
H6CA H 0.446829 0.249654 0.270425 0.076 Uiso 0.175(2) 1 calc GR . P A 2
H7CA H 0.328638 0.261339 0.219568 0.076 Uiso 0.175(2) 1 calc GR . P A 2
C65 C 0.2616(17) 0.2181(13) 0.0550(9) 0.069(5) Uani 0.175(2) 1 d D U P A 2
H8CA H 0.236797 0.243900 0.113084 0.104 Uiso 0.175(2) 1 calc GR . P A 2
H9CA H 0.187013 0.181529 0.014127 0.104 Uiso 0.175(2) 1 calc GR . P A 2
H0DA H 0.309199 0.270348 0.032521 0.104 Uiso 0.175(2) 1 calc GR . P A 2
C53 C 0.36689(11) 0.20269(9) 0.13788(7) 0.0378(5) Uani 0.825(2) 1 d D . P A 1
C54 C 0.29039(14) 0.10999(8) 0.11984(8) 0.0439(5) Uani 0.825(2) 1 d DG . P A 1
C55 C 0.19662(13) 0.07573(7) 0.05011(9) 0.0504(6) Uani 0.825(2) 1 d G . P A 1
H1DA H 0.144331 0.012368 0.037787 0.060 Uiso 0.825(2) 1 calc R . P A 1
C56 C 0.17936(13) 0.13418(10) -0.00157(8) 0.0516(6) Uani 0.825(2) 1 d G . P A 1
H2DA H 0.115274 0.110770 -0.049229 0.062 Uiso 0.825(2) 1 calc R . P A 1
C51 C 0.25587(15) 0.22689(9) 0.01646(9) 0.0476(6) Uani 0.825(2) 1 d G . P A 1
H3DA H 0.244069 0.266840 -0.018866 0.057 Uiso 0.825(2) 1 calc R . P A 1
C52 C 0.34963(13) 0.26115(7) 0.08619(9) 0.0400(5) Uani 0.825(2) 1 d G . P A 1
H4DA H 0.401922 0.324511 0.098514 0.048 Uiso 0.825(2) 1 calc R . P A 1
C57 C 0.4668(3) 0.2434(2) 0.21462(18) 0.0525(7) Uani 0.825(2) 1 d D . P A 1
H5DA H 0.428781 0.240159 0.269544 0.079 Uiso 0.825(2) 1 calc GR . P A 1
H6DA H 0.509047 0.309713 0.217337 0.079 Uiso 0.825(2) 1 calc GR . P A 1
H7DA H 0.527505 0.206760 0.206910 0.079 Uiso 0.825(2) 1 calc GR . P A 1
C58 C 0.3050(3) 0.0472(2) 0.1777(2) 0.0671(7) Uani 0.825(2) 1 d D . P A 1
H8DA H 0.387615 0.036746 0.173896 0.101 Uiso 0.825(2) 1 calc GR . P A 1
H9DA H 0.240571 -0.013900 0.157731 0.101 Uiso 0.825(2) 1 calc GR . P A 1
H0EA H 0.296413 0.077937 0.238918 0.101 Uiso 0.825(2) 1 calc GR . P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N6 C5 1.4652(16) . ?
N6 C7 1.2658(17) . ?
N5 C42 1.2627(18) . ?
N5 C4 1.4652(17) . ?
N4 C34 1.4640(16) . ?
N4 C35 1.2638(18) . ?
N2 C21 1.2635(18) . ?
N2 C20 1.4609(17) . ?
N3 C29 1.4651(17) . ?
N3 C28 1.2682(19) . ?
N1 C15 1.4583(16) . ?
N1 C14 1.2692(17) . ?
C12 C14 1.4773(18) . ?
C12 C11 1.3899(18) . ?
C12 C13 1.3996(18) . ?
C42 C40 1.4793(18) . ?
C21 C22 1.4789(19) . ?
C22 C27 1.3901(19) . ?
C22 C23 1.404(2) . ?
C36 C37 1.4028(19) . ?
C36 C35 1.4771(18) . ?
C36 C41 1.3918(19) . ?
C5 C4 1.5331(18) . ?
C5 C6 1.5291(18) . ?
C37 C38 1.3872(19) . ?
C15 C16 1.5345(18) . ?
C15 C20 1.5335(18) . ?
C9 C8 1.4033(18) . ?
C9 C10 1.3856(19) . ?
C4 C3 1.5345(18) . ?
C39 C40 1.3946(19) . ?
C39 C38 1.396(2) . ?
C26 C27 1.4017(19) . ?
C26 C28 1.4749(19) . ?
C26 C25 1.392(2) . ?
C34 C29 1.5318(19) . ?
C34 C33 1.5317(18) . ?
C16 C17 1.5289(18) . ?
C40 C41 1.3972(18) . ?
C29 C30 1.5300(18) . ?
C11 C10 1.398(2) . ?
C17 C18 1.5263(19) . ?
C20 C19 1.5325(19) . ?
C19 C18 1.528(2) . ?
C30 C31 1.527(2) . ?
C2 C3 1.520(2) . ?
C2 C1 1.521(2) . ?
C32 C33 1.5267(19) . ?
C32 C31 1.521(2) . ?
C7 C8 1.4735(18) . ?
C8 C13 1.3919(18) . ?
C23 C24 1.383(2) . ?
C25 C24 1.393(2) . ?
C6 C1 1.5275(19) . ?
C43 C44 1.394(2) . ?
C43 C48 1.382(2) . ?
C43 C49 1.511(2) . ?
C44 C45 1.391(2) . ?
C44 C50 1.506(2) . ?
C48 C47 1.364(3) . ?
C45 C46 1.413(3) . ?
C46 C47 1.371(3) . ?
C62 C61 1.3900 . ?
C62 C63 1.3900 . ?
C62 C65 1.489(8) . ?
C61 C60 1.3900 . ?
C61 C66 1.491(8) . ?
C60 C59 1.3900 . ?
C59 C64 1.3900 . ?
C64 C63 1.3900 . ?
C53 C54 1.3900 . ?
C53 C52 1.3900 . ?
C53 C57 1.506(3) . ?
C54 C55 1.3900 . ?
C54 C58 1.508(3) . ?
C55 C56 1.3900 . ?
C56 C51 1.3900 . ?
C51 C52 1.3900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7 N6 C5 115.98(10) . . ?
C42 N5 C4 118.23(11) . . ?
C35 N4 C34 116.12(11) . . ?
C21 N2 C20 118.10(11) . . ?
C28 N3 C29 116.83(11) . . ?
C14 N1 C15 117.64(11) . . ?
C11 C12 C14 120.88(12) . . ?
C11 C12 C13 118.86(12) . . ?
C13 C12 C14 120.26(12) . . ?
N5 C42 C40 120.81(12) . . ?
N2 C21 C22 122.33(12) . . ?
C27 C22 C21 120.39(12) . . ?
C27 C22 C23 119.27(13) . . ?
C23 C22 C21 120.33(12) . . ?
C37 C36 C35 122.76(12) . . ?
C41 C36 C37 119.34(12) . . ?
C41 C36 C35 117.90(12) . . ?
N6 C5 C4 110.26(10) . . ?
N6 C5 C6 108.71(10) . . ?
C6 C5 C4 111.94(10) . . ?
C38 C37 C36 119.92(13) . . ?
N1 C15 C16 108.46(10) . . ?
N1 C15 C20 109.26(10) . . ?
C20 C15 C16 110.50(10) . . ?
N1 C14 C12 121.00(12) . . ?
C10 C9 C8 119.71(12) . . ?
N5 C4 C5 109.34(10) . . ?
N5 C4 C3 106.44(10) . . ?
C5 C4 C3 110.40(11) . . ?
C40 C39 C38 120.54(12) . . ?
C27 C26 C28 122.57(12) . . ?
C25 C26 C27 119.23(12) . . ?
C25 C26 C28 118.20(12) . . ?
N4 C34 C29 109.33(11) . . ?
N4 C34 C33 108.49(10) . . ?
C33 C34 C29 110.90(11) . . ?
C17 C16 C15 111.70(11) . . ?
C39 C40 C42 121.05(12) . . ?
C39 C40 C41 118.76(12) . . ?
C41 C40 C42 120.19(12) . . ?
C22 C27 C26 120.54(12) . . ?
N4 C35 C36 124.06(12) . . ?
N3 C29 C34 109.39(10) . . ?
N3 C29 C30 108.12(11) . . ?
C30 C29 C34 110.78(11) . . ?
N3 C28 C26 123.41(12) . . ?
C12 C11 C10 120.35(12) . . ?
C37 C38 C39 120.21(12) . . ?
C36 C41 C40 121.19(12) . . ?
C18 C17 C16 110.44(11) . . ?
N2 C20 C15 108.73(10) . . ?
N2 C20 C19 109.32(11) . . ?
C19 C20 C15 110.22(10) . . ?
C18 C19 C20 111.71(11) . . ?
C31 C30 C29 112.84(12) . . ?
C3 C2 C1 110.58(12) . . ?
C31 C32 C33 111.00(12) . . ?
N6 C7 C8 124.51(11) . . ?
C9 C8 C7 123.18(12) . . ?
C13 C8 C9 119.33(12) . . ?
C13 C8 C7 117.49(11) . . ?
C8 C13 C12 121.19(12) . . ?
C2 C3 C4 113.16(11) . . ?
C24 C23 C22 120.54(13) . . ?
C26 C25 C24 120.63(13) . . ?
C9 C10 C11 120.54(12) . . ?
C17 C18 C19 111.08(11) . . ?
C1 C6 C5 111.17(12) . . ?
C32 C33 C34 111.10(12) . . ?
C23 C24 C25 119.76(13) . . ?
C2 C1 C6 110.50(12) . . ?
C32 C31 C30 111.25(12) . . ?
C44 C43 C49 121.27(16) . . ?
C48 C43 C44 119.85(15) . . ?
C48 C43 C49 118.88(17) . . ?
C43 C44 C50 118.62(15) . . ?
C45 C44 C43 118.63(15) . . ?
C45 C44 C50 122.73(17) . . ?
C47 C48 C43 121.65(18) . . ?
C44 C45 C46 120.42(17) . . ?
C47 C46 C45 119.48(16) . . ?
C48 C47 C46 119.96(17) . . ?
C61 C62 C63 120.0 . . ?
C61 C62 C65 119.0(8) . . ?
C63 C62 C65 120.9(8) . . ?
C62 C61 C60 120.0 . . ?
C62 C61 C66 119.5(7) . . ?
C60 C61 C66 120.5(7) . . ?
C59 C60 C61 120.0 . . ?
C64 C59 C60 120.0 . . ?
C59 C64 C63 120.0 . . ?
C64 C63 C62 120.0 . . ?
C54 C53 C52 120.0 . . ?
C54 C53 C57 121.56(15) . . ?
C52 C53 C57 118.41(15) . . ?
C53 C54 C58 120.42(15) . . ?
C55 C54 C53 120.0 . . ?
C55 C54 C58 119.53(15) . . ?
C54 C55 C56 120.0 . . ?
C51 C56 C55 120.0 . . ?
C56 C51 C52 120.0 . . ?
C51 C52 C53 120.0 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_EA_1-rac_100K_publ
_database_code_depnum_ccdc_archive 'CCDC 2073632'
loop_
_audit_author_name
_audit_author_address
'Marc Little'
;University of Liverpool
United Kingdom
;
_audit_update_record             
;
2021-03-27 deposited with the CCDC.	2021-05-14 downloaded from the CCDC.
;
_audit_creation_date             2020-11-16
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C42 H48 N6), 2(C4 H8 O2), 2(O)'
_chemical_formula_sum            'C92 H112 N12 O6'
_chemical_formula_weight         1481.93
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     DH_MC2-rac_EA
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.3324(6)
_cell_length_b                   14.3555(6)
_cell_length_c                   25.1851(9)
_cell_angle_alpha                89.815(3)
_cell_angle_beta                 77.839(4)
_cell_angle_gamma                60.849(4)
_cell_volume                     4393.8(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    15376
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      26.3690
_cell_measurement_theta_min      1.6550
_shelx_estimated_absorpt_T_max   0.989
_shelx_estimated_absorpt_T_min   0.983
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86304
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    1.120
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.247
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.163
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0730
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            27498
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.423
_diffrn_reflns_theta_min         1.635
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -95.00  47.00   0.50    5.00    --   -8.90  15.00 153.00  284
  2  ω    -31.00  -5.00   0.50    5.00    --    5.00 -57.00 -90.00   52
  3  ω    -19.00   7.00   0.50    5.00    --    5.00  57.00-180.00   52
  4  ω    -95.00 -41.00   0.50    5.00    --   -8.90 -68.00   0.00  108
  5  ω    -17.00  28.00   0.50    5.00    --   -8.90 -68.00   0.00   90
  6  ω    -97.00  10.00   0.50    5.00    --   -8.90 -68.00 -60.00  214
  7  ω    -96.00  -1.00   0.50    5.00    --   -8.90 -57.00-180.00  190
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0274798000
_diffrn_orient_matrix_UB_12      -0.0039499000
_diffrn_orient_matrix_UB_13      0.0209942000
_diffrn_orient_matrix_UB_21      0.0477064000
_diffrn_orient_matrix_UB_22      -0.0095582000
_diffrn_orient_matrix_UB_23      -0.0199789000
_diffrn_orient_matrix_UB_31      -0.0193504000
_diffrn_orient_matrix_UB_32      0.0559529000
_diffrn_orient_matrix_UB_33      0.0014596000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                16482
_reflns_number_total             27498
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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    ?
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     994
_refine_ls_number_reflns         27498
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1241
_refine_ls_R_factor_gt           0.0821
_refine_ls_restrained_S_all      1.222
_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2118
_refine_ls_wR_factor_ref         0.2277
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.5339(12)
 0.4661(12)
2. 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
3. Restrained distances
 O1-C91
 1.2 with sigma of 0.01
 C99-C100 = C94-C93
 1.49 with sigma of 0.01
 C90-C89
 1.51 with sigma of 0.01
 O2-C91
 1.34 with sigma of 0.01
 O2-C90
 1.45 with sigma of 0.01
 C92-C91
 1.49 with sigma of 0.01
 C87-C88
 1.51 with sigma of 0.01
 O3-C86
 1.34 with sigma of 0.01
 O3-C87
 1.45 with sigma of 0.01
 C85-C86
 1.49 with sigma of 0.01
 C85-O3
 2.31 with sigma of 0.01
 O4-C86
 1.2 with sigma of 0.02
 O6-C94 = O9-C99
 1.2 with sigma of 0.01
 O7-C94 = O8-C99
 1.34 with sigma of 0.01
 O8-C98 = O7-C95
 1.45 with sigma of 0.01
 C97-C98 = C95-C96
 1.51 with sigma of 0.01
 C93-O6
 2.34 with sigma of 0.02
 O9-C100
 2.34 with sigma of 0.02
 O1-C92
 2.34 with sigma of 0.02
4. Restrained planarity
 O6, O7, C93, C94, C95, C96
 with sigma of 0.01
 O3, O4, C85, C86, C87, C88
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uiso(C93) = Uiso(O6)
Uiso(C89) = Uiso(C88)
Uiso(O4) = Uiso(C85)
6. Rigid body (RIGU) restrains
 O6, O7, C93, C94, C95, C96
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O8, O9, C97, C98, C99, C100
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O1, O2, C89, C90, C91, C92
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O3, O4, C85, C86, C87, C88
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
7. Others
 Fixed Sof: O1(0.5) O2(0.5) C89(0.5) H89A(0.5) H89B(0.5) H89C(0.5) C90(0.5)
 H90A(0.5) H90B(0.5) C91(0.5) C92(0.5) H92A(0.5) H92B(0.5) H92C(0.5) O8(0.5)
 O9(0.5) C97(0.5) H97A(0.5) H97B(0.5) H97C(0.5) C98(0.5) H98A(0.5) H98B(0.5)
 C99(0.5) C100(0.5) H10A(0.5) H10B(0.5) H10C(0.5) O3(0.5) O4(0.5) C85(0.5)
 H85A(0.5) H85B(0.5) H85C(0.5) C86(0.5) C87(0.5) H87A(0.5) H87B(0.5) C88(0.5)
 H88A(0.5) H88B(0.5) H88C(0.5) O6(0.5) O7(0.5) C93(0.5) H93A(0.5) H93B(0.5)
 H93C(0.5) C94(0.5) C95(0.5) H95A(0.5) H95B(0.5) C96(0.5) H96A(0.5) H96B(0.5)
 H96C(0.5) O10(0.25) O11(0.5) O5(0.25) O12(0.25) O13(0.25) O14(0.25) O15(0.25)
8.a Ternary CH refined with riding coordinates:
 C25(H25), C30(H30), C31(H31), C36(H36), C37(H37), C42(H42), C67(H67),
 C72(H72), C73(H73), C78(H78), C79(H79), C84(H84)
8.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C32(H32A,
 H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C38(H38A,H38B),
 C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C68(H68A,H68B), C69(H69A,H69B),
  C70(H70A,H70B), C71(H71A,H71B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,
 H76B), C77(H77A,H77B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B),
 C83(H83A,H83B), C90(H90A,H90B), C98(H98A,H98B), C87(H87A,H87B), C95(H95A,H95B)
8.c Me refined with riding coordinates:
 C93(H93A,H93B,H93C)
8.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23),
  C24(H24), C44(H44), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50),
 C52(H52), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C60(H60), C62(H62),
  C63(H63), C64(H64), C65(H65), C66(H66)
8.e Idealised Me refined as rotating group:
 C89(H89A,H89B,H89C), C92(H92A,H92B,H92C), C97(H97A,H97B,H97C), C100(H10A,H10B,
 H10C), C85(H85A,H85B,H85C), C88(H88A,H88B,H88C), C96(H96A,H96B,H96C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.6460(2) 0.2979(2) 0.82109(11) 0.0387(6) Uani 1 1 d . . . . .
N2 N 0.5861(2) 0.50533(19) 0.77967(11) 0.0355(6) Uani 1 1 d . . . . .
N3 N 0.2397(2) 0.89214(19) 0.96671(12) 0.0377(6) Uani 1 1 d . . . . .
N4 N 0.1086(2) 0.8732(2) 1.06605(11) 0.0370(6) Uani 1 1 d . . . . .
N5 N 0.2486(2) 0.3942(2) 1.12850(11) 0.0371(6) Uani 1 1 d . . . . .
N6 N 0.3923(2) 0.2176(2) 1.04607(11) 0.0367(6) Uani 1 1 d . . . . .
C1 C 0.4184(3) 0.6595(2) 0.82635(14) 0.0350(7) Uani 1 1 d . . . . .
C2 C 0.3594(3) 0.7307(2) 0.87407(14) 0.0380(8) Uani 1 1 d . . . . .
H2 H 0.391137 0.719067 0.904676 0.046 Uiso 1 1 calc R U . . .
C3 C 0.2555(3) 0.8179(2) 0.87795(14) 0.0356(7) Uani 1 1 d . . . . .
C4 C 0.2077(3) 0.8304(2) 0.83401(14) 0.0398(8) Uani 1 1 d . . . . .
H4 H 0.135343 0.888330 0.836510 0.048 Uiso 1 1 calc R U . . .
C5 C 0.2640(3) 0.7596(2) 0.78662(14) 0.0410(8) Uani 1 1 d . . . . .
H5 H 0.230360 0.769208 0.756822 0.049 Uiso 1 1 calc R U . . .
C6 C 0.3684(3) 0.6755(2) 0.78247(14) 0.0367(7) Uani 1 1 d . . . . .
H6 H 0.407085 0.627847 0.749574 0.044 Uiso 1 1 calc R U . . .
C7 C 0.5304(3) 0.5712(3) 0.82210(14) 0.0379(8) Uani 1 1 d . . . . .
H7 H 0.562282 0.563209 0.852476 0.045 Uiso 1 1 calc R U . . .
C8 C 0.1967(3) 0.8961(2) 0.92720(14) 0.0361(7) Uani 1 1 d . . . . .
H8 H 0.123482 0.951888 0.929446 0.043 Uiso 1 1 calc R U . . .
C9 C 0.5026(3) 0.2567(3) 0.85725(14) 0.0400(8) Uani 1 1 d . . . . .
C10 C 0.5114(3) 0.2555(2) 0.91116(13) 0.0338(7) Uani 1 1 d . . . . .
H10 H 0.565711 0.267937 0.920280 0.041 Uiso 1 1 calc R U . . .
C11 C 0.4434(3) 0.2367(3) 0.95187(14) 0.0387(8) Uani 1 1 d . . . . .
C12 C 0.3608(4) 0.2211(4) 0.93846(16) 0.0619(11) Uani 1 1 d . . . . .
H12 H 0.312343 0.209538 0.966112 0.074 Uiso 1 1 calc R U . . .
C13 C 0.3505(5) 0.2228(5) 0.88599(18) 0.0843(17) Uani 1 1 d . . . . .
H13 H 0.294553 0.212421 0.877277 0.101 Uiso 1 1 calc R U . . .
C14 C 0.4203(4) 0.2392(4) 0.84512(16) 0.0654(12) Uani 1 1 d . . . . .
H14 H 0.412685 0.238816 0.808555 0.078 Uiso 1 1 calc R U . . .
C15 C 0.5737(3) 0.2759(2) 0.81345(13) 0.0359(7) Uani 1 1 d . . . . .
H15 H 0.565397 0.271851 0.777230 0.043 Uiso 1 1 calc R U . . .
C16 C 0.4535(3) 0.2357(2) 1.00824(13) 0.0329(7) Uani 1 1 d . . . . .
H16 H 0.507589 0.248994 1.016986 0.039 Uiso 1 1 calc R U . . .
C17 C 0.1100(3) 0.5386(3) 1.09165(15) 0.0402(8) Uani 1 1 d . . . . .
C18 C 0.1527(3) 0.6071(2) 1.09356(14) 0.0377(8) Uani 1 1 d . . . . .
H18 H 0.218025 0.583601 1.105986 0.045 Uiso 1 1 calc R U . . .
C19 C 0.1009(3) 0.7096(2) 1.07749(14) 0.0384(8) Uani 1 1 d . . . . .
C20 C 0.0046(3) 0.7434(3) 1.05956(16) 0.0430(8) Uani 1 1 d . . . . .
H20 H -0.031929 0.813197 1.048618 0.052 Uiso 1 1 calc R U . . .
C21 C -0.0375(3) 0.6757(3) 1.05774(17) 0.0491(9) Uani 1 1 d . . . . .
H21 H -0.103240 0.699193 1.045773 0.059 Uiso 1 1 calc R U . . .
C22 C 0.0157(3) 0.5730(3) 1.07330(16) 0.0481(9) Uani 1 1 d . . . . .
H22 H -0.013227 0.526407 1.071260 0.058 Uiso 1 1 calc R U . . .
C23 C 0.1660(3) 0.4282(2) 1.10804(14) 0.0381(8) Uani 1 1 d . . . . .
H23 H 0.138498 0.381471 1.102888 0.046 Uiso 1 1 calc R U . . .
C24 C 0.1521(3) 0.7780(3) 1.07792(14) 0.0385(8) Uani 1 1 d . . . . .
H24 H 0.220748 0.748618 1.087591 0.046 Uiso 1 1 calc R U . . .
C25 C 0.1773(3) 0.9777(2) 1.01196(14) 0.0341(7) Uani 1 1 d . . . . .
H25 H 0.101274 1.024735 1.006950 0.041 Uiso 1 1 calc R U . . .
C26 C 0.2342(3) 1.0444(2) 1.01200(15) 0.0397(8) Uani 1 1 d . . . . .
H26A H 0.311952 0.996327 1.012877 0.048 Uiso 1 1 calc R U . . .
H26B H 0.233402 1.078510 0.977738 0.048 Uiso 1 1 calc R U . . .
C27 C 0.1789(3) 1.1309(3) 1.06044(15) 0.0460(9) Uani 1 1 d . . . . .
H27A H 0.103493 1.183642 1.057746 0.055 Uiso 1 1 calc R U . . .
H27B H 0.220686 1.169321 1.059962 0.055 Uiso 1 1 calc R U . . .
C28 C 0.1739(4) 1.0815(3) 1.11377(16) 0.0520(10) Uani 1 1 d . . . . .
H28A H 0.134974 1.139036 1.144918 0.062 Uiso 1 1 calc R U . . .
H28B H 0.249539 1.033401 1.117911 0.062 Uiso 1 1 calc R U . . .
C29 C 0.1142(3) 1.0178(3) 1.11451(15) 0.0461(9) Uani 1 1 d . . . . .
H29A H 0.037035 1.067045 1.113041 0.055 Uiso 1 1 calc R U . . .
H29B H 0.113386 0.984927 1.149090 0.055 Uiso 1 1 calc R U . . .
C30 C 0.1704(3) 0.9294(2) 1.06589(14) 0.0356(7) Uani 1 1 d . . . . .
H30 H 0.246552 0.876926 1.069096 0.043 Uiso 1 1 calc R U . . .
C31 C 0.6995(3) 0.4246(2) 0.77808(13) 0.0369(7) Uani 1 1 d . . . . .
H31 H 0.718591 0.435924 0.812575 0.044 Uiso 1 1 calc R U . . .
C32 C 0.7745(3) 0.4372(2) 0.72924(14) 0.0393(8) Uani 1 1 d . . . . .
H32A H 0.750871 0.432553 0.695601 0.047 Uiso 1 1 calc R U . . .
H32B H 0.767140 0.508993 0.734349 0.047 Uiso 1 1 calc R U . . .
C33 C 0.8948(3) 0.3513(3) 0.72223(16) 0.0446(8) Uani 1 1 d . . . . .
H33A H 0.940476 0.360422 0.689526 0.053 Uiso 1 1 calc R U . . .
H33B H 0.920718 0.358918 0.754549 0.053 Uiso 1 1 calc R U . . .
C34 C 0.9067(3) 0.2402(3) 0.71582(14) 0.0441(8) Uani 1 1 d . . . . .
H34A H 0.984418 0.184494 0.712287 0.053 Uiso 1 1 calc R U . . .
H34B H 0.885097 0.231055 0.682208 0.053 Uiso 1 1 calc R U . . .
C35 C 0.8338(3) 0.2267(2) 0.76542(14) 0.0392(8) Uani 1 1 d . . . . .
H35A H 0.841711 0.154590 0.760791 0.047 Uiso 1 1 calc R U . . .
H35B H 0.857947 0.232360 0.798737 0.047 Uiso 1 1 calc R U . . .
C36 C 0.7133(3) 0.3123(2) 0.77228(13) 0.0355(7) Uani 1 1 d . . . . .
H36 H 0.688434 0.303760 0.739303 0.043 Uiso 1 1 calc R U . . .
C37 C 0.4084(3) 0.2170(3) 1.10166(13) 0.0368(7) Uani 1 1 d . . . . .
H37 H 0.455742 0.249318 1.103801 0.044 Uiso 1 1 calc R U . . .
C38 C 0.4659(3) 0.1011(3) 1.11488(15) 0.0420(8) Uani 1 1 d . . . . .
H38A H 0.422351 0.066932 1.109717 0.050 Uiso 1 1 calc R U . . .
H38B H 0.539272 0.060434 1.089327 0.050 Uiso 1 1 calc R U . . .
C39 C 0.4790(3) 0.0962(3) 1.17295(16) 0.0490(9) Uani 1 1 d . . . . .
H39A H 0.528518 0.123923 1.177178 0.059 Uiso 1 1 calc R U . . .
H39B H 0.513001 0.020654 1.180921 0.059 Uiso 1 1 calc R U . . .
C40 C 0.3678(3) 0.1627(3) 1.21348(15) 0.0464(9) Uani 1 1 d . . . . .
H40A H 0.320726 0.130740 1.211899 0.056 Uiso 1 1 calc R U . . .
H40B H 0.378691 0.161766 1.251054 0.056 Uiso 1 1 calc R U . . .
C41 C 0.3110(3) 0.2781(3) 1.20010(14) 0.0413(8) Uani 1 1 d . . . . .
H41A H 0.354875 0.311965 1.205200 0.050 Uiso 1 1 calc R U . . .
H41B H 0.237715 0.319095 1.225701 0.050 Uiso 1 1 calc R U . . .
C42 C 0.2973(3) 0.2836(2) 1.14140(13) 0.0354(7) Uani 1 1 d . . . . .
H42 H 0.248263 0.254484 1.137193 0.042 Uiso 1 1 calc R U . . .
N7 N 0.7333(2) 0.66047(19) 0.36781(11) 0.0367(6) Uani 1 1 d . . . . .
N8 N 0.5989(2) 0.60959(19) 0.45056(10) 0.0327(6) Uani 1 1 d . . . . .
N9 N 0.3756(2) 0.91795(19) 0.67948(11) 0.0342(6) Uani 1 1 d . . . . .
N10 N 0.4376(2) 1.06804(19) 0.71988(11) 0.0345(6) Uani 1 1 d . . . . .
N11 N 0.7663(2) 1.1369(2) 0.52734(12) 0.0382(6) Uani 1 1 d . . . . .
N12 N 0.8863(2) 0.9927(2) 0.42697(12) 0.0380(6) Uani 1 1 d . . . . .
C43 C 0.7567(3) 1.0806(2) 0.61746(15) 0.0385(8) Uani 1 1 d . . . . .
C44 C 0.6537(3) 1.0880(2) 0.62323(14) 0.0361(7) Uani 1 1 d . . . . .
H44 H 0.620654 1.103995 0.592974 0.043 Uiso 1 1 calc R U . . .
C45 C 0.5985(3) 1.0725(2) 0.67170(14) 0.0351(7) Uani 1 1 d . . . . .
C46 C 0.6474(3) 1.0509(2) 0.71624(15) 0.0419(8) Uani 1 1 d . . . . .
H46 H 0.610307 1.041736 0.750098 0.050 Uiso 1 1 calc R U . . .
C47 C 0.7496(3) 1.0426(3) 0.71127(17) 0.0493(9) Uani 1 1 d . . . . .
H47 H 0.782650 1.026240 0.741529 0.059 Uiso 1 1 calc R U . . .
C48 C 0.8040(3) 1.0580(2) 0.66247(15) 0.0436(8) Uani 1 1 d . . . . .
H48 H 0.873407 1.053094 0.659659 0.052 Uiso 1 1 calc R U . . .
C49 C 0.8133(3) 1.1008(2) 0.56638(15) 0.0379(8) Uani 1 1 d . . . . .
H49 H 0.886570 1.086504 0.562534 0.045 Uiso 1 1 calc R U . . .
C50 C 0.4892(3) 1.0860(2) 0.67679(14) 0.0349(7) Uani 1 1 d . . . . .
H50 H 0.455142 1.108862 0.647071 0.042 Uiso 1 1 calc R U . . .
C51 C 0.8877(3) 0.8244(3) 0.41842(14) 0.0383(8) Uani 1 1 d . . . . .
C52 C 0.8341(3) 0.7744(2) 0.40237(14) 0.0358(7) Uani 1 1 d . . . . .
H52 H 0.768036 0.816096 0.390838 0.043 Uiso 1 1 calc R U . . .
C53 C 0.8760(3) 0.6637(2) 0.40294(14) 0.0363(7) Uani 1 1 d . . . . .
C54 C 0.9709(3) 0.6045(3) 0.42091(15) 0.0422(8) Uani 1 1 d . . . . .
H54 H 0.999881 0.529388 0.421706 0.051 Uiso 1 1 calc R U . . .
C55 C 1.0244(3) 0.6538(3) 0.43790(16) 0.0435(8) Uani 1 1 d . . . . .
H55 H 1.089197 0.612308 0.450559 0.052 Uiso 1 1 calc R U . . .
C56 C 0.9835(3) 0.7629(3) 0.43636(15) 0.0409(8) Uani 1 1 d . . . . .
H56 H 1.020733 0.796077 0.447537 0.049 Uiso 1 1 calc R U . . .
C57 C 0.8388(3) 0.9414(2) 0.41829(14) 0.0376(8) Uani 1 1 d . . . . .
H57 H 0.767690 0.980592 0.411316 0.045 Uiso 1 1 calc R U . . .
C58 C 0.8186(3) 0.6112(2) 0.38554(13) 0.0357(7) Uani 1 1 d . . . . .
H58 H 0.847737 0.536468 0.387917 0.043 Uiso 1 1 calc R U . . .
C59 C 0.5147(3) 0.7378(2) 0.64016(13) 0.0323(7) Uani 1 1 d . . . . .
C60 C 0.4999(3) 0.7513(2) 0.58680(13) 0.0324(7) Uani 1 1 d . . . . .
H60 H 0.446058 0.818859 0.579347 0.039 Uiso 1 1 calc R U . . .
C61 C 0.5616(3) 0.6689(2) 0.54522(13) 0.0329(7) Uani 1 1 d . . . . .
C62 C 0.6400(3) 0.5697(3) 0.55601(15) 0.0470(9) Uani 1 1 d . . . . .
H62 H 0.683631 0.512271 0.527382 0.056 Uiso 1 1 calc R U . . .
C63 C 0.6541(3) 0.5550(3) 0.60905(16) 0.0549(10) Uani 1 1 d . . . . .
H63 H 0.706554 0.486819 0.616698 0.066 Uiso 1 1 calc R U . . .
C64 C 0.5928(3) 0.6384(3) 0.65036(15) 0.0451(9) Uani 1 1 d . . . . .
H64 H 0.604027 0.627854 0.686247 0.054 Uiso 1 1 calc R U . . .
C65 C 0.4485(3) 0.8250(2) 0.68542(13) 0.0336(7) Uani 1 1 d . . . . .
H65 H 0.461066 0.810756 0.720890 0.040 Uiso 1 1 calc R U . . .
C66 C 0.5446(3) 0.6842(2) 0.48914(13) 0.0353(7) Uani 1 1 d . . . . .
H66 H 0.491035 0.752415 0.482200 0.042 Uiso 1 1 calc R U . . .
C67 C 0.8256(3) 1.1615(2) 0.48030(14) 0.0360(7) Uani 1 1 d . . . . .
H67 H 0.903409 1.132788 0.482789 0.043 Uiso 1 1 calc R U . . .
C68 C 0.7696(3) 1.2833(2) 0.48151(15) 0.0427(8) Uani 1 1 d . . . . .
H68A H 0.776907 1.314130 0.514472 0.051 Uiso 1 1 calc R U . . .
H68B H 0.690192 1.312476 0.484044 0.051 Uiso 1 1 calc R U . . .
C69 C 0.8195(3) 1.3176(3) 0.43037(16) 0.0469(9) Uani 1 1 d . . . . .
H69A H 0.777610 1.396731 0.431404 0.056 Uiso 1 1 calc R U . . .
H69B H 0.896625 1.296214 0.429976 0.056 Uiso 1 1 calc R U . . .
C70 C 0.8164(3) 1.2658(3) 0.37919(16) 0.0505(9) Uani 1 1 d . . . . .
H70A H 0.851778 1.285944 0.346645 0.061 Uiso 1 1 calc R U . . .
H70B H 0.738891 1.292369 0.378034 0.061 Uiso 1 1 calc R U . . .
C71 C 0.8754(3) 1.1444(3) 0.37764(15) 0.0453(8) Uani 1 1 d . . . . .
H71A H 0.953986 1.117417 0.376456 0.054 Uiso 1 1 calc R U . . .
H71B H 0.871297 1.112364 0.344066 0.054 Uiso 1 1 calc R U . . .
C72 C 0.8242(3) 1.1099(2) 0.42773(15) 0.0383(8) Uani 1 1 d . . . . .
H72 H 0.746445 1.132625 0.427323 0.046 Uiso 1 1 calc R U . . .
C73 C 0.6829(3) 0.5987(2) 0.35426(13) 0.0347(7) Uani 1 1 d . . . . .
H73 H 0.734361 0.520567 0.354804 0.042 Uiso 1 1 calc R U . . .
C74 C 0.6606(3) 0.6170(2) 0.29717(14) 0.0394(8) Uani 1 1 d . . . . .
H74A H 0.612072 0.694583 0.295814 0.047 Uiso 1 1 calc R U . . .
H74B H 0.730791 0.593063 0.269664 0.047 Uiso 1 1 calc R U . . .
C75 C 0.6060(3) 0.5546(2) 0.28379(14) 0.0425(8) Uani 1 1 d . . . . .
H75A H 0.591705 0.567323 0.246923 0.051 Uiso 1 1 calc R U . . .
H75B H 0.656487 0.476823 0.283315 0.051 Uiso 1 1 calc R U . . .
C76 C 0.4987(3) 0.5882(3) 0.32532(15) 0.0434(8) Uani 1 1 d . . . . .
H76A H 0.466658 0.544395 0.316501 0.052 Uiso 1 1 calc R U . . .
H76B H 0.445725 0.664477 0.323644 0.052 Uiso 1 1 calc R U . . .
C77 C 0.5178(3) 0.5734(3) 0.38297(14) 0.0402(8) Uani 1 1 d . . . . .
H77A H 0.446234 0.600641 0.409806 0.048 Uiso 1 1 calc R U . . .
H77B H 0.563497 0.495936 0.385796 0.048 Uiso 1 1 calc R U . . .
C78 C 0.5751(3) 0.6330(2) 0.39658(13) 0.0350(7) Uani 1 1 d . . . . .
H78 H 0.525243 0.712004 0.397611 0.042 Uiso 1 1 calc R U . . .
C79 C 0.3238(3) 1.0944(2) 0.72297(13) 0.0330(7) Uani 1 1 d . . . . .
H79 H 0.301281 1.126233 0.689333 0.040 Uiso 1 1 calc R U . . .
C80 C 0.2509(3) 1.1764(2) 0.77330(14) 0.0366(7) Uani 1 1 d . . . . .
H80A H 0.278921 1.147101 0.805807 0.044 Uiso 1 1 calc R U . . .
H80B H 0.255373 1.242688 0.768358 0.044 Uiso 1 1 calc R U . . .
C81 C 0.1310(3) 1.2044(2) 0.78342(14) 0.0391(8) Uani 1 1 d . . . . .
H81A H 0.100201 1.240345 0.752669 0.047 Uiso 1 1 calc R U . . .
H81B H 0.087746 1.254718 0.817333 0.047 Uiso 1 1 calc R U . . .
C82 C 0.1222(3) 1.1024(2) 0.78881(14) 0.0394(8) Uani 1 1 d . . . . .
H82A H 0.146815 1.069920 0.821513 0.047 Uiso 1 1 calc R U . . .
H82B H 0.044572 1.120814 0.793433 0.047 Uiso 1 1 calc R U . . .
C83 C 0.1930(3) 1.0224(2) 0.73813(13) 0.0347(7) Uani 1 1 d . . . . .
H83A H 0.165190 1.053752 0.705875 0.042 Uiso 1 1 calc R U . . .
H83B H 0.187273 0.956662 0.742205 0.042 Uiso 1 1 calc R U . . .
C84 C 0.3134(3) 0.9928(2) 0.72862(13) 0.0328(7) Uani 1 1 d . . . . .
H84 H 0.342428 0.957866 0.760415 0.039 Uiso 1 1 calc R U . . .
O1 O 0.0432(9) 0.5091(8) 0.7777(4) 0.132(3) Uiso 0.5 1 d D . P A 1
O2 O 0.1292(7) 0.5358(6) 0.8430(4) 0.107(2) Uiso 0.5 1 d D . P A 1
C89 C 0.199(2) 0.5436(18) 0.9229(8) 0.165(5) Uiso 0.5 1 d D . P A 1
H89A H 0.235443 0.465310 0.915160 0.247 Uiso 0.5 1 calc R U P A 1
H89B H 0.133934 0.568980 0.953174 0.247 Uiso 0.5 1 calc R U P A 1
H89C H 0.250429 0.563206 0.932970 0.247 Uiso 0.5 1 calc R U P A 1
C90 C 0.1659(10) 0.5943(8) 0.8731(5) 0.092(3) Uiso 0.5 1 d D . P A 1
H90A H 0.105587 0.669444 0.884092 0.111 Uiso 0.5 1 calc R U P A 1
H90B H 0.229078 0.595738 0.848691 0.111 Uiso 0.5 1 calc R U P A 1
C91 C 0.0800(8) 0.5657(6) 0.8038(4) 0.062(2) Uiso 0.5 1 d D . P A 1
C92 C 0.0965(14) 0.6423(11) 0.7712(7) 0.129(5) Uiso 0.5 1 d D . P A 1
H92A H 0.168341 0.604940 0.745004 0.193 Uiso 0.5 1 calc R U P A 1
H92B H 0.093977 0.697472 0.795172 0.193 Uiso 0.5 1 calc R U P A 1
H92C H 0.038373 0.676076 0.751314 0.193 Uiso 0.5 1 calc R U P A 1
O8 O 0.8470(7) 0.7720(6) 0.6361(4) 0.106(2) Uiso 0.5 1 d D . P B 1
O9 O 0.9391(9) 0.6240(7) 0.6645(5) 0.132(3) Uiso 0.5 1 d D . P B 1
C97 C 0.7440(11) 0.7992(12) 0.5590(6) 0.093(3) Uiso 0.5 1 d D . P B 1
H97A H 0.737553 0.752172 0.533670 0.140 Uiso 0.5 1 calc R U P B 1
H97B H 0.770441 0.843053 0.538297 0.140 Uiso 0.5 1 calc R U P B 1
H97C H 0.671837 0.846113 0.583591 0.140 Uiso 0.5 1 calc R U P B 1
C98 C 0.8267(12) 0.7297(10) 0.5932(5) 0.101(4) Uiso 0.5 1 d D . P B 1
H98A H 0.803331 0.678590 0.608391 0.122 Uiso 0.5 1 calc R U P B 1
H98B H 0.898653 0.686269 0.566888 0.122 Uiso 0.5 1 calc R U P B 1
C99 C 0.9049(8) 0.7257(7) 0.6687(4) 0.074(2) Uiso 0.5 1 d D . P B 1
C100 C 0.9256(11) 0.7663(9) 0.7136(5) 0.097(3) Uiso 0.5 1 d D . P B 1
H10A H 0.969057 0.800764 0.700032 0.145 Uiso 0.5 1 calc R U P B 1
H10B H 0.966412 0.707017 0.733716 0.145 Uiso 0.5 1 calc R U P B 1
H10C H 0.855522 0.818953 0.737952 0.145 Uiso 0.5 1 calc R U P B 1
O3 O 0.4020(8) 0.5206(6) 0.9425(4) 0.123(3) Uiso 0.5 1 d D . P C 2
O4 O 0.3998(12) 0.5555(11) 1.0298(7) 0.182(4) Uiso 0.5 1 d D . P C 2
C85 C 0.5651(12) 0.4913(16) 0.9619(10) 0.182(4) Uiso 0.5 1 d D . P C 2
H85A H 0.575784 0.549680 0.973588 0.273 Uiso 0.5 1 calc R U P C 2
H85B H 0.584474 0.479032 0.921819 0.273 Uiso 0.5 1 calc R U P C 2
H85C H 0.612171 0.425560 0.976378 0.273 Uiso 0.5 1 calc R U P C 2
C86 C 0.4498(9) 0.5204(7) 0.9824(4) 0.075(2) Uiso 0.5 1 d D . P C 2
C87 C 0.2890(10) 0.5601(9) 0.9526(6) 0.110(4) Uiso 0.5 1 d D . P C 2
H87A H 0.251967 0.638722 0.962372 0.131 Uiso 0.5 1 calc R U P C 2
H87B H 0.268070 0.529807 0.985370 0.131 Uiso 0.5 1 calc R U P C 2
C88 C 0.2408(19) 0.5400(16) 0.9080(8) 0.165(5) Uiso 0.5 1 d D . P C 2
H88A H 0.275157 0.551826 0.872650 0.247 Uiso 0.5 1 calc R U P C 2
H88B H 0.161259 0.589577 0.916512 0.247 Uiso 0.5 1 calc R U P C 2
H88C H 0.255247 0.465869 0.906410 0.247 Uiso 0.5 1 calc R U P C 2
O6 O 0.5400(14) 1.0419(13) 0.5327(7) 0.224(5) Uiso 0.5 1 d D . P D 2
O7 O 0.6330(7) 0.8702(7) 0.5190(4) 0.125(3) Uiso 0.5 1 d D . P D 2
C93 C 0.5111(17) 0.963(2) 0.4614(7) 0.224(5) Uiso 0.5 1 d D . P D 2
H93A H 0.539906 0.888772 0.445392 0.336 Uiso 0.5 1 calc R U P D 2
H93B H 0.431132 0.996886 0.475249 0.336 Uiso 0.5 1 calc R U P D 2
H93C H 0.528287 1.002992 0.433306 0.336 Uiso 0.5 1 calc R U P D 2
C94 C 0.5622(8) 0.9610(9) 0.5067(6) 0.112(4) Uiso 0.5 1 d D . P D 2
C95 C 0.6842(10) 0.8613(11) 0.5600(5) 0.120(5) Uiso 0.5 1 d D . P D 2
H95A H 0.629153 0.893329 0.595343 0.144 Uiso 0.5 1 calc R U P D 2
H95B H 0.726593 0.899464 0.553164 0.144 Uiso 0.5 1 calc R U P D 2
C96 C 0.7601(13) 0.7437(12) 0.5616(7) 0.145(7) Uiso 0.5 1 d D . P D 2
H96A H 0.824180 0.716805 0.530515 0.217 Uiso 0.5 1 calc R U P D 2
H96B H 0.721088 0.704092 0.559703 0.217 Uiso 0.5 1 calc R U P D 2
H96C H 0.784501 0.733706 0.595815 0.217 Uiso 0.5 1 calc R U P D 2
O10 O 0.920(2) 0.6469(19) 0.5819(11) 0.157(8) Uiso 0.25 1 d . . P E 2
O11 O 0.9887(13) 0.6353(11) 0.7327(7) 0.188(5) Uiso 0.5 1 d . . P F 2
O5 O 0.6238(15) 0.5087(13) 1.0156(8) 0.105(5) Uiso 0.25 1 d . . P G 3
O12 O 0.0375(12) 0.5875(11) 0.7732(6) 0.080(4) Uiso 0.25 1 d . . P H 2
O13 O 0.7628(11) 0.8068(10) 0.5953(6) 0.069(3) Uiso 0.25 1 d . . P I 3
O14 O 0.079(3) 0.642(3) 0.8210(16) 0.213(12) Uiso 0.25 1 d . . P J 3
O15 O 0.4793(14) 0.5671(12) 0.9621(7) 0.094(4) Uiso 0.25 1 d . . P K 4


_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 C15 1.270(4) . ?
N1 C36 1.476(4) . ?
N2 C7 1.259(4) . ?
N2 C31 1.458(4) . ?
N3 C8 1.264(4) . ?
N3 C25 1.455(4) . ?
N4 C24 1.262(4) . ?
N4 C30 1.460(4) . ?
N5 C23 1.264(4) . ?
N5 C42 1.458(4) . ?
N6 C16 1.270(4) . ?
N6 C37 1.466(4) . ?
C1 C2 1.393(5) . ?
C1 C6 1.399(5) . ?
C1 C7 1.464(5) . ?
C2 H2 0.9500 . ?
C2 C3 1.385(5) . ?
C3 C4 1.387(5) . ?
C3 C8 1.468(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.383(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.372(5) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.389(5) . ?
C9 C14 1.410(5) . ?
C9 C15 1.460(5) . ?
C10 H10 0.9500 . ?
C10 C11 1.381(5) . ?
C11 C12 1.412(5) . ?
C11 C16 1.456(5) . ?
C12 H12 0.9500 . ?
C12 C13 1.359(6) . ?
C13 H13 0.9500 . ?
C13 C14 1.382(6) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.395(4) . ?
C17 C22 1.377(5) . ?
C17 C23 1.491(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.392(4) . ?
C19 C20 1.398(5) . ?
C19 C24 1.485(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.375(5) . ?
C21 H21 0.9500 . ?
C21 C22 1.390(5) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 H25 1.0000 . ?
C25 C26 1.531(4) . ?
C25 C30 1.529(5) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.517(5) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.522(5) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.524(5) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.536(5) . ?
C30 H30 1.0000 . ?
C31 H31 1.0000 . ?
C31 C32 1.527(5) . ?
C31 C36 1.529(4) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.525(5) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.525(5) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.528(5) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.527(5) . ?
C36 H36 1.0000 . ?
C37 H37 1.0000 . ?
C37 C38 1.527(4) . ?
C37 C42 1.518(5) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.510(5) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.527(6) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40 C41 1.523(5) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.528(4) . ?
C42 H42 1.0000 . ?
N7 C58 1.257(4) . ?
N7 C73 1.468(4) . ?
N8 C66 1.254(4) . ?
N8 C78 1.469(4) . ?
N9 C65 1.266(4) . ?
N9 C84 1.446(4) . ?
N10 C50 1.279(4) . ?
N10 C79 1.467(4) . ?
N11 C49 1.274(4) . ?
N11 C67 1.454(4) . ?
N12 C57 1.269(4) . ?
N12 C72 1.469(4) . ?
C43 C44 1.404(5) . ?
C43 C48 1.399(5) . ?
C43 C49 1.478(5) . ?
C44 H44 0.9500 . ?
C44 C45 1.388(5) . ?
C45 C46 1.401(5) . ?
C45 C50 1.459(5) . ?
C46 H46 0.9500 . ?
C46 C47 1.390(5) . ?
C47 H47 0.9500 . ?
C47 C48 1.389(5) . ?
C48 H48 0.9500 . ?
C49 H49 0.9500 . ?
C50 H50 0.9500 . ?
C51 C52 1.391(4) . ?
C51 C56 1.396(5) . ?
C51 C57 1.472(4) . ?
C52 H52 0.9500 . ?
C52 C53 1.400(4) . ?
C53 C54 1.381(5) . ?
C53 C58 1.482(4) . ?
C54 H54 0.9500 . ?
C54 C55 1.394(5) . ?
C55 H55 0.9500 . ?
C55 C56 1.384(5) . ?
C56 H56 0.9500 . ?
C57 H57 0.9500 . ?
C58 H58 0.9500 . ?
C59 C60 1.402(4) . ?
C59 C64 1.385(4) . ?
C59 C65 1.470(4) . ?
C60 H60 0.9500 . ?
C60 C61 1.370(4) . ?
C61 C62 1.389(4) . ?
C61 C66 1.481(4) . ?
C62 H62 0.9500 . ?
C62 C63 1.393(5) . ?
C63 H63 0.9500 . ?
C63 C64 1.374(5) . ?
C64 H64 0.9500 . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?
C67 H67 1.0000 . ?
C67 C68 1.524(4) . ?
C67 C72 1.527(5) . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
C68 C69 1.538(5) . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?
C69 C70 1.510(5) . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
C70 C71 1.517(5) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C71 C72 1.528(5) . ?
C72 H72 1.0000 . ?
C73 H73 1.0000 . ?
C73 C74 1.532(4) . ?
C73 C78 1.527(5) . ?
C74 H74A 0.9900 . ?
C74 H74B 0.9900 . ?
C74 C75 1.525(5) . ?
C75 H75A 0.9900 . ?
C75 H75B 0.9900 . ?
C75 C76 1.516(5) . ?
C76 H76A 0.9900 . ?
C76 H76B 0.9900 . ?
C76 C77 1.529(5) . ?
C77 H77A 0.9900 . ?
C77 H77B 0.9900 . ?
C77 C78 1.527(4) . ?
C78 H78 1.0000 . ?
C79 H79 1.0000 . ?
C79 C80 1.529(5) . ?
C79 C84 1.541(4) . ?
C80 H80A 0.9900 . ?
C80 H80B 0.9900 . ?
C80 C81 1.524(5) . ?
C81 H81A 0.9900 . ?
C81 H81B 0.9900 . ?
C81 C82 1.533(4) . ?
C82 H82A 0.9900 . ?
C82 H82B 0.9900 . ?
C82 C83 1.518(5) . ?
C83 H83A 0.9900 . ?
C83 H83B 0.9900 . ?
C83 C84 1.526(4) . ?
C84 H84 1.0000 . ?
O1 C91 1.393(9) . ?
O2 C90 1.469(9) . ?
O2 C91 1.285(9) . ?
C89 H89A 0.9800 . ?
C89 H89B 0.9800 . ?
C89 H89C 0.9800 . ?
C89 C90 1.498(11) . ?
C90 H90A 0.9900 . ?
C90 H90B 0.9900 . ?
C91 C92 1.452(10) . ?
C92 H92A 0.9800 . ?
C92 H92B 0.9800 . ?
C92 H92C 0.9800 . ?
O8 C98 1.389(10) . ?
O8 C99 1.244(8) . ?
O9 C99 1.290(8) . ?
C97 H97A 0.9800 . ?
C97 H97B 0.9800 . ?
C97 H97C 0.9800 . ?
C97 C98 1.554(11) . ?
C98 H98A 0.9900 . ?
C98 H98B 0.9900 . ?
C99 C100 1.421(10) . ?
C100 H10A 0.9800 . ?
C100 H10B 0.9800 . ?
C100 H10C 0.9800 . ?
O3 C86 1.331(9) . ?
O3 C87 1.393(10) . ?
O4 C85 0.68(2) 2_667 ?
O4 C86 1.217(15) . ?
O4 C86 1.833(19) 2_667 ?
C85 H85A 0.9800 . ?
C85 H85B 0.9800 . ?
C85 H85C 0.9800 . ?
C85 C86 1.463(11) . ?
C86 C86 1.70(2) 2_667 ?
C87 H87A 0.9900 . ?
C87 H87B 0.9900 . ?
C87 C88 1.530(11) . ?
C88 H88A 0.9800 . ?
C88 H88B 0.9800 . ?
C88 H88C 0.9800 . ?
O6 C93 0.75(2) 2_676 ?
O6 H93B 0.51(3) 2_676 ?
O6 C94 1.199(11) . ?
O7 C94 1.291(10) . ?
O7 C95 1.358(10) . ?
C93 H93A 0.9800 . ?
C93 H93B 0.9800 . ?
C93 H93C 0.9800 . ?
C93 C94 1.476(12) . ?
C94 C94 1.69(2) 2_676 ?
C95 H95A 0.9900 . ?
C95 H95B 0.9900 . ?
C95 C96 1.504(11) . ?
C96 H96A 0.9800 . ?
C96 H96B 0.9800 . ?
C96 H96C 0.9800 . ?
O11 O12 1.351(19) 1_655 ?

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
C15 N1 C36 117.0(3) . . ?
C7 N2 C31 118.2(3) . . ?
C8 N3 C25 118.3(3) . . ?
C24 N4 C30 117.2(3) . . ?
C23 N5 C42 117.2(2) . . ?
C16 N6 C37 118.7(3) . . ?
C2 C1 C6 118.3(3) . . ?
C2 C1 C7 120.7(3) . . ?
C6 C1 C7 121.0(3) . . ?
C1 C2 H2 119.2 . . ?
C3 C2 C1 121.6(3) . . ?
C3 C2 H2 119.2 . . ?
C2 C3 C4 118.5(3) . . ?
C2 C3 C8 121.1(3) . . ?
C4 C3 C8 120.3(3) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 C3 120.8(3) . . ?
C5 C4 H4 119.6 . . ?
C4 C5 H5 119.9 . . ?
C6 C5 C4 120.3(3) . . ?
C6 C5 H5 119.9 . . ?
C1 C6 H6 119.8 . . ?
C5 C6 C1 120.5(3) . . ?
C5 C6 H6 119.8 . . ?
N2 C7 C1 122.4(3) . . ?
N2 C7 H7 118.8 . . ?
C1 C7 H7 118.8 . . ?
N3 C8 C3 122.6(3) . . ?
N3 C8 H8 118.7 . . ?
C3 C8 H8 118.7 . . ?
C10 C9 C14 117.7(3) . . ?
C10 C9 C15 122.9(3) . . ?
C14 C9 C15 119.3(3) . . ?
C9 C10 H10 119.1 . . ?
C11 C10 C9 121.9(3) . . ?
C11 C10 H10 119.1 . . ?
C10 C11 C12 118.9(3) . . ?
C10 C11 C16 121.3(3) . . ?
C12 C11 C16 119.8(3) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 C11 120.0(4) . . ?
C13 C12 H12 120.0 . . ?
C12 C13 H13 119.5 . . ?
C12 C13 C14 120.9(4) . . ?
C14 C13 H13 119.5 . . ?
C9 C14 H14 119.7 . . ?
C13 C14 C9 120.5(3) . . ?
C13 C14 H14 119.7 . . ?
N1 C15 C9 123.6(3) . . ?
N1 C15 H15 118.2 . . ?
C9 C15 H15 118.2 . . ?
N6 C16 C11 122.1(3) . . ?
N6 C16 H16 118.9 . . ?
C11 C16 H16 118.9 . . ?
C18 C17 C23 121.1(3) . . ?
C22 C17 C18 119.2(3) . . ?
C22 C17 C23 119.6(3) . . ?
C17 C18 H18 119.6 . . ?
C19 C18 C17 120.8(3) . . ?
C19 C18 H18 119.6 . . ?
C18 C19 C20 119.0(3) . . ?
C18 C19 C24 118.9(3) . . ?
C20 C19 C24 122.1(3) . . ?
C19 C20 H20 119.9 . . ?
C21 C20 C19 120.1(3) . . ?
C21 C20 H20 119.9 . . ?
C20 C21 H21 119.8 . . ?
C20 C21 C22 120.4(3) . . ?
C22 C21 H21 119.8 . . ?
C17 C22 C21 120.4(3) . . ?
C17 C22 H22 119.8 . . ?
C21 C22 H22 119.8 . . ?
N5 C23 C17 122.7(3) . . ?
N5 C23 H23 118.6 . . ?
C17 C23 H23 118.6 . . ?
N4 C24 C19 123.2(3) . . ?
N4 C24 H24 118.4 . . ?
C19 C24 H24 118.4 . . ?
N3 C25 H25 109.2 . . ?
N3 C25 C26 108.8(3) . . ?
N3 C25 C30 109.7(2) . . ?
C26 C25 H25 109.2 . . ?
C30 C25 H25 109.2 . . ?
C30 C25 C26 110.7(3) . . ?
C25 C26 H26A 109.1 . . ?
C25 C26 H26B 109.1 . . ?
H26A C26 H26B 107.9 . . ?
C27 C26 C25 112.3(3) . . ?
C27 C26 H26A 109.1 . . ?
C27 C26 H26B 109.1 . . ?
C26 C27 H27A 109.6 . . ?
C26 C27 H27B 109.6 . . ?
C26 C27 C28 110.4(3) . . ?
H27A C27 H27B 108.1 . . ?
C28 C27 H27A 109.6 . . ?
C28 C27 H27B 109.6 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 C29 110.6(3) . . ?
H28A C28 H28B 108.1 . . ?
C29 C28 H28A 109.5 . . ?
C29 C28 H28B 109.5 . . ?
C28 C29 H29A 109.4 . . ?
C28 C29 H29B 109.4 . . ?
C28 C29 C30 111.2(3) . . ?
H29A C29 H29B 108.0 . . ?
C30 C29 H29A 109.4 . . ?
C30 C29 H29B 109.4 . . ?
N4 C30 C25 109.2(3) . . ?
N4 C30 C29 110.1(3) . . ?
N4 C30 H30 109.0 . . ?
C25 C30 C29 110.5(2) . . ?
C25 C30 H30 109.0 . . ?
C29 C30 H30 109.0 . . ?
N2 C31 H31 109.5 . . ?
N2 C31 C32 108.3(2) . . ?
N2 C31 C36 109.8(3) . . ?
C32 C31 H31 109.5 . . ?
C32 C31 C36 110.1(3) . . ?
C36 C31 H31 109.5 . . ?
C31 C32 H32A 109.2 . . ?
C31 C32 H32B 109.2 . . ?
H32A C32 H32B 107.9 . . ?
C33 C32 C31 112.0(3) . . ?
C33 C32 H32A 109.2 . . ?
C33 C32 H32B 109.2 . . ?
C32 C33 H33A 109.7 . . ?
C32 C33 H33B 109.7 . . ?
H33A C33 H33B 108.2 . . ?
C34 C33 C32 109.7(3) . . ?
C34 C33 H33A 109.7 . . ?
C34 C33 H33B 109.7 . . ?
C33 C34 H34A 109.7 . . ?
C33 C34 H34B 109.7 . . ?
C33 C34 C35 110.0(3) . . ?
H34A C34 H34B 108.2 . . ?
C35 C34 H34A 109.7 . . ?
C35 C34 H34B 109.7 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 108.1 . . ?
C36 C35 C34 110.9(3) . . ?
C36 C35 H35A 109.5 . . ?
C36 C35 H35B 109.5 . . ?
N1 C36 C31 110.1(3) . . ?
N1 C36 C35 109.3(2) . . ?
N1 C36 H36 109.0 . . ?
C31 C36 H36 109.0 . . ?
C35 C36 C31 110.4(3) . . ?
C35 C36 H36 109.0 . . ?
N6 C37 H37 109.2 . . ?
N6 C37 C38 109.1(3) . . ?
N6 C37 C42 108.9(3) . . ?
C38 C37 H37 109.2 . . ?
C42 C37 H37 109.2 . . ?
C42 C37 C38 111.2(3) . . ?
C37 C38 H38A 109.4 . . ?
C37 C38 H38B 109.4 . . ?
H38A C38 H38B 108.0 . . ?
C39 C38 C37 111.3(3) . . ?
C39 C38 H38A 109.4 . . ?
C39 C38 H38B 109.4 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 C40 110.9(3) . . ?
H39A C39 H39B 108.0 . . ?
C40 C39 H39A 109.5 . . ?
C40 C39 H39B 109.5 . . ?
C39 C40 H40A 109.6 . . ?
C39 C40 H40B 109.6 . . ?
H40A C40 H40B 108.1 . . ?
C41 C40 C39 110.4(3) . . ?
C41 C40 H40A 109.6 . . ?
C41 C40 H40B 109.6 . . ?
C40 C41 H41A 109.3 . . ?
C40 C41 H41B 109.3 . . ?
C40 C41 C42 111.7(3) . . ?
H41A C41 H41B 108.0 . . ?
C42 C41 H41A 109.3 . . ?
C42 C41 H41B 109.3 . . ?
N5 C42 C37 108.9(3) . . ?
N5 C42 C41 110.7(3) . . ?
N5 C42 H42 109.1 . . ?
C37 C42 C41 110.0(3) . . ?
C37 C42 H42 109.1 . . ?
C41 C42 H42 109.1 . . ?
C58 N7 C73 117.2(2) . . ?
C66 N8 C78 117.5(3) . . ?
C65 N9 C84 116.4(3) . . ?
C50 N10 C79 117.9(3) . . ?
C49 N11 C67 117.8(3) . . ?
C57 N12 C72 116.8(3) . . ?
C44 C43 C49 121.9(3) . . ?
C48 C43 C44 118.4(3) . . ?
C48 C43 C49 119.7(3) . . ?
C43 C44 H44 118.9 . . ?
C45 C44 C43 122.1(3) . . ?
C45 C44 H44 118.9 . . ?
C44 C45 C46 118.3(3) . . ?
C44 C45 C50 120.4(3) . . ?
C46 C45 C50 121.3(3) . . ?
C45 C46 H46 119.8 . . ?
C47 C46 C45 120.5(3) . . ?
C47 C46 H46 119.8 . . ?
C46 C47 H47 119.7 . . ?
C48 C47 C46 120.6(4) . . ?
C48 C47 H47 119.7 . . ?
C43 C48 H48 119.9 . . ?
C47 C48 C43 120.1(3) . . ?
C47 C48 H48 119.9 . . ?
N11 C49 C43 121.8(3) . . ?
N11 C49 H49 119.1 . . ?
C43 C49 H49 119.1 . . ?
N10 C50 C45 122.3(3) . . ?
N10 C50 H50 118.8 . . ?
C45 C50 H50 118.8 . . ?
C52 C51 C56 119.1(3) . . ?
C52 C51 C57 119.0(3) . . ?
C56 C51 C57 121.9(3) . . ?
C51 C52 H52 119.4 . . ?
C51 C52 C53 121.1(3) . . ?
C53 C52 H52 119.4 . . ?
C52 C53 C58 120.7(3) . . ?
C54 C53 C52 118.8(3) . . ?
C54 C53 C58 120.5(3) . . ?
C53 C54 H54 119.7 . . ?
C53 C54 C55 120.7(3) . . ?
C55 C54 H54 119.7 . . ?
C54 C55 H55 119.9 . . ?
C56 C55 C54 120.1(3) . . ?
C56 C55 H55 119.9 . . ?
C51 C56 H56 119.9 . . ?
C55 C56 C51 120.2(3) . . ?
C55 C56 H56 119.9 . . ?
N12 C57 C51 123.7(3) . . ?
N12 C57 H57 118.2 . . ?
C51 C57 H57 118.2 . . ?
N7 C58 C53 123.3(3) . . ?
N7 C58 H58 118.3 . . ?
C53 C58 H58 118.3 . . ?
C60 C59 C65 122.1(3) . . ?
C64 C59 C60 118.5(3) . . ?
C64 C59 C65 119.4(3) . . ?
C59 C60 H60 119.4 . . ?
C61 C60 C59 121.3(3) . . ?
C61 C60 H60 119.4 . . ?
C60 C61 C62 119.6(3) . . ?
C60 C61 C66 120.6(3) . . ?
C62 C61 C66 119.8(3) . . ?
C61 C62 H62 120.2 . . ?
C61 C62 C63 119.6(3) . . ?
C63 C62 H62 120.2 . . ?
C62 C63 H63 119.8 . . ?
C64 C63 C62 120.4(3) . . ?
C64 C63 H63 119.8 . . ?
C59 C64 H64 119.7 . . ?
C63 C64 C59 120.6(3) . . ?
C63 C64 H64 119.7 . . ?
N9 C65 C59 123.3(3) . . ?
N9 C65 H65 118.4 . . ?
C59 C65 H65 118.4 . . ?
N8 C66 C61 121.9(3) . . ?
N8 C66 H66 119.1 . . ?
C61 C66 H66 119.1 . . ?
N11 C67 H67 109.4 . . ?
N11 C67 C68 108.0(3) . . ?
N11 C67 C72 109.7(2) . . ?
C68 C67 H67 109.4 . . ?
C68 C67 C72 110.9(3) . . ?
C72 C67 H67 109.4 . . ?
C67 C68 H68A 109.2 . . ?
C67 C68 H68B 109.2 . . ?
C67 C68 C69 112.1(3) . . ?
H68A C68 H68B 107.9 . . ?
C69 C68 H68A 109.2 . . ?
C69 C68 H68B 109.2 . . ?
C68 C69 H69A 109.6 . . ?
C68 C69 H69B 109.6 . . ?
H69A C69 H69B 108.1 . . ?
C70 C69 C68 110.4(3) . . ?
C70 C69 H69A 109.6 . . ?
C70 C69 H69B 109.6 . . ?
C69 C70 H70A 109.5 . . ?
C69 C70 H70B 109.5 . . ?
C69 C70 C71 110.9(3) . . ?
H70A C70 H70B 108.0 . . ?
C71 C70 H70A 109.5 . . ?
C71 C70 H70B 109.5 . . ?
C70 C71 H71A 109.4 . . ?
C70 C71 H71B 109.4 . . ?
C70 C71 C72 111.1(3) . . ?
H71A C71 H71B 108.0 . . ?
C72 C71 H71A 109.4 . . ?
C72 C71 H71B 109.4 . . ?
N12 C72 C67 108.4(3) . . ?
N12 C72 C71 110.2(3) . . ?
N12 C72 H72 109.2 . . ?
C67 C72 C71 110.6(2) . . ?
C67 C72 H72 109.2 . . ?
C71 C72 H72 109.2 . . ?
N7 C73 H73 109.1 . . ?
N7 C73 C74 110.3(2) . . ?
N7 C73 C78 109.6(2) . . ?
C74 C73 H73 109.1 . . ?
C78 C73 H73 109.1 . . ?
C78 C73 C74 109.7(3) . . ?
C73 C74 H74A 109.6 . . ?
C73 C74 H74B 109.6 . . ?
H74A C74 H74B 108.2 . . ?
C75 C74 C73 110.1(3) . . ?
C75 C74 H74A 109.6 . . ?
C75 C74 H74B 109.6 . . ?
C74 C75 H75A 109.4 . . ?
C74 C75 H75B 109.4 . . ?
H75A C75 H75B 108.0 . . ?
C76 C75 C74 111.3(3) . . ?
C76 C75 H75A 109.4 . . ?
C76 C75 H75B 109.4 . . ?
C75 C76 H76A 109.6 . . ?
C75 C76 H76B 109.6 . . ?
C75 C76 C77 110.5(3) . . ?
H76A C76 H76B 108.1 . . ?
C77 C76 H76A 109.6 . . ?
C77 C76 H76B 109.6 . . ?
C76 C77 H77A 109.4 . . ?
C76 C77 H77B 109.4 . . ?
H77A C77 H77B 108.0 . . ?
C78 C77 C76 111.2(3) . . ?
C78 C77 H77A 109.4 . . ?
C78 C77 H77B 109.4 . . ?
N8 C78 C73 108.9(3) . . ?
N8 C78 C77 109.0(2) . . ?
N8 C78 H78 109.2 . . ?
C73 C78 H78 109.2 . . ?
C77 C78 C73 111.4(3) . . ?
C77 C78 H78 109.2 . . ?
N10 C79 H79 109.8 . . ?
N10 C79 C80 107.4(2) . . ?
N10 C79 C84 110.3(2) . . ?
C80 C79 H79 109.8 . . ?
C80 C79 C84 109.9(3) . . ?
C84 C79 H79 109.8 . . ?
C79 C80 H80A 109.1 . . ?
C79 C80 H80B 109.1 . . ?
H80A C80 H80B 107.8 . . ?
C81 C80 C79 112.5(3) . . ?
C81 C80 H80A 109.1 . . ?
C81 C80 H80B 109.1 . . ?
C80 C81 H81A 109.6 . . ?
C80 C81 H81B 109.6 . . ?
C80 C81 C82 110.2(3) . . ?
H81A C81 H81B 108.1 . . ?
C82 C81 H81A 109.6 . . ?
C82 C81 H81B 109.6 . . ?
C81 C82 H82A 109.7 . . ?
C81 C82 H82B 109.7 . . ?
H82A C82 H82B 108.2 . . ?
C83 C82 C81 110.0(3) . . ?
C83 C82 H82A 109.7 . . ?
C83 C82 H82B 109.7 . . ?
C82 C83 H83A 109.3 . . ?
C82 C83 H83B 109.3 . . ?
C82 C83 C84 111.7(3) . . ?
H83A C83 H83B 107.9 . . ?
C84 C83 H83A 109.3 . . ?
C84 C83 H83B 109.3 . . ?
N9 C84 C79 110.3(3) . . ?
N9 C84 C83 108.9(2) . . ?
N9 C84 H84 109.2 . . ?
C79 C84 H84 109.2 . . ?
C83 C84 C79 110.1(3) . . ?
C83 C84 H84 109.2 . . ?
C91 O2 C90 127.9(8) . . ?
H89A C89 H89B 109.5 . . ?
H89A C89 H89C 109.5 . . ?
H89B C89 H89C 109.5 . . ?
C90 C89 H89A 109.5 . . ?
C90 C89 H89B 109.5 . . ?
C90 C89 H89C 109.5 . . ?
O2 C90 C89 111.8(11) . . ?
O2 C90 H90A 109.3 . . ?
O2 C90 H90B 109.3 . . ?
C89 C90 H90A 109.3 . . ?
C89 C90 H90B 109.3 . . ?
H90A C90 H90B 107.9 . . ?
O1 C91 C92 113.1(9) . . ?
O2 C91 O1 126.0(8) . . ?
O2 C91 C92 117.3(9) . . ?
C91 C92 H92A 109.5 . . ?
C91 C92 H92B 109.5 . . ?
C91 C92 H92C 109.5 . . ?
H92A C92 H92B 109.5 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 109.5 . . ?
C99 O8 C98 130.1(9) . . ?
H97A C97 H97B 109.5 . . ?
H97A C97 H97C 109.5 . . ?
H97B C97 H97C 109.5 . . ?
C98 C97 H97A 109.5 . . ?
C98 C97 H97B 109.5 . . ?
C98 C97 H97C 109.5 . . ?
O8 C98 C97 123.8(11) . . ?
O8 C98 H98A 106.4 . . ?
O8 C98 H98B 106.4 . . ?
C97 C98 H98A 106.4 . . ?
C97 C98 H98B 106.4 . . ?
H98A C98 H98B 106.5 . . ?
O8 C99 O9 112.2(9) . . ?
O8 C99 C100 131.6(9) . . ?
O9 C99 C100 115.5(9) . . ?
C99 C100 H10A 109.5 . . ?
C99 C100 H10B 109.5 . . ?
C99 C100 H10C 109.5 . . ?
H10A C100 H10B 109.5 . . ?
H10A C100 H10C 109.5 . . ?
H10B C100 H10C 109.5 . . ?
C86 O3 C87 121.5(11) . . ?
C85 O4 C86 90(3) 2_667 . ?
H85A C85 H85B 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
C86 C85 H85A 109.5 . . ?
C86 C85 H85B 109.5 . . ?
C86 C85 H85C 109.5 . . ?
O3 C86 C85 112.5(10) . . ?
O4 C86 O3 123.7(13) . . ?
O4 C86 C85 123.0(15) . . ?
C85 C86 C85 106.8(13) 2_667 . ?
O3 C87 H87A 107.5 . . ?
O3 C87 H87B 107.5 . . ?
O3 C87 C88 119.5(13) . . ?
H87A C87 H87B 107.0 . . ?
C88 C87 H87A 107.5 . . ?
C88 C87 H87B 107.5 . . ?
C87 C88 H88A 109.5 . . ?
C87 C88 H88B 109.5 . . ?
C87 C88 H88C 109.5 . . ?
H88A C88 H88B 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
C93 O6 C94 73(2) 2_676 . ?
C94 O7 C95 123.5(12) . . ?
H93A C93 H93B 109.5 . . ?
H93A C93 H93C 109.5 . . ?
H93B C93 H93C 109.5 . . ?
C94 C93 H93A 109.5 . . ?
C94 C93 H93B 109.5 . . ?
C94 C93 H93C 109.5 . . ?
O6 C94 O7 118.6(14) . . ?
O6 C94 C93 122.0(16) . . ?
O7 C94 C93 119.5(15) . . ?
C93 C94 O7 126.6(19) 2_676 . ?
C93 C94 C93 103.0(15) 2_676 . ?
O7 C95 H95A 110.1 . . ?
O7 C95 H95B 110.1 . . ?
O7 C95 C96 107.8(12) . . ?
H95A C95 H95B 108.5 . . ?
C96 C95 H95A 110.1 . . ?
C96 C95 H95B 110.1 . . ?
C95 C96 H96A 109.5 . . ?
C95 C96 H96B 109.5 . . ?
C95 C96 H96C 109.5 . . ?
H96A C96 H96B 109.5 . . ?
H96A C96 H96C 109.5 . . ?
H96B C96 H96C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C31 C32 C33 -176.5(3) . . . . ?
N2 C31 C36 N1 -64.3(3) . . . . ?
N2 C31 C36 C35 174.9(3) . . . . ?
N3 C25 C26 C27 -175.9(3) . . . . ?
N3 C25 C30 N4 -64.1(3) . . . . ?
N3 C25 C30 C29 174.7(3) . . . . ?
N6 C37 C38 C39 -176.9(3) . . . . ?
N6 C37 C42 N5 -62.3(3) . . . . ?
N6 C37 C42 C41 176.2(2) . . . . ?
C1 C2 C3 C4 3.5(4) . . . . ?
C1 C2 C3 C8 -176.2(3) . . . . ?
C2 C1 C6 C5 0.2(4) . . . . ?
C2 C1 C7 N2 179.9(3) . . . . ?
C2 C3 C4 C5 -2.3(5) . . . . ?
C2 C3 C8 N3 4.6(5) . . . . ?
C3 C4 C5 C6 0.1(5) . . . . ?
C4 C3 C8 N3 -175.2(3) . . . . ?
C4 C5 C6 C1 1.0(5) . . . . ?
C6 C1 C2 C3 -2.5(4) . . . . ?
C6 C1 C7 N2 -0.9(5) . . . . ?
C7 N2 C31 C32 -121.8(3) . . . . ?
C7 N2 C31 C36 118.0(3) . . . . ?
C7 C1 C2 C3 176.7(3) . . . . ?
C7 C1 C6 C5 -179.0(3) . . . . ?
C8 N3 C25 C26 -111.5(3) . . . . ?
C8 N3 C25 C30 127.2(3) . . . . ?
C8 C3 C4 C5 177.4(3) . . . . ?
C9 C10 C11 C12 -1.7(5) . . . . ?
C9 C10 C11 C16 -180.0(3) . . . . ?
C10 C9 C14 C13 0.7(6) . . . . ?
C10 C9 C15 N1 -3.2(5) . . . . ?
C10 C11 C12 C13 1.2(7) . . . . ?
C10 C11 C16 N6 -179.4(3) . . . . ?
C11 C12 C13 C14 0.2(8) . . . . ?
C12 C11 C16 N6 2.4(5) . . . . ?
C12 C13 C14 C9 -1.1(8) . . . . ?
C14 C9 C10 C11 0.8(5) . . . . ?
C14 C9 C15 N1 176.2(4) . . . . ?
C15 N1 C36 C31 121.0(3) . . . . ?
C15 N1 C36 C35 -117.6(3) . . . . ?
C15 C9 C10 C11 -179.8(3) . . . . ?
C15 C9 C14 C13 -178.8(4) . . . . ?
C16 N6 C37 C38 -105.4(3) . . . . ?
C16 N6 C37 C42 133.1(3) . . . . ?
C16 C11 C12 C13 179.5(4) . . . . ?
C17 C18 C19 C20 0.3(5) . . . . ?
C17 C18 C19 C24 -177.4(3) . . . . ?
C18 C17 C22 C21 -1.1(6) . . . . ?
C18 C17 C23 N5 6.0(5) . . . . ?
C18 C19 C20 C21 -0.3(6) . . . . ?
C18 C19 C24 N4 -177.2(3) . . . . ?
C19 C20 C21 C22 -0.4(6) . . . . ?
C20 C19 C24 N4 5.2(6) . . . . ?
C20 C21 C22 C17 1.2(6) . . . . ?
C22 C17 C18 C19 0.4(5) . . . . ?
C22 C17 C23 N5 -175.3(4) . . . . ?
C23 N5 C42 C37 109.7(3) . . . . ?
C23 N5 C42 C41 -129.2(3) . . . . ?
C23 C17 C18 C19 179.1(3) . . . . ?
C23 C17 C22 C21 -179.9(4) . . . . ?
C24 N4 C30 C25 129.1(3) . . . . ?
C24 N4 C30 C29 -109.5(3) . . . . ?
C24 C19 C20 C21 177.3(4) . . . . ?
C25 N3 C8 C3 175.8(3) . . . . ?
C25 C26 C27 C28 56.1(4) . . . . ?
C26 C25 C30 N4 175.8(2) . . . . ?
C26 C25 C30 C29 54.6(3) . . . . ?
C26 C27 C28 C29 -56.8(4) . . . . ?
C27 C28 C29 C30 57.7(4) . . . . ?
C28 C29 C30 N4 -177.2(3) . . . . ?
C28 C29 C30 C25 -56.6(4) . . . . ?
C30 N4 C24 C19 -177.4(3) . . . . ?
C30 C25 C26 C27 -55.3(4) . . . . ?
C31 N2 C7 C1 175.9(3) . . . . ?
C31 C32 C33 C34 57.4(4) . . . . ?
C32 C31 C36 N1 176.5(2) . . . . ?
C32 C31 C36 C35 55.8(4) . . . . ?
C32 C33 C34 C35 -57.8(4) . . . . ?
C33 C34 C35 C36 58.8(4) . . . . ?
C34 C35 C36 N1 -179.0(3) . . . . ?
C34 C35 C36 C31 -57.7(4) . . . . ?
C36 N1 C15 C9 178.4(3) . . . . ?
C36 C31 C32 C33 -56.4(4) . . . . ?
C37 N6 C16 C11 179.4(3) . . . . ?
C37 C38 C39 C40 56.3(4) . . . . ?
C38 C37 C42 N5 177.4(2) . . . . ?
C38 C37 C42 C41 55.9(3) . . . . ?
C38 C39 C40 C41 -56.0(4) . . . . ?
C39 C40 C41 C42 56.4(4) . . . . ?
C40 C41 C42 N5 -176.8(3) . . . . ?
C40 C41 C42 C37 -56.4(3) . . . . ?
C42 N5 C23 C17 -178.4(3) . . . . ?
C42 C37 C38 C39 -56.7(4) . . . . ?
N7 C73 C74 C75 -178.8(3) . . . . ?
N7 C73 C78 N8 -61.7(3) . . . . ?
N7 C73 C78 C77 178.1(2) . . . . ?
N10 C79 C80 C81 -175.9(2) . . . . ?
N10 C79 C84 N9 -66.1(3) . . . . ?
N10 C79 C84 C83 173.8(2) . . . . ?
N11 C67 C68 C69 -174.6(3) . . . . ?
N11 C67 C72 N12 -65.0(3) . . . . ?
N11 C67 C72 C71 174.1(3) . . . . ?
C43 C44 C45 C46 1.1(4) . . . . ?
C43 C44 C45 C50 177.0(3) . . . . ?
C44 C43 C48 C47 0.4(5) . . . . ?
C44 C43 C49 N11 7.6(5) . . . . ?
C44 C45 C46 C47 -1.5(5) . . . . ?
C44 C45 C50 N10 176.9(3) . . . . ?
C45 C46 C47 C48 1.4(5) . . . . ?
C46 C45 C50 N10 -7.3(4) . . . . ?
C46 C47 C48 C43 -0.9(5) . . . . ?
C48 C43 C44 C45 -0.6(4) . . . . ?
C48 C43 C49 N11 -169.6(3) . . . . ?
C49 N11 C67 C68 -108.4(3) . . . . ?
C49 N11 C67 C72 130.6(3) . . . . ?
C49 C43 C44 C45 -177.8(3) . . . . ?
C49 C43 C48 C47 177.7(3) . . . . ?
C50 N10 C79 C80 -120.8(3) . . . . ?
C50 N10 C79 C84 119.5(3) . . . . ?
C50 C45 C46 C47 -177.4(3) . . . . ?
C51 C52 C53 C54 1.4(5) . . . . ?
C51 C52 C53 C58 -179.7(3) . . . . ?
C52 C51 C56 C55 0.2(5) . . . . ?
C52 C51 C57 N12 -172.8(3) . . . . ?
C52 C53 C54 C55 -0.4(5) . . . . ?
C52 C53 C58 N7 2.6(5) . . . . ?
C53 C54 C55 C56 -0.7(6) . . . . ?
C54 C53 C58 N7 -178.5(3) . . . . ?
C54 C55 C56 C51 0.8(6) . . . . ?
C56 C51 C52 C53 -1.3(5) . . . . ?
C56 C51 C57 N12 10.0(6) . . . . ?
C57 N12 C72 C67 128.4(3) . . . . ?
C57 N12 C72 C71 -110.4(3) . . . . ?
C57 C51 C52 C53 -178.6(3) . . . . ?
C57 C51 C56 C55 177.4(3) . . . . ?
C58 N7 C73 C74 -130.5(3) . . . . ?
C58 N7 C73 C78 108.6(3) . . . . ?
C58 C53 C54 C55 -179.3(3) . . . . ?
C59 C60 C61 C62 0.5(5) . . . . ?
C59 C60 C61 C66 179.6(3) . . . . ?
C60 C59 C64 C63 -0.1(5) . . . . ?
C60 C59 C65 N9 -1.3(5) . . . . ?
C60 C61 C62 C63 0.5(5) . . . . ?
C60 C61 C66 N8 -178.9(3) . . . . ?
C61 C62 C63 C64 -1.3(6) . . . . ?
C62 C61 C66 N8 0.2(5) . . . . ?
C62 C63 C64 C59 1.1(6) . . . . ?
C64 C59 C60 C61 -0.7(5) . . . . ?
C64 C59 C65 N9 180.0(3) . . . . ?
C65 N9 C84 C79 123.0(3) . . . . ?
C65 N9 C84 C83 -116.2(3) . . . . ?
C65 C59 C60 C61 -179.4(3) . . . . ?
C65 C59 C64 C63 178.6(3) . . . . ?
C66 N8 C78 C73 128.5(3) . . . . ?
C66 N8 C78 C77 -109.7(3) . . . . ?
C66 C61 C62 C63 -178.6(3) . . . . ?
C67 N11 C49 C43 175.7(3) . . . . ?
C67 C68 C69 C70 55.1(4) . . . . ?
C68 C67 C72 N12 175.7(3) . . . . ?
C68 C67 C72 C71 54.8(4) . . . . ?
C68 C69 C70 C71 -56.6(4) . . . . ?
C69 C70 C71 C72 58.3(4) . . . . ?
C70 C71 C72 N12 -176.8(3) . . . . ?
C70 C71 C72 C67 -57.0(4) . . . . ?
C72 N12 C57 C51 -177.4(3) . . . . ?
C72 C67 C68 C69 -54.4(4) . . . . ?
C73 N7 C58 C53 -177.5(3) . . . . ?
C73 C74 C75 C76 58.8(4) . . . . ?
C74 C73 C78 N8 177.1(2) . . . . ?
C74 C73 C78 C77 56.8(3) . . . . ?
C74 C75 C76 C77 -56.9(4) . . . . ?
C75 C76 C77 C78 54.9(4) . . . . ?
C76 C77 C78 N8 -175.8(3) . . . . ?
C76 C77 C78 C73 -55.6(3) . . . . ?
C78 N8 C66 C61 179.7(3) . . . . ?
C78 C73 C74 C75 -57.9(3) . . . . ?
C79 N10 C50 C45 173.9(3) . . . . ?
C79 C80 C81 C82 56.4(4) . . . . ?
C80 C79 C84 N9 175.8(2) . . . . ?
C80 C79 C84 C83 55.6(3) . . . . ?
C80 C81 C82 C83 -56.4(4) . . . . ?
C81 C82 C83 C84 58.4(4) . . . . ?
C82 C83 C84 N9 -179.2(2) . . . . ?
C82 C83 C84 C79 -58.2(3) . . . . ?
C84 N9 C65 C59 176.6(3) . . . . ?
C84 C79 C80 C81 -55.9(3) . . . . ?
C90 O2 C91 O1 -177.7(11) . . . . ?
C90 O2 C91 C92 25.1(17) . . . . ?
C91 O2 C90 C89 168.6(15) . . . . ?
C98 O8 C99 O9 -8.9(17) . . . . ?
C98 O8 C99 C100 -178.5(13) . . . . ?
C99 O8 C98 C97 174.7(11) . . . . ?
C85 O4 C86 O3 128(2) 2_667 . . . ?
C85 O4 C86 O4 -41(2) 2_667 . . 2_667 ?
C85 O4 C86 C85 -63(3) 2_667 . . . ?
C85 O4 C86 C86 -41(2) 2_667 . . 2_667 ?
C86 O3 C87 C88 -168.8(11) . . . . ?
C86 O4 C86 O3 169.8(14) 2_667 . . . ?
C86 O4 C86 O4 0.000(2) 2_667 . . 2_667 ?
C86 O4 C86 C85 -21.5(12) 2_667 . . . ?
C86 O4 C86 C85 41(2) 2_667 . . 2_667 ?
C87 O3 C86 O4 168.0(9) . . . 2_667 ?
C87 O3 C86 O4 -1.4(16) . . . . ?
C87 O3 C86 C85 -171.2(10) . . . . ?
C87 O3 C86 C85 33.0(19) . . . 2_667 ?
C87 O3 C86 C86 151(3) . . . 2_667 ?
C93 O6 C94 O7 -114(3) 2_676 . . . ?
C93 O6 C94 C93 66(3) 2_676 . . . ?
C93 O6 C94 C94 43(2) 2_676 . . 2_676 ?
C94 O7 C95 C96 180.0(2) . . . . ?
C95 O7 C94 O6 0.0(3) . . . . ?
C95 O7 C94 C93 179.90(18) . . . . ?
C95 O7 C94 C93 -42.2(18) . . . 2_676 ?
C95 O7 C94 C94 -131(3) . . . 2_676 ?

_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 1.228
_oxdiff_exptl_absorpt_empirical_full_min 0.805
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.5339(12) 18533 30995 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.4661(12) 18385 30995 nmt -1.0005 0.9734 -0.0004 0.0012 1.0007 -0.0008
0.0005 0.0129 -1.0010

_twin_special_details            
;
Component 2 rotated by -179.9854° 
around [0.44 0.90 0.01] (reciprocal) or [0.00 1.00 -0.00] (direct)
;
####################################################################### 
# 
# 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_MeOH_1-R_100K_publ
_database_code_depnum_ccdc_archive 'CCDC 2073635'
loop_
_audit_author_name
_audit_author_address
'Marc Little'
;University of Liverpool
United Kingdom
;
_audit_update_record             
;
2021-03-27 deposited with the CCDC.	2021-05-14 downloaded from the CCDC.
;
_audit_creation_date             2020-01-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H48 N6, 0.75(C H4 O)'
_chemical_formula_sum            'C42.75 H51 N6 O0.75'
_chemical_formula_weight         660.89
_chemical_absolute_configuration '-R,R diamine from synthesis'
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N6 O2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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      hexagonal
_space_group_IT_number           173
_space_group_name_H-M_alt        'P 63'
_space_group_name_Hall           'P 6c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'

_cell_length_a                   20.450(2)
_cell_length_b                   20.450(2)
_cell_length_c                   5.9423(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2152.2(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5593
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.4280
_cell_measurement_theta_min      1.9560
_shelx_estimated_absorpt_T_max   0.992
_shelx_estimated_absorpt_T_min   0.978
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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    1.020
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             711
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.362
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.135
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1107
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            19869
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        21.941
_diffrn_reflns_theta_max         21.941
_diffrn_reflns_theta_min         3.043
_diffrn_ambient_temperature      100
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  15.00   1.00   40.00    --  -20.00 -68.00   0.00  125
  2  ω   -100.00  25.00   1.00   70.00    --  -10.00 -68.00 120.00  125
  3  ω   -100.00  25.00   1.00   70.00    --  -10.00 -68.00 240.00  125
  4  ω   -100.00  25.00   1.00   70.00    --  -10.00 -30.00  90.00  125
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0325419000
_diffrn_orient_matrix_UB_12      -0.0358793000
_diffrn_orient_matrix_UB_13      0.0126702000
_diffrn_orient_matrix_UB_21      -0.0229270000
_diffrn_orient_matrix_UB_22      0.0145881000
_diffrn_orient_matrix_UB_23      -0.0410758000
_diffrn_orient_matrix_UB_31      0.0047379000
_diffrn_orient_matrix_UB_32      -0.0094552000
_diffrn_orient_matrix_UB_33      -0.1113483000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.777
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                1504
_reflns_number_total             1724
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.173
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 
;
 Flack x determined using 547 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   6.7(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         1724
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0646
_refine_ls_restrained_S_all      1.078
_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)+(0.0900P)²+0.9330P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1554
_refine_ls_wR_factor_ref         0.1637
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O2-C16
 1.43 with sigma of 0.01
 O1-C15
 1.43 with sigma of 0.01
3. Others
 Fixed Sof: O1(0.16667) H1A(0.16667) C15(0.16667) H15A(0.16667) H15B(0.16667)
 H15C(0.16667) O2(0.08333) H2(0.08333) C16(0.08333) H16B(0.08333) H16C(0.08333)
 H16A(0.08333)
 Fixed X: H16B(0.63521) H16C(0.64635) H16A(0.71844)
 Fixed Y: H16B(0.28156) H16C(0.36479) H16A(0.35365)
 Fixed Z: H16B(0.69215) H16C(0.69215) H16A(0.69215)
4.a Ternary CH refined with riding coordinates:
 C1(H1), C6(H6)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B)
4.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14)
4.d Tetrahedral OH refined with riding coordinates:
 O1(H1A), O2(H2)
4.e Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.4142(3) 0.2734(3) 0.5809(9) 0.0401(13) Uani 1 1 d . . . . .
N2 N 0.4048(3) 0.1263(3) 0.5311(8) 0.0436(13) Uani 1 1 d . . . . .
C1 C 0.3668(4) 0.1443(3) 0.7088(10) 0.0423(16) Uani 1 1 d . . . . .
H1 H 0.401690 0.166175 0.840226 0.051 Uiso 1 1 calc R . . . .
C2 C 0.2967(4) 0.0714(4) 0.7822(12) 0.0481(17) Uani 1 1 d . . . . .
H2A H 0.265089 0.046374 0.648408 0.058 Uiso 1 1 calc R . . . .
H2B H 0.312449 0.036822 0.847166 0.058 Uiso 1 1 calc R . . . .
C3 C 0.2501(4) 0.0848(3) 0.9533(11) 0.0480(16) Uani 1 1 d . . . . .
H3A H 0.279652 0.104836 1.093595 0.058 Uiso 1 1 calc R . . . .
H3B H 0.204147 0.036322 0.989269 0.058 Uiso 1 1 calc R . . . .
C4 C 0.2278(4) 0.1402(3) 0.8642(11) 0.0487(17) Uani 1 1 d . . . . .
H4A H 0.199290 0.149959 0.981125 0.058 Uiso 1 1 calc R . . . .
H4B H 0.194638 0.118252 0.731432 0.058 Uiso 1 1 calc R . . . .
C5 C 0.2978(3) 0.2143(3) 0.7981(11) 0.0424(15) Uani 1 1 d . . . . .
H5A H 0.328463 0.238555 0.933982 0.051 Uiso 1 1 calc R . . . .
H5B H 0.282095 0.248938 0.733418 0.051 Uiso 1 1 calc R . . . .
C6 C 0.3459(3) 0.2011(3) 0.6255(10) 0.0388(15) Uani 1 1 d . . . . .
H6 H 0.316559 0.182049 0.482590 0.047 Uiso 1 1 calc R . . . .
C7 C 0.4234(3) 0.3013(4) 0.3848(11) 0.0444(16) Uani 1 1 d . . . . .
H7 H 0.386640 0.273014 0.273370 0.053 Uiso 1 1 calc R . . . .
C8 C 0.4875(3) 0.3748(3) 0.3207(11) 0.0438(15) Uani 1 1 d . . . . .
C9 C 0.4873(4) 0.4056(4) 0.1123(10) 0.0492(17) Uani 1 1 d . . . . .
H9 H 0.447334 0.377369 0.009382 0.059 Uiso 1 1 calc R . . . .
C10 C 0.5444(3) 0.4765(3) 0.0536(12) 0.0463(16) Uani 1 1 d . . . . .
H10 H 0.542743 0.497456 -0.087477 0.056 Uiso 1 1 calc R . . . .
C11 C 0.6045(4) 0.5176(4) 0.1994(10) 0.0471(17) Uani 1 1 d . . . . .
H11 H 0.644153 0.566262 0.157980 0.056 Uiso 1 1 calc R . . . .
C12 C 0.6058(3) 0.4865(4) 0.4071(10) 0.0444(16) Uani 1 1 d . . . . .
C13 C 0.5475(4) 0.4155(4) 0.4660(11) 0.0447(16) Uani 1 1 d . . . . .
H13 H 0.548736 0.394447 0.607383 0.054 Uiso 1 1 calc R . . . .
C14 C 0.6680(3) 0.5298(4) 0.5678(10) 0.0439(16) Uani 1 1 d . . . . .
H14 H 0.667293 0.506666 0.707065 0.053 Uiso 1 1 calc R . . . .
O1 O 0.000000 0.000000 0.190(8) 0.173(13) Uiso 0.5 3 d DS T P . .
H1A H 0.021351 -0.023351 0.142589 0.259 Uiso 0.1667 1 calc R . . . .
C15 C 0.000000 0.000000 0.429(8) 0.140(15) Uiso 0.5 3 d DS T P . .
H15A H -0.043265 0.003615 0.483683 0.210 Uiso 0.1667 1 calc GR . . A -1
H15B H 0.046880 0.043265 0.483684 0.210 Uiso 0.1667 1 calc GR . . A -1
H15C H -0.003615 -0.046879 0.483683 0.210 Uiso 0.1667 1 calc GR . . A -1
O2 O 0.666667 0.333333 0.376(16) 0.20(3) Uiso 0.25 3 d DS T P . .
H2 H 0.648911 0.359998 0.329289 0.305 Uiso 0.0833 1 calc R . . . .
C16 C 0.666667 0.333333 0.617(16) 0.18(4) Uiso 0.25 3 d DS T P . .
H16B H 0.635210 0.281560 0.692150 0.264 Uiso 0.0833 1 d R . . B -1
H16C H 0.646350 0.364790 0.692150 0.264 Uiso 0.0833 1 d R . . C -1
H16A H 0.718440 0.353650 0.692150 0.264 Uiso 0.0833 1 d R . . D -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C6 1.463(7) . ?
N1 C7 1.269(8) . ?
N2 C1 1.463(7) . ?
N2 C14 1.253(7) 2_655 ?
C1 C2 1.527(9) . ?
C1 C6 1.508(8) . ?
C2 C3 1.509(9) . ?
C3 C4 1.513(9) . ?
C4 C5 1.527(9) . ?
C5 C6 1.535(8) . ?
C7 C8 1.468(9) . ?
C8 C9 1.390(9) . ?
C8 C13 1.387(9) . ?
C9 C10 1.376(9) . ?
C10 C11 1.391(9) . ?
C11 C12 1.395(8) . ?
C12 C13 1.386(9) . ?
C12 C14 1.479(9) . ?
O1 C15 1.420(14) . ?
O2 C16 1.430(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7 N1 C6 118.2(5) . . ?
C14 N2 C1 118.4(5) 2_655 . ?
N2 C1 C2 108.5(5) . . ?
N2 C1 C6 110.3(5) . . ?
C6 C1 C2 110.9(5) . . ?
C3 C2 C1 112.6(5) . . ?
C2 C3 C4 110.7(5) . . ?
C3 C4 C5 110.5(5) . . ?
C4 C5 C6 111.3(5) . . ?
N1 C6 C1 110.0(5) . . ?
N1 C6 C5 108.4(5) . . ?
C1 C6 C5 111.7(5) . . ?
N1 C7 C8 123.6(5) . . ?
C9 C8 C7 119.4(6) . . ?
C13 C8 C7 121.5(6) . . ?
C13 C8 C9 119.1(6) . . ?
C10 C9 C8 120.6(6) . . ?
C9 C10 C11 120.5(6) . . ?
C10 C11 C12 119.2(6) . . ?
C11 C12 C14 120.3(6) . . ?
C13 C12 C11 119.9(6) . . ?
C13 C12 C14 119.7(6) . . ?
C12 C13 C8 120.7(6) . . ?
N2 C14 C12 123.9(6) 3_665 . ?

_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 1.398
_oxdiff_exptl_absorpt_empirical_full_min 0.650
####################################################################### 
# 
# 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_1pX_1-rac_100K_publ
_database_code_depnum_ccdc_archive 'CCDC 2073634'
loop_
_audit_author_name
_audit_author_address
'Marc Little'
;University of Liverpool
United Kingdom
;
_audit_update_record             
;
2021-03-27 deposited with the CCDC.	2021-05-14 downloaded from the CCDC.
;
_audit_creation_date             2019-09-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H48 N6, 2(0.5(C8 H10))'
_chemical_formula_sum            'C50 H58 N6'
_chemical_formula_weight         743.02
_chemical_melting_point          ?
_chemical_oxdiff_formula         C42H48N6
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 '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                   25.2103(4)
_cell_length_b                   14.0669(2)
_cell_length_c                   25.3934(4)
_cell_angle_alpha                90
_cell_angle_beta                 102.506(2)
_cell_angle_gamma                90
_cell_volume                     8791.6(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    31055
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.7840
_cell_measurement_theta_min      2.1380
_shelx_estimated_absorpt_T_max   0.994
_shelx_estimated_absorpt_T_min   0.965
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
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    1.123
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3200
_exptl_crystal_size_max          0.537
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.088
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            70247
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.075
_diffrn_reflns_theta_min         1.778
_diffrn_ambient_temperature      100
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  15.00   1.00    5.00    --  -20.00 -68.00   0.00  125
  2  ω   -110.00  15.00   1.00    5.00    --  -20.00 -68.00 120.00  125
  3  ω   -110.00  15.00   1.00    5.00    --  -20.00 -68.00 240.00  125
  4  ω   -110.00  15.00   1.00    5.00    --  -20.00 -30.00  90.00  125
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0046428000
_diffrn_orient_matrix_UB_12      0.0445487000
_diffrn_orient_matrix_UB_13      0.0112939000
_diffrn_orient_matrix_UB_21      0.0282405000
_diffrn_orient_matrix_UB_22      0.0045088000
_diffrn_orient_matrix_UB_23      0.0110644000
_diffrn_orient_matrix_UB_31      0.0034186000
_diffrn_orient_matrix_UB_32      0.0231797000
_diffrn_orient_matrix_UB_33      -0.0238428000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11060
_reflns_number_total             15555
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         15555
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0637
_refine_ls_restrained_S_all      1.015
_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)+(0.0659P)²+5.3816P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1397
_refine_ls_wR_factor_ref         0.1559
_refine_special_details          ?
_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 Ternary CH refined with riding coordinates:
 C9(H9), C14(H14), C23(H23), C28(H28), C37(H37), C42(H42)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C24(H24A,
 H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C38(H38A,H38B),
 C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C15(H15), C17(H17), C19(H19),
 C20(H20), C21(H21), C22(H22), C29(H29), C31(H31), C32(H32), C33(H33), C35(H35),
  C36(H36), C43(H43), C45(H45), C47(H47), C49(H49)
2.d Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C50(H50A,H50B,H50C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.82086(4) 0.61357(8) 0.67837(4) 0.0212(2) Uani 1 1 d . . . . .
N2 N 0.78695(4) 0.79334(8) 0.72011(4) 0.0200(2) Uani 1 1 d . . . . .
N3 N 0.61690(4) 1.01096(7) 0.53224(4) 0.0207(2) Uani 1 1 d . . . . .
N4 N 0.55110(4) 0.93007(7) 0.43289(4) 0.0211(2) Uani 1 1 d . . . . .
N5 N 0.62597(4) 0.51830(7) 0.37051(4) 0.0203(2) Uani 1 1 d . . . . .
N6 N 0.69758(4) 0.41298(7) 0.45344(4) 0.0205(2) Uani 1 1 d . . . . .
C1 C 0.72235(5) 0.45375(9) 0.54701(5) 0.0221(2) Uani 1 1 d . . . . .
C2 C 0.75641(5) 0.50530(9) 0.58756(5) 0.0204(2) Uani 1 1 d . . . . .
H2 H 0.785465 0.541293 0.579340 0.025 Uiso 1 1 calc R . . . .
C3 C 0.74816(5) 0.50447(10) 0.64039(5) 0.0230(2) Uani 1 1 d . . . . .
C4 C 0.70546(6) 0.45156(13) 0.65200(6) 0.0389(4) Uani 1 1 d . . . . .
H4 H 0.699661 0.450515 0.687733 0.047 Uiso 1 1 calc R . . . .
C5 C 0.67120(7) 0.40015(15) 0.61160(6) 0.0511(5) Uani 1 1 d . . . . .
H5 H 0.641973 0.364584 0.619772 0.061 Uiso 1 1 calc R . . . .
C6 C 0.67964(6) 0.40078(12) 0.55960(6) 0.0373(4) Uani 1 1 d . . . . .
H6 H 0.656364 0.365118 0.532229 0.045 Uiso 1 1 calc R . . . .
C7 C 0.72936(5) 0.45773(9) 0.49097(5) 0.0210(2) Uani 1 1 d . . . . .
H7 H 0.758151 0.494391 0.482719 0.025 Uiso 1 1 calc R . . . .
C8 C 0.78242(5) 0.55932(9) 0.68455(5) 0.0215(2) Uani 1 1 d . . . . .
H8 H 0.775294 0.553684 0.719654 0.026 Uiso 1 1 calc R . . . .
C9 C 0.85105(5) 0.66039(9) 0.72727(5) 0.0189(2) Uani 1 1 d . . . . .
H9 H 0.836981 0.637588 0.758961 0.023 Uiso 1 1 calc R . . . .
C10 C 0.91131(5) 0.63461(10) 0.73550(5) 0.0232(2) Uani 1 1 d . . . . .
H10A H 0.915602 0.564801 0.739129 0.028 Uiso 1 1 calc R . . . .
H10B H 0.925036 0.654746 0.703545 0.028 Uiso 1 1 calc R . . . .
C11 C 0.94464(5) 0.68277(10) 0.78586(5) 0.0251(3) Uani 1 1 d . . . . .
H11A H 0.932146 0.660468 0.818116 0.030 Uiso 1 1 calc R . . . .
H11B H 0.983414 0.665457 0.790274 0.030 Uiso 1 1 calc R . . . .
C12 C 0.93835(5) 0.79036(10) 0.78096(6) 0.0260(3) Uani 1 1 d . . . . .
H12A H 0.953522 0.813240 0.750413 0.031 Uiso 1 1 calc R . . . .
H12B H 0.958814 0.820936 0.814337 0.031 Uiso 1 1 calc R . . . .
C13 C 0.87846(5) 0.81770(9) 0.77180(5) 0.0223(2) Uani 1 1 d . . . . .
H13A H 0.874942 0.887436 0.767057 0.027 Uiso 1 1 calc R . . . .
H13B H 0.864548 0.800342 0.804104 0.027 Uiso 1 1 calc R . . . .
C14 C 0.84384(5) 0.76848(9) 0.72227(5) 0.0192(2) Uani 1 1 d . . . . .
H14 H 0.854766 0.791291 0.688852 0.023 Uiso 1 1 calc R . . . .
C15 C 0.76233(5) 0.84087(8) 0.67958(5) 0.0187(2) Uani 1 1 d . . . . .
H15 H 0.780636 0.854930 0.651519 0.022 Uiso 1 1 calc R . . . .
C16 C 0.70589(5) 0.87499(8) 0.67484(5) 0.0187(2) Uani 1 1 d . . . . .
C17 C 0.67743(5) 0.91381(8) 0.62660(5) 0.0193(2) Uani 1 1 d . . . . .
H17 H 0.693725 0.915666 0.596211 0.023 Uiso 1 1 calc R . . . .
C18 C 0.62493(5) 0.95022(8) 0.62237(5) 0.0200(2) Uani 1 1 d . . . . .
C19 C 0.60115(5) 0.94551(9) 0.66718(5) 0.0239(3) Uani 1 1 d . . . . .
H19 H 0.565511 0.969649 0.664755 0.029 Uiso 1 1 calc R . . . .
C20 C 0.62936(5) 0.90567(10) 0.71534(5) 0.0251(3) Uani 1 1 d . . . . .
H20 H 0.612724 0.901974 0.745461 0.030 Uiso 1 1 calc R . . . .
C21 C 0.68160(5) 0.87142(9) 0.71947(5) 0.0215(2) Uani 1 1 d . . . . .
H21 H 0.700993 0.845464 0.752618 0.026 Uiso 1 1 calc R . . . .
C22 C 0.59559(5) 0.99786(8) 0.57270(5) 0.0199(2) Uani 1 1 d . . . . .
H22 H 0.559536 1.019447 0.570922 0.024 Uiso 1 1 calc R . . . .
C23 C 0.58602(5) 1.06815(8) 0.48784(5) 0.0187(2) Uani 1 1 d . . . . .
H23 H 0.548362 1.078391 0.493404 0.022 Uiso 1 1 calc R . . . .
C24 C 0.61493(5) 1.16419(9) 0.48887(5) 0.0237(3) Uani 1 1 d . . . . .
H24A H 0.613755 1.197473 0.522948 0.028 Uiso 1 1 calc R . . . .
H24B H 0.653540 1.153175 0.488106 0.028 Uiso 1 1 calc R . . . .
C25 C 0.58908(6) 1.22752(9) 0.44121(6) 0.0283(3) Uani 1 1 d . . . . .
H25A H 0.551667 1.244601 0.443910 0.034 Uiso 1 1 calc R . . . .
H25B H 0.610322 1.286947 0.442243 0.034 Uiso 1 1 calc R . . . .
C26 C 0.58760(6) 1.17581(10) 0.38812(6) 0.0311(3) Uani 1 1 d . . . . .
H26A H 0.625171 1.163551 0.384034 0.037 Uiso 1 1 calc R . . . .
H26B H 0.569386 1.216310 0.357650 0.037 Uiso 1 1 calc R . . . .
C27 C 0.55709(6) 1.08165(10) 0.38675(5) 0.0265(3) Uani 1 1 d . . . . .
H27A H 0.557003 1.048657 0.352292 0.032 Uiso 1 1 calc R . . . .
H27B H 0.518889 1.094439 0.388488 0.032 Uiso 1 1 calc R . . . .
C28 C 0.58329(5) 1.01718(9) 0.43392(5) 0.0204(2) Uani 1 1 d . . . . .
H28 H 0.620905 1.000157 0.430486 0.024 Uiso 1 1 calc R . . . .
C29 C 0.57090(5) 0.85510(9) 0.41695(5) 0.0209(2) Uani 1 1 d . . . . .
H29 H 0.603886 0.859942 0.404798 0.025 Uiso 1 1 calc R . . . .
C30 C 0.54509(5) 0.76074(9) 0.41641(5) 0.0199(2) Uani 1 1 d . . . . .
C31 C 0.49976(5) 0.74469(9) 0.43898(6) 0.0250(3) Uani 1 1 d . . . . .
H31 H 0.482300 0.796595 0.452153 0.030 Uiso 1 1 calc R . . . .
C32 C 0.48050(5) 0.65321(10) 0.44202(6) 0.0290(3) Uani 1 1 d . . . . .
H32 H 0.449495 0.642684 0.456860 0.035 Uiso 1 1 calc R . . . .
C33 C 0.50625(5) 0.57629(9) 0.42349(6) 0.0256(3) Uani 1 1 d . . . . .
H33 H 0.493085 0.513664 0.426419 0.031 Uiso 1 1 calc R . . . .
C34 C 0.55104(5) 0.59072(9) 0.40076(5) 0.0207(2) Uani 1 1 d . . . . .
C35 C 0.56942(5) 0.68377(9) 0.39656(5) 0.0210(2) Uani 1 1 d . . . . .
H35 H 0.599120 0.694577 0.379801 0.025 Uiso 1 1 calc R . . . .
C36 C 0.58113(5) 0.50900(9) 0.38507(5) 0.0199(2) Uani 1 1 d . . . . .
H36 H 0.566321 0.447054 0.385906 0.024 Uiso 1 1 calc R . . . .
C37 C 0.65285(5) 0.43101(8) 0.35855(5) 0.0185(2) Uani 1 1 d . . . . .
H37 H 0.629248 0.375329 0.362193 0.022 Uiso 1 1 calc R . . . .
C38 C 0.66188(5) 0.43414(9) 0.30094(5) 0.0226(2) Uani 1 1 d . . . . .
H38A H 0.626435 0.440087 0.275194 0.027 Uiso 1 1 calc R . . . .
H38B H 0.684091 0.490479 0.296618 0.027 Uiso 1 1 calc R . . . .
C39 C 0.69070(5) 0.34419(10) 0.28837(5) 0.0254(3) Uani 1 1 d . . . . .
H39A H 0.697007 0.348198 0.251291 0.031 Uiso 1 1 calc R . . . .
H39B H 0.667305 0.288287 0.290204 0.031 Uiso 1 1 calc R . . . .
C40 C 0.74497(6) 0.33155(11) 0.32834(6) 0.0299(3) Uani 1 1 d . . . . .
H40A H 0.769711 0.384169 0.323909 0.036 Uiso 1 1 calc R . . . .
H40B H 0.761961 0.271101 0.320706 0.036 Uiso 1 1 calc R . . . .
C41 C 0.73704(5) 0.33057(10) 0.38639(5) 0.0263(3) Uani 1 1 d . . . . .
H41A H 0.772920 0.326321 0.411568 0.032 Uiso 1 1 calc R . . . .
H41B H 0.715708 0.273737 0.391873 0.032 Uiso 1 1 calc R . . . .
C42 C 0.70747(5) 0.42032(9) 0.39909(5) 0.0193(2) Uani 1 1 d . . . . .
H42 H 0.730587 0.477314 0.396850 0.023 Uiso 1 1 calc R . . . .
C43 C 0.74428(7) 0.74472(13) 0.55247(7) 0.0419(4) Uani 1 1 d . . . . .
H43 H 0.741567 0.740743 0.589136 0.050 Uiso 1 1 calc R . . . .
C44 C 0.70305(6) 0.70854(11) 0.51308(7) 0.0364(3) Uani 1 1 d . . . . .
C45 C 0.71014(7) 0.71300(15) 0.46007(7) 0.0496(5) Uani 1 1 d . . . . .
H45 H 0.683163 0.686502 0.431897 0.060 Uiso 1 1 calc R . . . .
C46 C 0.65297(7) 0.66694(15) 0.52716(8) 0.0496(4) Uani 1 1 d . . . . .
H46A H 0.661576 0.645018 0.564683 0.074 Uiso 1 1 calc GR . . . .
H46B H 0.640197 0.613152 0.503247 0.074 Uiso 1 1 calc GR . . . .
H46C H 0.624498 0.715542 0.522742 0.074 Uiso 1 1 calc GR . . . .
C47 C 0.48520(9) 0.43454(14) 0.26997(11) 0.0844(11) Uani 1 1 d . . . . .
H47 H 0.475210 0.493472 0.283317 0.101 Uiso 1 1 calc R . . . .
C48 C 0.46968(9) 0.34997(15) 0.29113(12) 0.0714(8) Uani 1 1 d . . . . .
C49 C 0.48519(8) 0.26593(14) 0.26970(10) 0.0677(7) Uani 1 1 d . . . . .
H49 H 0.474963 0.206892 0.282738 0.081 Uiso 1 1 calc R . . . .
C50 C 0.43755(12) 0.3491(2) 0.33447(13) 0.0946(10) Uani 1 1 d . . . . .
H50A H 0.460874 0.328161 0.368524 0.142 Uiso 1 1 calc GR . . . .
H50B H 0.406787 0.305344 0.324281 0.142 Uiso 1 1 calc GR . . . .
H50C H 0.423999 0.413272 0.338885 0.142 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C8 1.2697(16) . ?
N1 C9 1.4648(15) . ?
N2 C14 1.4657(14) . ?
N2 C15 1.2706(15) . ?
N3 C22 1.2718(16) . ?
N3 C23 1.4642(15) . ?
N4 C28 1.4669(16) . ?
N4 C29 1.2699(16) . ?
N5 C36 1.2700(16) . ?
N5 C37 1.4657(15) . ?
N6 C7 1.2711(16) . ?
N6 C42 1.4582(15) . ?
C1 C2 1.3931(17) . ?
C1 C6 1.4021(18) . ?
C1 C7 1.4726(17) . ?
C2 C3 1.4015(17) . ?
C3 C4 1.3917(18) . ?
C3 C8 1.4762(17) . ?
C4 C5 1.392(2) . ?
C5 C6 1.382(2) . ?
C9 C10 1.5316(16) . ?
C9 C14 1.5334(18) . ?
C10 C11 1.5280(18) . ?
C11 C12 1.524(2) . ?
C12 C13 1.5264(17) . ?
C13 C14 1.5322(17) . ?
C15 C16 1.4815(16) . ?
C16 C17 1.3904(17) . ?
C16 C21 1.4009(17) . ?
C17 C18 1.4013(16) . ?
C18 C19 1.3978(18) . ?
C18 C22 1.4775(17) . ?
C19 C20 1.3926(18) . ?
C20 C21 1.3848(17) . ?
C23 C24 1.5325(17) . ?
C23 C28 1.5338(18) . ?
C24 C25 1.5301(18) . ?
C25 C26 1.525(2) . ?
C26 C27 1.5283(18) . ?
C27 C28 1.5334(18) . ?
C29 C30 1.4770(17) . ?
C30 C31 1.4034(17) . ?
C30 C35 1.3916(17) . ?
C31 C32 1.3834(19) . ?
C32 C33 1.3949(18) . ?
C33 C34 1.3897(18) . ?
C34 C35 1.4004(17) . ?
C34 C36 1.4789(17) . ?
C37 C38 1.5290(17) . ?
C37 C42 1.5377(17) . ?
C38 C39 1.5268(18) . ?
C39 C40 1.527(2) . ?
C40 C41 1.5299(19) . ?
C41 C42 1.5356(17) . ?
C43 C44 1.375(2) . ?
C43 C45 1.391(3) 7_666 ?
C44 C45 1.397(2) . ?
C44 C46 1.503(2) . ?
C47 C47 1.383(6) 2_655 ?
C47 C48 1.396(3) . ?
C48 C49 1.392(3) . ?
C48 C50 1.501(4) . ?
C49 C49 1.372(5) 2_655 ?

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
C8 N1 C9 115.83(10) . . ?
C15 N2 C14 117.27(10) . . ?
C22 N3 C23 117.03(10) . . ?
C29 N4 C28 116.44(10) . . ?
C36 N5 C37 117.04(10) . . ?
C7 N6 C42 117.73(10) . . ?
C2 C1 C6 119.28(12) . . ?
C2 C1 C7 120.71(11) . . ?
C6 C1 C7 119.96(11) . . ?
C1 C2 C3 120.51(11) . . ?
C2 C3 C8 122.62(11) . . ?
C4 C3 C2 119.28(12) . . ?
C4 C3 C8 118.09(11) . . ?
C3 C4 C5 120.45(13) . . ?
C6 C5 C4 120.09(13) . . ?
C5 C6 C1 120.40(13) . . ?
N6 C7 C1 121.18(11) . . ?
N1 C8 C3 123.84(11) . . ?
N1 C9 C10 109.10(10) . . ?
N1 C9 C14 110.19(10) . . ?
C10 C9 C14 110.03(10) . . ?
C11 C10 C9 111.02(10) . . ?
C12 C11 C10 110.08(11) . . ?
C11 C12 C13 110.16(11) . . ?
C12 C13 C14 112.34(10) . . ?
N2 C14 C9 109.71(9) . . ?
N2 C14 C13 107.56(10) . . ?
C13 C14 C9 110.11(10) . . ?
N2 C15 C16 121.89(11) . . ?
C17 C16 C15 120.15(11) . . ?
C17 C16 C21 119.62(11) . . ?
C21 C16 C15 120.20(11) . . ?
C16 C17 C18 120.66(11) . . ?
C17 C18 C22 121.42(11) . . ?
C19 C18 C17 118.98(11) . . ?
C19 C18 C22 119.52(11) . . ?
C20 C19 C18 120.44(11) . . ?
C21 C20 C19 120.20(12) . . ?
C20 C21 C16 120.09(12) . . ?
N3 C22 C18 122.30(11) . . ?
N3 C23 C24 107.43(10) . . ?
N3 C23 C28 110.13(10) . . ?
C24 C23 C28 110.88(10) . . ?
C25 C24 C23 112.35(10) . . ?
C26 C25 C24 110.25(11) . . ?
C25 C26 C27 110.44(11) . . ?
C26 C27 C28 111.42(11) . . ?
N4 C28 C23 108.91(10) . . ?
N4 C28 C27 109.69(10) . . ?
C27 C28 C23 110.45(10) . . ?
N4 C29 C30 123.13(11) . . ?
C31 C30 C29 122.47(11) . . ?
C35 C30 C29 118.34(11) . . ?
C35 C30 C31 118.99(11) . . ?
C32 C31 C30 119.94(12) . . ?
C31 C32 C33 120.54(12) . . ?
C34 C33 C32 120.40(12) . . ?
C33 C34 C35 118.71(11) . . ?
C33 C34 C36 120.58(11) . . ?
C35 C34 C36 120.56(11) . . ?
C30 C35 C34 121.36(11) . . ?
N5 C36 C34 122.64(11) . . ?
N5 C37 C38 110.21(10) . . ?
N5 C37 C42 109.29(9) . . ?
C38 C37 C42 110.25(10) . . ?
C39 C38 C37 110.63(10) . . ?
C38 C39 C40 110.85(10) . . ?
C39 C40 C41 110.87(11) . . ?
C40 C41 C42 111.45(11) . . ?
N6 C42 C37 109.19(9) . . ?
N6 C42 C41 109.32(10) . . ?
C41 C42 C37 110.17(10) . . ?
C44 C43 C45 121.60(16) . 7_666 ?
C43 C44 C45 116.75(16) . . ?
C43 C44 C46 120.84(16) . . ?
C45 C44 C46 122.41(15) . . ?
C43 C45 C44 121.61(15) 7_666 . ?
C47 C47 C48 121.54(17) 2_655 . ?
C47 C48 C50 122.0(2) . . ?
C49 C48 C47 116.6(3) . . ?
C49 C48 C50 121.4(2) . . ?
C49 C49 C48 121.89(17) 2_655 . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.490
_oxdiff_exptl_absorpt_empirical_full_min 0.767
####################################################################### 
# 
# 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_3mX_2_1-rac_100K_publ
_database_code_depnum_ccdc_archive 'CCDC 2073637'
loop_
_audit_author_name
_audit_author_address
'Marc Little'
;University of Liverpool
United Kingdom
;
_audit_update_record             
;
2021-03-27 deposited with the CCDC.	2021-05-14 downloaded from the CCDC.
;
_audit_creation_date             2019-09-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C42 H48 N6), 3(C8 H10), 0.1(H2 O)'
_chemical_formula_sum            'C108 H126.20 N12 O0.10'
_chemical_formula_weight         1594.00
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   29.9687(5)
_cell_length_b                   22.3149(3)
_cell_length_c                   14.6297(2)
_cell_angle_alpha                90
_cell_angle_beta                 103.221(2)
_cell_angle_gamma                90
_cell_volume                     9524.3(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    41292
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.6900
_cell_measurement_theta_min      1.9550
_shelx_estimated_absorpt_T_max   0.994
_shelx_estimated_absorpt_T_min   0.971
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86472
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
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    1.112
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3436
_exptl_crystal_size_max          0.448
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.095
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0762
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            133758
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.390
_diffrn_reflns_theta_min         1.825
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  15.00   1.00   20.00    --  -20.00 -68.00   0.00  125
  2  ω   -110.00  15.00   1.00   20.00    --  -20.00 -68.00 120.00  125
  3  ω   -110.00  15.00   1.00   20.00    --  -20.00 -68.00 240.00  125
  4  ω   -110.00  15.00   1.00   20.00    --  -20.00 -30.00  90.00  125
  5  ω   -110.00  15.00   1.00   20.00    --  -20.00 -30.00 210.00  125
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0242852000
_diffrn_orient_matrix_UB_12      -0.0017650000
_diffrn_orient_matrix_UB_13      -0.0113041000
_diffrn_orient_matrix_UB_21      -0.0010336000
_diffrn_orient_matrix_UB_22      0.0238494000
_diffrn_orient_matrix_UB_23      -0.0324595000
_diffrn_orient_matrix_UB_31      0.0008614000
_diffrn_orient_matrix_UB_32      -0.0209375000
_diffrn_orient_matrix_UB_33      -0.0360160000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                13778
_reflns_number_total             19494
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.198
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1147
_refine_ls_number_reflns         19494
_refine_ls_number_restraints     160
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0668
_refine_ls_restrained_S_all      1.071
_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)+(0.0434P)²+7.2918P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1481
_refine_special_details          ?
_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
 C102-C101 = C115-C114 = C116-C110 = C108-C104
 1.49 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C101) \\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(C107) \\sim Ueq,
Uanis(C103) \\sim Ueq, Uanis(C104) \\sim Ueq, Uanis(C105) \\sim Ueq,
Uanis(C106) \\sim Ueq, Uanis(C108) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C101, C108, C104, C105, C103, C106, C102, C107
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C115, C114, C109, C113, C110, C112, C111, C116
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C108)=Sof(H10C)=Sof(H10D)=Sof(H10E)=Sof(C102)=Sof(C107)=Sof(H107)=
 Sof(C106)=Sof(H106)=Sof(C105)=Sof(H105)=Sof(C104)=Sof(C103)=Sof(H103)=
 Sof(C101)=Sof(H10F)=Sof(H10G)=Sof(H10H)=1-FVAR(1)
 Sof(C114)=Sof(C109)=Sof(H109)=Sof(C110)=Sof(C111)=Sof(H111)=Sof(C112)=
 Sof(H112)=Sof(C113)=Sof(H113)=Sof(C115)=Sof(H11C)=Sof(H11D)=Sof(H11E)=
 Sof(C116)=Sof(H11F)=Sof(H11G)=Sof(H11H)=FVAR(1)
 Fixed Sof: O1(0.1)
6.a Ternary CH refined with riding coordinates:
 C43(H43), C37(H37), C48(H48), C42(H42), C62(H62), C75(H75), C14(H14), C9(H9),
 C57(H57), C28(H28), C71(H71), C23(H23)
6.b Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B), C41(H41A,H41B), C44(H44A,H44B), C39(H39A,H39B), C45(H45A,
 H45B), C38(H38A,H38B), C46(H46A,H46B), C40(H40A,H40B), C13(H13A,H13B),
 C61(H61A,H61B), C76(H76A,H76B), C27(H27A,H27B), C10(H10A,H10B), C12(H12A,H12B),
  C58(H58A,H58B), C11(H11A,H11B), C74(H74A,H74B), C60(H60A,H60B), C24(H24A,
 H24B), C72(H72A,H72B), C26(H26A,H26B), C59(H59A,H59B), C73(H73A,H73B),
 C25(H25A,H25B)
6.c Aromatic/amide H refined with riding coordinates:
 C84(H84), C29(H29), C81(H81), C36(H36), C31(H31), C79(H79), C33(H33), C2(H2),
 C83(H83), C35(H35), C7(H7), C77(H77), C15(H15), C8(H8), C17(H17), C4(H4),
 C82(H82), C63(H63), C56(H56), C55(H55), C51(H51), C70(H70), C49(H49), C5(H5),
 C21(H21), C34(H34), C53(H53), C52(H52), C6(H6), C20(H20), C95(H95), C22(H22),
 C19(H19), C65(H65), C98(H98), C69(H69), C68(H68), C87(H87), C67(H67),
 C100(H100), C99(H99), C89(H89), C91(H91), C90(H90), C109(H109), C111(H111),
 C112(H112), C113(H113), C107(H107), C106(H106), C105(H105), C103(H103)
6.d Fitted hexagon refined as free rotating group:
 C114(C109,C110,C111,C112,C113), C102(C107,C106,C105,C104,C103)
6.e Idealised Me refined as rotating group:
 C97(H97A,H97B,H97C), C92(H92A,H92B,H92C), C93(H93A,H93B,H93C), C85(H85A,H85B,
 H85C), C115(H11C,H11D,H11E), C116(H11F,H11G,H11H), C108(H10C,H10D,H10E),
 C101(H10F,H10G,H10H)
;
_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
N7 N 0.89992(6) 0.40192(8) 0.96365(12) 0.0284(4) Uani 1 1 d . . . . .
N8 N 0.93108(6) 0.33474(8) 0.81756(12) 0.0283(4) Uani 1 1 d . . . . .
N6 N 0.59977(6) 0.60073(8) 1.04678(12) 0.0283(4) Uani 1 1 d . . . . .
N5 N 0.56873(6) 0.67189(8) 0.87411(12) 0.0292(4) Uani 1 1 d . . . . .
N9 N 0.87990(7) 0.45501(8) 0.40311(13) 0.0315(4) Uani 1 1 d . . . . .
N2 N 0.69411(6) 0.28345(8) 0.93066(13) 0.0311(4) Uani 1 1 d . . . . .
N11 N 0.80871(6) 0.71798(8) 0.72735(13) 0.0290(4) Uani 1 1 d . . . . .
N4 N 0.61628(7) 0.53997(8) 0.51438(12) 0.0302(4) Uani 1 1 d . . . . .
N1 N 0.67437(7) 0.32927(8) 1.10211(13) 0.0321(4) Uani 1 1 d . . . . .
N3 N 0.63640(7) 0.41255(8) 0.52256(13) 0.0324(4) Uani 1 1 d . . . . .
N12 N 0.82815(7) 0.67457(8) 0.91932(13) 0.0337(5) Uani 1 1 d . . . . .
N10 N 0.86133(7) 0.58094(9) 0.37617(13) 0.0363(5) Uani 1 1 d . . . . .
C32 C 0.55617(8) 0.62167(9) 0.72373(15) 0.0270(5) Uani 1 1 d . . . . .
C84 C 0.91409(8) 0.36020(9) 0.73995(15) 0.0261(5) Uani 1 1 d . . . . .
H84 H 0.881717 0.364278 0.721448 0.031 Uiso 1 1 calc R . . . .
C30 C 0.55145(8) 0.57261(9) 0.57385(14) 0.0269(5) Uani 1 1 d . . . . .
C80 C 0.94187(8) 0.38386(9) 0.67679(14) 0.0256(5) Uani 1 1 d . . . . .
C78 C 0.94539(8) 0.42925(9) 0.52787(15) 0.0264(5) Uani 1 1 d . . . . .
C3 C 0.62403(8) 0.41349(10) 1.09635(14) 0.0278(5) Uani 1 1 d . . . . .
C29 C 0.57346(8) 0.54308(9) 0.50516(14) 0.0273(5) Uani 1 1 d . . . . .
H29 H 0.554311 0.525473 0.451058 0.033 Uiso 1 1 calc R . . . .
C81 C 0.98975(8) 0.38164(10) 0.70109(15) 0.0295(5) Uani 1 1 d . . . . .
H81 H 1.004936 0.365183 0.759871 0.035 Uiso 1 1 calc R . . . .
C36 C 0.58487(8) 0.64431(9) 0.81284(15) 0.0263(5) Uani 1 1 d . . . . .
H36 H 0.617033 0.637920 0.824965 0.032 Uiso 1 1 calc R . . . .
C43 C 0.89895(8) 0.31070(9) 0.87052(15) 0.0264(5) Uani 1 1 d . . . . .
H43 H 0.866999 0.321779 0.837459 0.032 Uiso 1 1 calc R . . . .
C31 C 0.57727(8) 0.59321(9) 0.66020(14) 0.0262(5) Uani 1 1 d . . . . .
H31 H 0.609563 0.587706 0.675604 0.031 Uiso 1 1 calc R . . . .
C79 C 0.91988(8) 0.40804(9) 0.59059(15) 0.0275(5) Uani 1 1 d . . . . .
H79 H 0.887371 0.410209 0.574039 0.033 Uiso 1 1 calc R . . . .
C33 C 0.50879(8) 0.62876(10) 0.70155(15) 0.0304(5) Uani 1 1 d . . . . .
H33 H 0.494250 0.648292 0.744626 0.036 Uiso 1 1 calc R . . . .
C2 C 0.61808(8) 0.47482(10) 1.08105(14) 0.0278(5) Uani 1 1 d . . . . .
H2 H 0.642783 0.498451 1.070459 0.033 Uiso 1 1 calc R . . . .
C83 C 0.99277(8) 0.42624(9) 0.55335(15) 0.0288(5) Uani 1 1 d . . . . .
H83 H 1.010230 0.440084 0.510948 0.035 Uiso 1 1 calc R . . . .
C35 C 0.50413(8) 0.57986(10) 0.55337(15) 0.0295(5) Uani 1 1 d . . . . .
H35 H 0.486244 0.565748 0.495175 0.035 Uiso 1 1 calc R . . . .
C7 C 0.56961(8) 0.56731(10) 1.06840(15) 0.0283(5) Uani 1 1 d . . . . .
H7 H 0.541941 0.584906 1.076715 0.034 Uiso 1 1 calc R . . . .
C16 C 0.63352(8) 0.28613(10) 0.78932(15) 0.0284(5) Uani 1 1 d . . . . .
C77 C 0.92286(8) 0.45424(9) 0.43509(15) 0.0281(5) Uani 1 1 d . . . . .
H77 H 0.941744 0.470669 0.397349 0.034 Uiso 1 1 calc R . . . .
C15 C 0.65627(8) 0.26365(10) 0.88298(16) 0.0299(5) Uani 1 1 d . . . . .
H15 H 0.641695 0.232383 0.909295 0.036 Uiso 1 1 calc R . . . .
C18 C 0.63003(8) 0.35209(10) 0.65592(15) 0.0303(5) Uani 1 1 d . . . . .
C37 C 0.60149(8) 0.69406(10) 0.95779(15) 0.0278(5) Uani 1 1 d . . . . .
H37 H 0.633292 0.683021 0.953554 0.033 Uiso 1 1 calc R . . . .
C8 C 0.66832(8) 0.38552(10) 1.09442(15) 0.0297(5) Uani 1 1 d . . . . .
H8 H 0.693073 0.410288 1.087219 0.036 Uiso 1 1 calc R . . . .
C48 C 0.90931(8) 0.33750(9) 0.96949(15) 0.0272(5) Uani 1 1 d . . . . .
H48 H 0.942202 0.330438 1.000850 0.033 Uiso 1 1 calc R . . . .
C1 C 0.57592(8) 0.50202(10) 1.08113(14) 0.0278(5) Uani 1 1 d . . . . .
C96 C 0.52034(8) 0.32749(10) 0.85245(15) 0.0291(5) Uani 1 1 d . . . . .
C17 C 0.65244(8) 0.33203(10) 0.74438(15) 0.0301(5) Uani 1 1 d . . . . .
H17 H 0.680853 0.349536 0.774823 0.036 Uiso 1 1 calc R . . . .
C64 C 0.86893(8) 0.71218(10) 0.64259(15) 0.0301(5) Uani 1 1 d . . . . .
C66 C 0.86984(8) 0.64461(10) 0.51317(16) 0.0331(5) Uani 1 1 d . . . . .
C4 C 0.58710(8) 0.37893(10) 1.11008(15) 0.0318(5) Uani 1 1 d . . . . .
H4 H 0.590916 0.337010 1.120301 0.038 Uiso 1 1 calc R . . . .
C42 C 0.59116(8) 0.66577(9) 1.04584(15) 0.0271(5) Uani 1 1 d . . . . .
H42 H 0.558355 0.673158 1.046782 0.033 Uiso 1 1 calc R . . . .
C50 C 0.92417(8) 0.50202(10) 1.01290(15) 0.0294(5) Uani 1 1 d . . . . .
C82 C 1.01524(8) 0.40318(10) 0.64029(16) 0.0306(5) Uani 1 1 d . . . . .
H82 H 1.047778 0.402270 0.657673 0.037 Uiso 1 1 calc R . . . .
C54 C 0.87678(8) 0.59040(10) 0.97253(14) 0.0285(5) Uani 1 1 d . . . . .
C63 C 0.84660(8) 0.73689(10) 0.71446(15) 0.0303(5) Uani 1 1 d . . . . .
H63 H 0.861438 0.768629 0.753004 0.036 Uiso 1 1 calc R . . . .
C56 C 0.83297(8) 0.61836(10) 0.92511(15) 0.0309(5) Uani 1 1 d . . . . .
H56 H 0.807698 0.593404 0.898192 0.037 Uiso 1 1 calc R . . . .
C55 C 0.88222(8) 0.52849(10) 0.97099(15) 0.0282(5) Uani 1 1 d . . . . .
H55 H 0.857172 0.503999 0.941169 0.034 Uiso 1 1 calc R . . . .
C47 C 0.87833(8) 0.30880(10) 1.02762(16) 0.0303(5) Uani 1 1 d . . . . .
H47A H 0.886024 0.325388 1.092082 0.036 Uiso 1 1 calc R . . . .
H47B H 0.845929 0.318696 0.999144 0.036 Uiso 1 1 calc R . . . .
C41 C 0.62214(8) 0.69235(10) 1.13431(15) 0.0308(5) Uani 1 1 d . . . . .
H41A H 0.614219 0.674423 1.190449 0.037 Uiso 1 1 calc R . . . .
H41B H 0.654453 0.682206 1.135768 0.037 Uiso 1 1 calc R . . . .
C62 C 0.79091(8) 0.74653(10) 0.80155(16) 0.0292(5) Uani 1 1 d . . . . .
H62 H 0.813604 0.776751 0.834521 0.035 Uiso 1 1 calc R . . . .
C51 C 0.96068(8) 0.53814(10) 1.05673(15) 0.0309(5) Uani 1 1 d . . . . .
H51 H 0.989067 0.520432 1.086857 0.037 Uiso 1 1 calc R . . . .
C44 C 0.90327(8) 0.24229(10) 0.87352(16) 0.0312(5) Uani 1 1 d . . . . .
H44A H 0.894127 0.226217 0.808858 0.037 Uiso 1 1 calc R . . . .
H44B H 0.935662 0.231138 0.899487 0.037 Uiso 1 1 calc R . . . .
C75 C 0.86378(8) 0.48085(10) 0.30939(15) 0.0319(5) Uani 1 1 d . . . . .
H75 H 0.890814 0.493200 0.284487 0.038 Uiso 1 1 calc R . . . .
C70 C 0.84636(9) 0.59892(11) 0.44623(16) 0.0351(6) Uani 1 1 d . . . . .
H70 H 0.818694 0.582062 0.455872 0.042 Uiso 1 1 calc R . . . .
C49 C 0.93049(8) 0.43633(10) 1.01038(15) 0.0288(5) Uani 1 1 d . . . . .
H49 H 0.958351 0.419359 1.044871 0.035 Uiso 1 1 calc R . . . .
C14 C 0.71182(8) 0.25613(10) 1.02255(16) 0.0307(5) Uani 1 1 d . . . . .
H14 H 0.688945 0.226434 1.035048 0.037 Uiso 1 1 calc R . . . .
C5 C 0.54523(8) 0.40503(11) 1.10893(15) 0.0332(5) Uani 1 1 d . . . . .
H5 H 0.520165 0.381043 1.116666 0.040 Uiso 1 1 calc R . . . .
C88 C 0.97934(8) 0.67578(10) 0.82237(15) 0.0320(5) Uani 1 1 d . . . . .
C9 C 0.71903(8) 0.30468(10) 1.09854(16) 0.0323(5) Uani 1 1 d . . . . .
H9 H 0.738862 0.337217 1.082417 0.039 Uiso 1 1 calc R . . . .
C21 C 0.59144(8) 0.26220(10) 0.74498(16) 0.0317(5) Uani 1 1 d . . . . .
H21 H 0.578387 0.231085 0.774748 0.038 Uiso 1 1 calc R . . . .
C34 C 0.48258(8) 0.60753(10) 0.61699(16) 0.0326(5) Uani 1 1 d . . . . .
H34 H 0.450192 0.611851 0.602630 0.039 Uiso 1 1 calc R . . . .
C53 C 0.91418(8) 0.62599(10) 1.01598(15) 0.0319(5) Uani 1 1 d . . . . .
H53 H 0.910775 0.668280 1.017405 0.038 Uiso 1 1 calc R . . . .
C52 C 0.95565(9) 0.60044(10) 1.05650(15) 0.0329(5) Uani 1 1 d . . . . .
H52 H 0.980953 0.625096 1.084392 0.039 Uiso 1 1 calc R . . . .
C6 C 0.53988(8) 0.46695(10) 1.09634(15) 0.0317(5) Uani 1 1 d . . . . .
H6 H 0.511458 0.485212 1.098167 0.038 Uiso 1 1 calc R . . . .
C20 C 0.56808(8) 0.28307(10) 0.65761(16) 0.0335(5) Uani 1 1 d . . . . .
H20 H 0.538953 0.266911 0.628597 0.040 Uiso 1 1 calc R . . . .
C95 C 0.55272(9) 0.37282(10) 0.86488(15) 0.0316(5) Uani 1 1 d . . . . .
H95 H 0.578817 0.370060 0.915710 0.038 Uiso 1 1 calc R . . . .
C57 C 0.78363(8) 0.69890(10) 0.87214(16) 0.0328(5) Uani 1 1 d . . . . .
H57 H 0.763944 0.665994 0.838179 0.039 Uiso 1 1 calc R . . . .
C39 C 0.62784(9) 0.78877(10) 1.05042(16) 0.0346(6) Uani 1 1 d . . . . .
H39A H 0.660447 0.781752 1.050337 0.041 Uiso 1 1 calc R . . . .
H39B H 0.622856 0.832585 1.051859 0.041 Uiso 1 1 calc R . . . .
C45 C 0.87330(8) 0.21425(10) 0.93354(16) 0.0323(5) Uani 1 1 d . . . . .
H45A H 0.840616 0.221487 0.903759 0.039 Uiso 1 1 calc R . . . .
H45B H 0.878386 0.170394 0.937220 0.039 Uiso 1 1 calc R . . . .
C22 C 0.65180(8) 0.39782(10) 0.60785(16) 0.0324(5) Uani 1 1 d . . . . .
H22 H 0.678636 0.417225 0.642280 0.039 Uiso 1 1 calc R . . . .
C28 C 0.63274(8) 0.50921(10) 0.44002(15) 0.0308(5) Uani 1 1 d . . . . .
H28 H 0.605831 0.493991 0.392014 0.037 Uiso 1 1 calc R . . . .
C19 C 0.58737(8) 0.32746(10) 0.61304(16) 0.0318(5) Uani 1 1 d . . . . .
H19 H 0.571588 0.341341 0.552946 0.038 Uiso 1 1 calc R . . . .
C65 C 0.84820(8) 0.66729(10) 0.58045(16) 0.0322(5) Uani 1 1 d . . . . .
H65 H 0.819055 0.652133 0.584218 0.039 Uiso 1 1 calc R . . . .
C38 C 0.59746(8) 0.76252(10) 0.96107(16) 0.0332(5) Uani 1 1 d . . . . .
H38A H 0.606368 0.780033 0.905665 0.040 Uiso 1 1 calc R . . . .
H38B H 0.565145 0.773562 0.957917 0.040 Uiso 1 1 calc R . . . .
C46 C 0.88432(8) 0.24053(10) 1.03188(16) 0.0318(5) Uani 1 1 d . . . . .
H46A H 0.916281 0.230504 1.063677 0.038 Uiso 1 1 calc R . . . .
H46B H 0.863713 0.222891 1.068772 0.038 Uiso 1 1 calc R . . . .
C98 C 0.48261(8) 0.33104(11) 0.77701(16) 0.0360(6) Uani 1 1 d . . . . .
H98 H 0.460504 0.299782 0.766192 0.043 Uiso 1 1 calc R . . . .
C94 C 0.54839(9) 0.42233(10) 0.80553(16) 0.0370(6) Uani 1 1 d . . . . .
C69 C 0.91188(8) 0.73315(11) 0.63769(16) 0.0332(5) Uani 1 1 d . . . . .
H69 H 0.926086 0.763937 0.679115 0.040 Uiso 1 1 calc R . . . .
C68 C 0.93431(9) 0.70937(11) 0.57244(16) 0.0363(6) Uani 1 1 d . . . . .
H68 H 0.964173 0.722966 0.570957 0.044 Uiso 1 1 calc R . . . .
C71 C 0.83389(9) 0.53616(11) 0.31504(16) 0.0361(6) Uani 1 1 d . . . . .
H71 H 0.807158 0.524257 0.341238 0.043 Uiso 1 1 calc R . . . .
C87 C 0.94526(9) 0.63249(10) 0.80591(15) 0.0342(6) Uani 1 1 d . . . . .
H87 H 0.918724 0.638282 0.830054 0.041 Uiso 1 1 calc R . . . .
C40 C 0.61703(9) 0.76020(10) 1.13751(16) 0.0337(5) Uani 1 1 d . . . . .
H40A H 0.638133 0.776212 1.194430 0.040 Uiso 1 1 calc R . . . .
H40B H 0.585302 0.770436 1.140873 0.040 Uiso 1 1 calc R . . . .
C13 C 0.75680(8) 0.22356(11) 1.02284(18) 0.0368(6) Uani 1 1 d . . . . .
H13A H 0.751250 0.191705 0.974457 0.044 Uiso 1 1 calc R . . . .
H13B H 0.779174 0.252208 1.007257 0.044 Uiso 1 1 calc R . . . .
C61 C 0.74591(8) 0.77823(10) 0.75737(17) 0.0348(5) Uani 1 1 d . . . . .
H61A H 0.751680 0.809543 0.713537 0.042 Uiso 1 1 calc R . . . .
H61B H 0.724068 0.748935 0.720973 0.042 Uiso 1 1 calc R . . . .
C67 C 0.91332(9) 0.66626(11) 0.51016(17) 0.0364(6) Uani 1 1 d . . . . .
H67 H 0.928461 0.651017 0.464667 0.044 Uiso 1 1 calc R . . . .
C23 C 0.66307(8) 0.45607(11) 0.48173(16) 0.0342(5) Uani 1 1 d . . . . .
H23 H 0.689359 0.470851 0.531678 0.041 Uiso 1 1 calc R . . . .
C86 C 0.94889(10) 0.58069(11) 0.75489(16) 0.0414(6) Uani 1 1 d . . . . .
C97 C 0.52659(9) 0.27546(10) 0.92007(16) 0.0355(6) Uani 1 1 d . . . . .
H97A H 0.559047 0.264249 0.937443 0.053 Uiso 1 1 calc GR . . . .
H97B H 0.508452 0.241263 0.890143 0.053 Uiso 1 1 calc GR . . . .
H97C H 0.516316 0.287067 0.976525 0.053 Uiso 1 1 calc GR . . . .
C76 C 0.83592(9) 0.43395(11) 0.24344(16) 0.0387(6) Uani 1 1 d . . . . .
H76A H 0.855533 0.398745 0.239723 0.046 Uiso 1 1 calc R . . . .
H76B H 0.809862 0.420395 0.269323 0.046 Uiso 1 1 calc R . . . .
C27 C 0.65972(9) 0.55329(11) 0.39301(16) 0.0369(6) Uani 1 1 d . . . . .
H27A H 0.639330 0.586485 0.364433 0.044 Uiso 1 1 calc R . . . .
H27B H 0.685183 0.570590 0.441050 0.044 Uiso 1 1 calc R . . . .
C10 C 0.74130(9) 0.27875(11) 1.19537(17) 0.0396(6) Uani 1 1 d . . . . .
H10A H 0.748541 0.311840 1.241469 0.047 Uiso 1 1 calc R . . . .
H10B H 0.719262 0.251681 1.215753 0.047 Uiso 1 1 calc R . . . .
C12 C 0.77650(9) 0.19580(11) 1.11930(19) 0.0426(6) Uani 1 1 d . . . . .
H12A H 0.754713 0.165873 1.133756 0.051 Uiso 1 1 calc R . . . .
H12B H 0.805608 0.175012 1.118672 0.051 Uiso 1 1 calc R . . . .
C92 C 0.97403(9) 0.73087(11) 0.87870(17) 0.0391(6) Uani 1 1 d . . . . .
H92A H 0.941478 0.741202 0.868404 0.059 Uiso 1 1 calc GR . . . .
H92B H 0.990735 0.764337 0.858734 0.059 Uiso 1 1 calc GR . . . .
H92C H 0.986437 0.722868 0.945555 0.059 Uiso 1 1 calc GR . . . .
C100 C 0.50956(10) 0.42564(11) 0.73195(16) 0.0420(6) Uani 1 1 d . . . . .
H100 H 0.505316 0.459433 0.691378 0.050 Uiso 1 1 calc R . . . .
C99 C 0.47720(9) 0.38048(12) 0.71725(17) 0.0422(6) Uani 1 1 d . . . . .
H99 H 0.451171 0.383113 0.666246 0.051 Uiso 1 1 calc R . . . .
C89 C 1.01771(9) 0.66777(13) 0.78548(16) 0.0420(6) Uani 1 1 d . . . . .
H89 H 1.040924 0.697605 0.794747 0.050 Uiso 1 1 calc R . . . .
C58 C 0.76078(9) 0.72608(13) 0.94587(18) 0.0446(7) Uani 1 1 d . . . . .
H58A H 0.753685 0.693737 0.986643 0.054 Uiso 1 1 calc R . . . .
H58B H 0.782423 0.754119 0.985805 0.054 Uiso 1 1 calc R . . . .
C11 C 0.78508(9) 0.24418(12) 1.19436(19) 0.0455(7) Uani 1 1 d . . . . .
H11A H 0.808662 0.272279 1.182384 0.055 Uiso 1 1 calc R . . . .
H11B H 0.796913 0.225526 1.256593 0.055 Uiso 1 1 calc R . . . .
C74 C 0.81779(10) 0.45928(12) 0.14534(17) 0.0452(7) Uani 1 1 d . . . . .
H74A H 0.798492 0.428826 0.105620 0.054 Uiso 1 1 calc R . . . .
H74B H 0.843828 0.468806 0.116662 0.054 Uiso 1 1 calc R . . . .
C60 C 0.72495(9) 0.80679(13) 0.83222(19) 0.0481(7) Uani 1 1 d . . . . .
H60A H 0.695548 0.826194 0.802175 0.058 Uiso 1 1 calc R . . . .
H60B H 0.745855 0.837993 0.866014 0.058 Uiso 1 1 calc R . . . .
C91 C 0.98846(11) 0.57319(13) 0.72082(18) 0.0502(8) Uani 1 1 d . . . . .
H91 H 0.992190 0.537806 0.687231 0.060 Uiso 1 1 calc R . . . .
C24 C 0.68151(10) 0.42504(12) 0.40425(19) 0.0456(7) Uani 1 1 d . . . . .
H24A H 0.701723 0.391437 0.431808 0.055 Uiso 1 1 calc R . . . .
H24B H 0.655560 0.408259 0.356779 0.055 Uiso 1 1 calc R . . . .
C72 C 0.81664(10) 0.56229(12) 0.21628(18) 0.0486(7) Uani 1 1 d . . . . .
H72A H 0.796804 0.597331 0.219553 0.058 Uiso 1 1 calc R . . . .
H72B H 0.843106 0.576196 0.192031 0.058 Uiso 1 1 calc R . . . .
C26 C 0.67911(10) 0.52233(12) 0.31718(18) 0.0475(7) Uani 1 1 d . . . . .
H26A H 0.653551 0.509111 0.265531 0.057 Uiso 1 1 calc R . . . .
H26B H 0.697971 0.551198 0.290996 0.057 Uiso 1 1 calc R . . . .
C93 C 0.58516(11) 0.46980(12) 0.81969(18) 0.0545(8) Uani 1 1 d . . . . .
H93A H 0.573536 0.506790 0.841955 0.082 Uiso 1 1 calc GR . . . .
H93B H 0.593728 0.477531 0.760021 0.082 Uiso 1 1 calc GR . . . .
H93C H 0.612088 0.455940 0.866300 0.082 Uiso 1 1 calc GR . . . .
C59 C 0.71673(10) 0.75950(15) 0.9015(2) 0.0547(8) Uani 1 1 d . . . . .
H59A H 0.693534 0.730538 0.868497 0.066 Uiso 1 1 calc R . . . .
H59B H 0.704479 0.778969 0.951414 0.066 Uiso 1 1 calc R . . . .
C90 C 1.02219(10) 0.61658(14) 0.73540(19) 0.0529(8) Uani 1 1 d . . . . .
H90 H 1.048637 0.611173 0.710808 0.063 Uiso 1 1 calc R . . . .
C73 C 0.78958(10) 0.51578(13) 0.14884(19) 0.0529(7) Uani 1 1 d . . . . .
H73A H 0.761321 0.505142 0.169361 0.063 Uiso 1 1 calc R . . . .
H73B H 0.780439 0.533300 0.085118 0.063 Uiso 1 1 calc R . . . .
C85 C 0.91047(12) 0.53565(12) 0.7366(2) 0.0629(9) Uani 1 1 d . . . . .
H85A H 0.919511 0.500452 0.776653 0.094 Uiso 1 1 calc GR . . . .
H85B H 0.903860 0.523497 0.670546 0.094 Uiso 1 1 calc GR . . . .
H85C H 0.883016 0.553689 0.750877 0.094 Uiso 1 1 calc GR . . . .
C114 C 0.75243(10) 0.45784(11) 0.8345(2) 0.0369(11) Uani 0.625(4) 1 d D U P A 1
C109 C 0.75949(10) 0.49035(13) 0.7580(2) 0.0458(11) Uani 0.625(4) 1 d G U P A 1
H109 H 0.779925 0.475695 0.722228 0.055 Uiso 0.625(4) 1 calc R . P A 1
C110 C 0.73665(12) 0.54430(13) 0.7338(2) 0.0474(14) Uani 0.625(4) 1 d DG U P A
1
C111 C 0.70675(10) 0.56574(11) 0.7862(2) 0.0512(11) Uani 0.625(4) 1 d G U P A 1
H111 H 0.691139 0.602612 0.769653 0.061 Uiso 0.625(4) 1 calc R . P A 1
C112 C 0.69969(10) 0.53323(13) 0.8627(2) 0.0566(13) Uani 0.625(4) 1 d G U P A 1
H112 H 0.679252 0.547890 0.898451 0.068 Uiso 0.625(4) 1 calc R . P A 1
C113 C 0.72253(11) 0.47929(12) 0.88685(19) 0.0469(11) Uani 0.625(4) 1 d G U P A
1
H113 H 0.717701 0.457070 0.939137 0.056 Uiso 0.625(4) 1 calc R . P A 1
C25 C 0.70827(11) 0.46851(13) 0.3567(2) 0.0539(8) Uani 1 1 d . . . . .
H25A H 0.735920 0.482285 0.402726 0.065 Uiso 1 1 calc R . . . .
H25B H 0.718386 0.447636 0.305198 0.065 Uiso 1 1 calc R . . . .
C115 C 0.77697(15) 0.39946(19) 0.8638(3) 0.0519(12) Uani 0.625(4) 1 d D U P A 1
H11C H 0.780138 0.377273 0.807779 0.078 Uiso 0.625(4) 1 calc GR . P A 1
H11D H 0.759278 0.375503 0.899141 0.078 Uiso 0.625(4) 1 calc GR . P A 1
H11E H 0.807423 0.407695 0.903341 0.078 Uiso 0.625(4) 1 calc GR . P A 1
C116 C 0.7432(2) 0.5804(2) 0.6495(3) 0.0684(17) Uani 0.625(4) 1 d D U P A 1
H11F H 0.763238 0.558267 0.617035 0.103 Uiso 0.625(4) 1 calc GR . P A 1
H11G H 0.757255 0.619100 0.670923 0.103 Uiso 0.625(4) 1 calc GR . P A 1
H11H H 0.713406 0.587051 0.606449 0.103 Uiso 0.625(4) 1 calc GR . P A 1
C108 C 0.7149(4) 0.6035(4) 0.6638(7) 0.071(3) Uani 0.375(4) 1 d D U P A 2
H10C H 0.737525 0.627358 0.640712 0.107 Uiso 0.375(4) 1 calc GR . P A 2
H10D H 0.703079 0.627014 0.709705 0.107 Uiso 0.375(4) 1 calc GR . P A 2
H10E H 0.689578 0.592840 0.611053 0.107 Uiso 0.375(4) 1 calc GR . P A 2
C102 C 0.7443(3) 0.4713(3) 0.8291(4) 0.090(3) Uani 0.375(4) 1 d D U P A 2
C107 C 0.7799(3) 0.4449(3) 0.7971(6) 0.102(3) Uani 0.375(4) 1 d G U P A 2
H107 H 0.794472 0.409978 0.826924 0.122 Uiso 0.375(4) 1 calc R . P A 2
C106 C 0.7942(2) 0.4697(3) 0.7214(6) 0.101(3) Uani 0.375(4) 1 d G U P A 2
H106 H 0.818511 0.451692 0.699490 0.122 Uiso 0.375(4) 1 calc R . P A 2
C105 C 0.7729(2) 0.5209(3) 0.6777(5) 0.078(3) Uani 0.375(4) 1 d G U P A 2
H105 H 0.782635 0.537796 0.625975 0.094 Uiso 0.375(4) 1 calc R . P A 2
C104 C 0.7373(2) 0.5472(2) 0.7097(4) 0.049(2) Uani 0.375(4) 1 d DG U P A 2
C103 C 0.7230(2) 0.5225(3) 0.7854(4) 0.0559(19) Uani 0.375(4) 1 d G U P A 2
H103 H 0.698679 0.540475 0.807329 0.067 Uiso 0.375(4) 1 calc R . P A 2
C101 C 0.7287(6) 0.4448(6) 0.9102(7) 0.139(5) Uani 0.375(4) 1 d D U P A 2
H10F H 0.727786 0.401084 0.904429 0.209 Uiso 0.375(4) 1 calc GR . P A 2
H10G H 0.697949 0.459831 0.910354 0.209 Uiso 0.375(4) 1 calc GR . P A 2
H10H H 0.749988 0.456260 0.968893 0.209 Uiso 0.375(4) 1 calc GR . P A 2
O1 O 0.6858(6) 0.5815(8) 0.9833(14) 0.050(5) Uani 0.1 1 d . . P B 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
N7 C48 1.464(3) . ?
N7 C49 1.269(3) . ?
N8 C84 1.268(3) . ?
N8 C43 1.468(3) . ?
N6 C7 1.267(3) . ?
N6 C42 1.474(3) . ?
N5 C36 1.271(3) . ?
N5 C37 1.469(3) . ?
N9 C77 1.265(3) . ?
N9 C75 1.464(3) . ?
N2 C15 1.267(3) . ?
N2 C14 1.461(3) . ?
N11 C63 1.265(3) . ?
N11 C62 1.461(3) . ?
N4 C29 1.261(3) . ?
N4 C28 1.464(3) . ?
N1 C8 1.270(3) . ?
N1 C9 1.458(3) . ?
N3 C22 1.271(3) . ?
N3 C23 1.469(3) . ?
N12 C56 1.263(3) . ?
N12 C57 1.460(3) . ?
N10 C70 1.274(3) . ?
N10 C71 1.462(3) . ?
C32 C36 1.477(3) . ?
C32 C31 1.391(3) . ?
C32 C33 1.391(3) . ?
C84 C80 1.476(3) . ?
C30 C29 1.477(3) . ?
C30 C31 1.400(3) . ?
C30 C35 1.390(3) . ?
C80 C81 1.398(3) . ?
C80 C79 1.391(3) . ?
C78 C79 1.404(3) . ?
C78 C83 1.385(3) . ?
C78 C77 1.480(3) . ?
C3 C2 1.392(3) . ?
C3 C8 1.473(3) . ?
C3 C4 1.401(3) . ?
C81 C82 1.384(3) . ?
C43 C48 1.531(3) . ?
C43 C44 1.532(3) . ?
C33 C34 1.388(3) . ?
C2 C1 1.402(3) . ?
C83 C82 1.394(3) . ?
C35 C34 1.393(3) . ?
C7 C1 1.476(3) . ?
C16 C15 1.472(3) . ?
C16 C17 1.405(3) . ?
C16 C21 1.386(3) . ?
C18 C17 1.389(3) . ?
C18 C22 1.474(3) . ?
C18 C19 1.401(3) . ?
C37 C42 1.528(3) . ?
C37 C38 1.534(3) . ?
C48 C47 1.535(3) . ?
C1 C6 1.392(3) . ?
C96 C95 1.385(3) . ?
C96 C98 1.390(3) . ?
C96 C97 1.509(3) . ?
C64 C63 1.476(3) . ?
C64 C65 1.399(3) . ?
C64 C69 1.387(3) . ?
C66 C70 1.476(3) . ?
C66 C65 1.392(3) . ?
C66 C67 1.400(3) . ?
C4 C5 1.380(3) . ?
C42 C41 1.529(3) . ?
C50 C55 1.398(3) . ?
C50 C51 1.392(3) . ?
C50 C49 1.480(3) . ?
C54 C56 1.476(3) . ?
C54 C55 1.392(3) . ?
C54 C53 1.402(3) . ?
C47 C46 1.534(3) . ?
C41 C40 1.524(3) . ?
C62 C57 1.532(3) . ?
C62 C61 1.529(3) . ?
C51 C52 1.398(3) . ?
C44 C45 1.526(3) . ?
C75 C71 1.538(3) . ?
C75 C76 1.535(3) . ?
C14 C9 1.532(3) . ?
C14 C13 1.531(3) . ?
C5 C6 1.398(3) . ?
C88 C87 1.386(3) . ?
C88 C92 1.509(3) . ?
C88 C89 1.389(3) . ?
C9 C10 1.535(3) . ?
C21 C20 1.390(3) . ?
C53 C52 1.373(3) . ?
C20 C19 1.383(3) . ?
C95 C94 1.393(3) . ?
C57 C58 1.529(3) . ?
C39 C38 1.528(3) . ?
C39 C40 1.524(3) . ?
C45 C46 1.518(3) . ?
C28 C23 1.533(3) . ?
C28 C27 1.532(3) . ?
C98 C99 1.394(3) . ?
C94 C100 1.395(4) . ?
C94 C93 1.508(4) . ?
C69 C68 1.392(3) . ?
C68 C67 1.374(4) . ?
C71 C72 1.534(3) . ?
C87 C86 1.393(3) . ?
C13 C12 1.531(3) . ?
C61 C60 1.521(3) . ?
C23 C24 1.535(3) . ?
C86 C91 1.397(4) . ?
C86 C85 1.506(4) . ?
C76 C74 1.522(3) . ?
C27 C26 1.530(3) . ?
C10 C11 1.525(4) . ?
C12 C11 1.519(4) . ?
C100 C99 1.381(4) . ?
C89 C90 1.380(4) . ?
C58 C59 1.526(4) . ?
C74 C73 1.525(4) . ?
C60 C59 1.521(4) . ?
C91 C90 1.381(4) . ?
C24 C25 1.525(4) . ?
C72 C73 1.530(4) . ?
C26 C25 1.519(4) . ?
C114 C109 1.3900 . ?
C114 C113 1.3900 . ?
C114 C115 1.509(4) . ?
C109 C110 1.3900 . ?
C110 C111 1.3900 . ?
C110 C116 1.523(5) . ?
C111 C112 1.3900 . ?
C112 C113 1.3900 . ?
C108 C104 1.508(7) . ?
C102 C107 1.3900 . ?
C102 C103 1.3900 . ?
C102 C101 1.493(8) . ?
C107 C106 1.3900 . ?
C106 C105 1.3900 . ?
C105 C104 1.3900 . ?
C104 C103 1.3900 . ?

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
C49 N7 C48 117.2(2) . . ?
C84 N8 C43 117.30(19) . . ?
C7 N6 C42 116.66(19) . . ?
C36 N5 C37 117.48(19) . . ?
C77 N9 C75 116.20(19) . . ?
C15 N2 C14 116.87(19) . . ?
C63 N11 C62 117.26(19) . . ?
C29 N4 C28 116.99(19) . . ?
C8 N1 C9 118.8(2) . . ?
C22 N3 C23 117.5(2) . . ?
C56 N12 C57 118.6(2) . . ?
C70 N10 C71 117.1(2) . . ?
C31 C32 C36 118.9(2) . . ?
C33 C32 C36 121.6(2) . . ?
C33 C32 C31 119.5(2) . . ?
N8 C84 C80 123.5(2) . . ?
C31 C30 C29 121.3(2) . . ?
C35 C30 C29 119.8(2) . . ?
C35 C30 C31 118.9(2) . . ?
C81 C80 C84 121.4(2) . . ?
C79 C80 C84 119.2(2) . . ?
C79 C80 C81 119.3(2) . . ?
C79 C78 C77 121.6(2) . . ?
C83 C78 C79 119.1(2) . . ?
C83 C78 C77 119.33(19) . . ?
C2 C3 C8 119.8(2) . . ?
C2 C3 C4 119.2(2) . . ?
C4 C3 C8 121.0(2) . . ?
N4 C29 C30 123.6(2) . . ?
C82 C81 C80 120.6(2) . . ?
N5 C36 C32 123.3(2) . . ?
N8 C43 C48 109.92(17) . . ?
N8 C43 C44 108.53(18) . . ?
C48 C43 C44 111.37(18) . . ?
C32 C31 C30 120.7(2) . . ?
C80 C79 C78 120.5(2) . . ?
C34 C33 C32 120.5(2) . . ?
C3 C2 C1 120.5(2) . . ?
C78 C83 C82 121.0(2) . . ?
C30 C35 C34 120.9(2) . . ?
N6 C7 C1 122.3(2) . . ?
C17 C16 C15 122.3(2) . . ?
C21 C16 C15 118.8(2) . . ?
C21 C16 C17 118.9(2) . . ?
N9 C77 C78 123.8(2) . . ?
N2 C15 C16 124.0(2) . . ?
C17 C18 C22 119.7(2) . . ?
C17 C18 C19 119.2(2) . . ?
C19 C18 C22 121.1(2) . . ?
N5 C37 C42 109.75(18) . . ?
N5 C37 C38 108.61(18) . . ?
C42 C37 C38 110.63(18) . . ?
N1 C8 C3 121.9(2) . . ?
N7 C48 C43 109.49(17) . . ?
N7 C48 C47 108.02(18) . . ?
C43 C48 C47 110.09(18) . . ?
C2 C1 C7 121.1(2) . . ?
C6 C1 C2 119.3(2) . . ?
C6 C1 C7 119.6(2) . . ?
C95 C96 C98 118.7(2) . . ?
C95 C96 C97 119.9(2) . . ?
C98 C96 C97 121.4(2) . . ?
C18 C17 C16 120.7(2) . . ?
C65 C64 C63 121.6(2) . . ?
C69 C64 C63 119.2(2) . . ?
C69 C64 C65 119.2(2) . . ?
C65 C66 C70 119.5(2) . . ?
C65 C66 C67 119.0(2) . . ?
C67 C66 C70 121.6(2) . . ?
C5 C4 C3 120.8(2) . . ?
N6 C42 C37 110.23(17) . . ?
N6 C42 C41 107.63(18) . . ?
C37 C42 C41 110.63(18) . . ?
C55 C50 C49 121.0(2) . . ?
C51 C50 C55 119.4(2) . . ?
C51 C50 C49 119.6(2) . . ?
C81 C82 C83 119.5(2) . . ?
C55 C54 C56 120.5(2) . . ?
C55 C54 C53 119.0(2) . . ?
C53 C54 C56 120.4(2) . . ?
N11 C63 C64 123.4(2) . . ?
N12 C56 C54 121.8(2) . . ?
C54 C55 C50 120.6(2) . . ?
C46 C47 C48 110.91(18) . . ?
C40 C41 C42 111.44(19) . . ?
N11 C62 C57 109.32(17) . . ?
N11 C62 C61 108.93(18) . . ?
C61 C62 C57 110.99(19) . . ?
C50 C51 C52 120.1(2) . . ?
C45 C44 C43 111.60(19) . . ?
N9 C75 C71 109.71(18) . . ?
N9 C75 C76 109.62(19) . . ?
C76 C75 C71 110.0(2) . . ?
N10 C70 C66 123.3(2) . . ?
N7 C49 C50 122.2(2) . . ?
N2 C14 C9 109.51(18) . . ?
N2 C14 C13 109.58(19) . . ?
C13 C14 C9 110.84(19) . . ?
C4 C5 C6 119.7(2) . . ?
C87 C88 C92 119.8(2) . . ?
C87 C88 C89 119.0(2) . . ?
C89 C88 C92 121.1(2) . . ?
N1 C9 C14 108.29(18) . . ?
N1 C9 C10 108.52(19) . . ?
C14 C9 C10 111.27(19) . . ?
C16 C21 C20 120.9(2) . . ?
C33 C34 C35 119.5(2) . . ?
C52 C53 C54 120.8(2) . . ?
C53 C52 C51 120.0(2) . . ?
C1 C6 C5 120.4(2) . . ?
C19 C20 C21 119.8(2) . . ?
C96 C95 C94 122.4(2) . . ?
N12 C57 C62 108.74(18) . . ?
N12 C57 C58 108.81(19) . . ?
C58 C57 C62 110.9(2) . . ?
C40 C39 C38 110.83(19) . . ?
C46 C45 C44 110.95(19) . . ?
N3 C22 C18 123.1(2) . . ?
N4 C28 C23 109.67(17) . . ?
N4 C28 C27 109.55(18) . . ?
C27 C28 C23 110.5(2) . . ?
C20 C19 C18 120.5(2) . . ?
C66 C65 C64 120.7(2) . . ?
C39 C38 C37 111.88(19) . . ?
C45 C46 C47 110.31(18) . . ?
C96 C98 C99 120.0(2) . . ?
C95 C94 C100 117.7(2) . . ?
C95 C94 C93 120.7(2) . . ?
C100 C94 C93 121.5(2) . . ?
C64 C69 C68 120.4(2) . . ?
C67 C68 C69 120.1(2) . . ?
N10 C71 C75 109.2(2) . . ?
N10 C71 C72 109.7(2) . . ?
C72 C71 C75 109.23(19) . . ?
C88 C87 C86 121.8(2) . . ?
C41 C40 C39 110.36(18) . . ?
C12 C13 C14 110.4(2) . . ?
C60 C61 C62 111.0(2) . . ?
C68 C67 C66 120.6(2) . . ?
N3 C23 C28 110.18(19) . . ?
N3 C23 C24 108.86(19) . . ?
C28 C23 C24 109.62(19) . . ?
C87 C86 C91 117.8(3) . . ?
C87 C86 C85 119.9(2) . . ?
C91 C86 C85 122.3(2) . . ?
C74 C76 C75 111.4(2) . . ?
C26 C27 C28 111.3(2) . . ?
C11 C10 C9 112.0(2) . . ?
C11 C12 C13 110.2(2) . . ?
C99 C100 C94 120.9(2) . . ?
C100 C99 C98 120.2(2) . . ?
C90 C89 C88 120.2(3) . . ?
C59 C58 C57 112.1(2) . . ?
C12 C11 C10 111.3(2) . . ?
C76 C74 C73 110.9(2) . . ?
C61 C60 C59 110.2(2) . . ?
C90 C91 C86 120.8(2) . . ?
C25 C24 C23 111.5(2) . . ?
C73 C72 C71 111.4(2) . . ?
C25 C26 C27 111.2(2) . . ?
C60 C59 C58 111.5(2) . . ?
C89 C90 C91 120.4(3) . . ?
C74 C73 C72 111.5(2) . . ?
C109 C114 C113 120.0 . . ?
C109 C114 C115 121.7(3) . . ?
C113 C114 C115 118.3(3) . . ?
C110 C109 C114 120.0 . . ?
C109 C110 C111 120.0 . . ?
C109 C110 C116 121.1(3) . . ?
C111 C110 C116 118.9(3) . . ?
C112 C111 C110 120.0 . . ?
C111 C112 C113 120.0 . . ?
C112 C113 C114 120.0 . . ?
C26 C25 C24 111.1(2) . . ?
C107 C102 C103 120.0 . . ?
C107 C102 C101 120.3(9) . . ?
C103 C102 C101 119.7(9) . . ?
C102 C107 C106 120.0 . . ?
C105 C106 C107 120.0 . . ?
C106 C105 C104 120.0 . . ?
C105 C104 C108 120.0(7) . . ?
C105 C104 C103 120.0 . . ?
C103 C104 C108 120.0(7) . . ?
C104 C103 C102 120.0 . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.315
_oxdiff_exptl_absorpt_empirical_full_min 0.754
