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

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

data_C12H12O4
_audit_block_doi                 10.5517/cc816r7
_database_code_depnum_ccdc_archive 'CCDC 239498'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1016/j.tet.2004.08.018 2004
_audit_update_record             
;
2004-05-20 deposited with the CCDC.	2025-05-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
methyl (2E)-3-(1,3-benzodioxol-5-yl)-2-methylacrylate
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H12 O4'
_chemical_formula_weight         220.22

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'

loop_
_symmetry_equiv_pos_as_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                   14.526(3)
_cell_length_b                   6.5167(13)
_cell_length_c                   23.570(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.77(3)
_cell_angle_gamma                90.00
_cell_volume                     2157.5(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      3.70
_cell_measurement_theta_max      12.03

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             928
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       ω--2θ
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        1
_diffrn_reflns_number            3435
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0514
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.79
_diffrn_reflns_theta_max         25.07
_reflns_number_total             1887
_reflns_number_gt                1037
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      
'calc w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+0.5445P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1887
_refine_ls_number_parameters     145
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1121
_refine_ls_R_factor_gt           0.0448
_refine_ls_wR_factor_ref         0.1253
_refine_ls_wR_factor_gt          0.1034
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.36479(16) 0.4908(3) 0.49367(10) 0.0453(6) Uani 1 d . . .
C2 C 0.40630(17) 0.6702(4) 0.52195(10) 0.0552(7) Uani 1 d . . .
H2 H 0.3982 0.7960 0.5027 0.066 Uiso 1 calc R . .
C3 C 0.45877(17) 0.6539(4) 0.57856(11) 0.0536(7) Uani 1 d . . .
C5 C 0.5464(2) 0.7161(5) 0.66937(11) 0.0733(9) Uani 1 d . . .
H5A H 0.5176 0.7738 0.6987 0.088 Uiso 1 calc R . .
H5B H 0.6144 0.7416 0.6814 0.088 Uiso 1 calc R . .
C7 C 0.47175(16) 0.4716(4) 0.60832(10) 0.0507(7) Uani 1 d . . .
C8 C 0.43366(19) 0.2948(4) 0.58286(11) 0.0586(7) Uani 1 d . . .
H8 H 0.4428 0.1708 0.6030 0.070 Uiso 1 calc R . .
C9 C 0.38033(17) 0.3077(4) 0.52515(11) 0.0536(7) Uani 1 d . . .
H9 H 0.3536 0.1880 0.5065 0.064 Uiso 1 calc R . .
C10 C 0.30664(16) 0.4789(4) 0.43313(10) 0.0496(6) Uani 1 d . . .
H10 H 0.2894 0.3457 0.4207 0.060 Uiso 1 calc R . .
C11 C 0.27323(16) 0.6211(4) 0.39204(10) 0.0483(6) Uani 1 d . . .
C12 C 0.2897(2) 0.8470(4) 0.39812(12) 0.0718(8) Uani 1 d . . .
H12A H 0.2581 0.9138 0.3621 0.108 Uiso 1 calc R . .
H12B H 0.3568 0.8744 0.4067 0.108 Uiso 1 calc R . .
H12C H 0.2649 0.8981 0.4294 0.108 Uiso 1 calc R . .
C13 C 0.21231(18) 0.5548(5) 0.33489(11) 0.0574(7) Uani 1 d . . .
C16 C 0.1468(2) 0.2734(6) 0.27310(12) 0.0900(11) Uani 1 d . . .
H16A H 0.1511 0.1265 0.2726 0.135 Uiso 1 calc R . .
H16B H 0.1654 0.3290 0.2400 0.135 Uiso 1 calc R . .
H16C H 0.0824 0.3130 0.2711 0.135 Uiso 1 calc R . .
O4 O 0.50661(15) 0.8078(3) 0.61403(8) 0.0863(7) Uani 1 d . . .
O6 O 0.52848(13) 0.5004(3) 0.66393(7) 0.0710(6) Uani 1 d . . .
O14 O 0.16775(15) 0.6703(4) 0.29828(8) 0.0911(7) Uani 1 d . . .
O15 O 0.20935(13) 0.3519(3) 0.32683(7) 0.0733(6) Uani 1 d . . .


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
C1 C9 1.393(3) . ?
C1 C2 1.403(3) . ?
C1 C10 1.463(3) . ?
C2 C3 1.361(3) . ?
C3 C7 1.368(3) . ?
C3 O4 1.375(3) . ?
C5 O4 1.417(3) . ?
C5 O6 1.429(3) . ?
C7 C8 1.351(3) . ?
C7 O6 1.372(3) . ?
C8 C9 1.386(3) . ?
C10 C11 1.339(3) . ?
C11 C13 1.475(3) . ?
C11 C12 1.493(4) . ?
C13 O14 1.202(3) . ?
C13 O15 1.335(3) . ?
C16 O15 1.451(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
C9 C1 C2 118.0(2) . . ?
C9 C1 C10 116.7(2) . . ?
C2 C1 C10 125.4(2) . . ?
C3 C2 C1 117.8(2) . . ?
C2 C3 C7 122.7(2) . . ?
C2 C3 O4 127.5(2) . . ?
C7 C3 O4 109.8(2) . . ?
O4 C5 O6 108.1(2) . . ?
C8 C7 C3 121.7(2) . . ?
C8 C7 O6 128.3(2) . . ?
C3 C7 O6 110.0(2) . . ?
C7 C8 C9 116.6(2) . . ?
C8 C9 C1 123.3(2) . . ?
C11 C10 C1 132.9(2) . . ?
C10 C11 C13 118.7(2) . . ?
C10 C11 C12 126.4(2) . . ?
C13 C11 C12 114.9(2) . . ?
O14 C13 O15 121.8(2) . . ?
O14 C13 C11 124.0(3) . . ?
O15 C13 C11 114.2(2) . . ?
C3 O4 C5 106.0(2) . . ?
C7 O6 C5 105.77(19) . . ?
C13 O15 C16 117.6(2) . . ?

_diffrn_measured_fraction_theta_max 0.449
_diffrn_reflns_theta_full        25.07
_diffrn_measured_fraction_theta_full 0.449
_refine_diff_density_max         0.142
_refine_diff_density_min         -0.161
_refine_diff_density_rms         0.036


####################################################################### 
# 
# 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_tbai3_autored
_database_code_depnum_ccdc_archive 'CCDC 2405509'
loop_
_audit_author_name
_audit_author_address
'Toshio Naito'
;Ehime University
Japan
;
_audit_update_record             
;
2024-11-26 deposited with the CCDC.	2025-05-30 downloaded from the CCDC.
;
_audit_creation_date             2024-11-26
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            TBAI3
_chemical_name_systematic        'tetrabutylammonium triiodide'
_chemical_formula_moiety         '0.667(I3), 0.667(C16 H36 N)'
_chemical_formula_sum            'C10.67 H24 I2 N0.67'
_chemical_formula_weight         415.44
_chemical_melting_point          ?
_chemical_oxdiff_formula         C16H36N1I3
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'
I I -0.4742 1.8119 '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      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                   9.5532(4)
_cell_length_b                   15.7479(6)
_cell_length_c                   15.9567(6)
_cell_angle_alpha                83.412(3)
_cell_angle_beta                 74.365(3)
_cell_angle_gamma                78.582(3)
_cell_volume                     2261.20(16)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    18054
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.3380
_cell_measurement_theta_min      1.7140
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.142
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62220
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic black'
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.223
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.034
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            43072
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.337
_diffrn_reflns_theta_min         1.812
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 7.111
_diffrn_detector_type            'Rigaku Saturn724+ area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.912
_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  70.00   0.50    6.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50    6.00    --  -20.00  45.00  90.00  360
  3  ω   -110.00  70.00   0.50    6.00    --  -20.00  45.00 180.00  360
  4  ω   -110.00  70.00   0.50    6.00    --  -20.00  45.00 270.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Rigaku Varimax with Saturn'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0258515000
_diffrn_orient_matrix_UB_12      0.0061060000
_diffrn_orient_matrix_UB_13      -0.0459333000
_diffrn_orient_matrix_UB_21      -0.0100498000
_diffrn_orient_matrix_UB_22      0.0454168000
_diffrn_orient_matrix_UB_23      0.0035408000
_diffrn_orient_matrix_UB_31      0.0732262000
_diffrn_orient_matrix_UB_32      -0.0045208000
_diffrn_orient_matrix_UB_33      0.0041649000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'MicroMax 007'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8542
_reflns_number_total             13528
_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 2.1 b46 (Rigaku, 2016)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.904
_refine_diff_density_min         -1.058
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         13528
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0509
_refine_ls_restrained_S_all      1.056
_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)+(0.0379P)²+4.7504P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1207
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C25(H25A,H25B), C1(H1A,H1B), C21(H21A,H21B), C17(H17A,H17B),
 C5(H5A,H5B), C13(H13A,H13B), C29(H29A,H29B), C26(H26A,H26B), C22(H22A,H22B),
 C10(H10A,H10B), C2(H2A,H2B), C6(H6A,H6B), C18(H18A,H18B), C15(H15A,H15B),
 C31(H31A,H31B), C14(H14A,H14B), C30(H30A,H30B), C19(H19A,H19B), C27(H27A,H27B),
  C7(H7A,H7B), C23(H23A,H23B), C11(H11A,H11B), C3(H3A,H3B)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C32(H32A,H32B,H32C), C20(H20A,H20B,H20C), C16(H16A,H16B,
 H16C), C28(H28A,H28B,H28C), C24(H24A,H24B,H24C), C8(H8A,H8B,H8C), C4(H4A,H4B,
 H4C)
;
_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
I5 I 0.31059(4) 0.24565(2) 0.49722(2) 0.04570(10) Uani 1 1 d . . . . .
I2 I 0.50143(4) 0.25113(2) -0.00533(2) 0.05173(10) Uani 1 1 d . . . . .
I4 I 0.61199(4) 0.26647(3) 0.48282(3) 0.05676(12) Uani 1 1 d . . . . .
I1 I 0.82081(5) 0.21655(3) -0.01714(3) 0.06554(13) Uani 1 1 d . . . . .
I6 I 0.00155(5) 0.24108(3) 0.50477(3) 0.06495(12) Uani 1 1 d . . . . .
I3 I 0.18961(5) 0.28021(3) 0.00505(3) 0.07098(14) Uani 1 1 d . . . . .
N007 N 0.0793(4) 0.9687(3) 0.7352(3) 0.0373(9) Uani 1 1 d . . . . .
N008 N 0.3159(4) 0.4979(3) 0.2695(2) 0.0372(9) Uani 1 1 d . . . . .
C9 C 0.2192(5) 0.5004(3) 0.3627(3) 0.0410(11) Uani 1 1 d . . . . .
H9A H 0.146874 0.553508 0.367023 0.049 Uiso 1 1 calc R U . . .
H9B H 0.165667 0.452271 0.373791 0.049 Uiso 1 1 calc R U . . .
C25 C -0.0808(5) 0.9829(3) 0.7868(3) 0.0419(11) Uani 1 1 d . . . . .
H25A H -0.126967 1.040991 0.771268 0.050 Uiso 1 1 calc R U . . .
H25B H -0.130161 0.942371 0.769069 0.050 Uiso 1 1 calc R U . . .
C1 C 0.2127(6) 0.5172(3) 0.2098(3) 0.0420(11) Uani 1 1 d . . . . .
H1A H 0.151717 0.573676 0.221674 0.050 Uiso 1 1 calc R U . . .
H1B H 0.147727 0.474602 0.224166 0.050 Uiso 1 1 calc R U . . .
C21 C 0.1610(6) 1.0320(3) 0.7584(3) 0.0439(12) Uani 1 1 d . . . . .
H21A H 0.262533 1.021387 0.723915 0.053 Uiso 1 1 calc R U . . .
H21B H 0.162269 1.020110 0.819218 0.053 Uiso 1 1 calc R U . . .
C17 C 0.0807(6) 0.9814(3) 0.6390(3) 0.0416(11) Uani 1 1 d . . . . .
H17A H 0.038842 0.935192 0.624923 0.050 Uiso 1 1 calc R U . . .
H17B H 0.016829 1.035752 0.629807 0.050 Uiso 1 1 calc R U . . .
C5 C 0.4174(5) 0.5641(3) 0.2521(3) 0.0413(11) Uani 1 1 d . . . . .
H5A H 0.479748 0.559004 0.193189 0.050 Uiso 1 1 calc R U . . .
H5B H 0.481192 0.549649 0.291612 0.050 Uiso 1 1 calc R U . . .
C13 C 0.4131(6) 0.4087(3) 0.2552(3) 0.0419(11) Uani 1 1 d . . . . .
H13A H 0.487414 0.412842 0.200497 0.050 Uiso 1 1 calc R U . . .
H13B H 0.464206 0.394788 0.301216 0.050 Uiso 1 1 calc R U . . .
C29 C 0.1550(5) 0.8770(3) 0.7566(3) 0.0398(11) Uani 1 1 d . . . . .
H29A H 0.254589 0.867779 0.719277 0.048 Uiso 1 1 calc R U . . .
H29B H 0.162662 0.873261 0.816351 0.048 Uiso 1 1 calc R U . . .
C26 C -0.1065(6) 0.9722(4) 0.8850(3) 0.0487(13) Uani 1 1 d . . . . .
H26A H -0.062669 1.014565 0.904216 0.058 Uiso 1 1 calc R U . . .
H26B H -0.059147 0.914777 0.901599 0.058 Uiso 1 1 calc R U . . .
C22 C 0.0982(6) 1.1271(3) 0.7446(3) 0.0463(12) Uani 1 1 d . . . . .
H22A H 0.089563 1.138969 0.685000 0.056 Uiso 1 1 calc R U . . .
H22B H 0.000064 1.139880 0.783091 0.056 Uiso 1 1 calc R U . . .
C10 C 0.2982(6) 0.4958(3) 0.4339(3) 0.0427(11) Uani 1 1 d . . . . .
H10A H 0.343921 0.546769 0.427468 0.051 Uiso 1 1 calc R U . . .
H10B H 0.375503 0.445020 0.428293 0.051 Uiso 1 1 calc R U . . .
C2 C 0.2870(6) 0.5169(4) 0.1126(3) 0.0478(13) Uani 1 1 d . . . . .
H2A H 0.343983 0.563482 0.095521 0.057 Uiso 1 1 calc R U . . .
H2B H 0.353825 0.462343 0.099843 0.057 Uiso 1 1 calc R U . . .
C6 C 0.3412(6) 0.6579(4) 0.2619(4) 0.0491(13) Uani 1 1 d . . . . .
H6A H 0.267991 0.662581 0.317458 0.059 Uiso 1 1 calc R U . . .
H6B H 0.290610 0.676472 0.216012 0.059 Uiso 1 1 calc R U . . .
C18 C 0.2298(6) 0.9824(4) 0.5766(3) 0.0462(12) Uani 1 1 d . . . . .
H18A H 0.297923 0.931139 0.589140 0.055 Uiso 1 1 calc R U . . .
H18B H 0.267266 1.032995 0.584606 0.055 Uiso 1 1 calc R U . . .
C15 C 0.4434(6) 0.2491(3) 0.2460(3) 0.0473(13) Uani 1 1 d . . . . .
H15A H 0.485134 0.238876 0.296084 0.057 Uiso 1 1 calc R U . . .
H15B H 0.523590 0.252537 0.194051 0.057 Uiso 1 1 calc R U . . .
C31 C 0.1650(6) 0.7164(3) 0.7688(4) 0.0479(13) Uani 1 1 d . . . . .
H31A H 0.264250 0.708902 0.730941 0.057 Uiso 1 1 calc R U . . .
H31B H 0.172573 0.713924 0.828480 0.057 Uiso 1 1 calc R U . . .
C14 C 0.3368(6) 0.3341(3) 0.2529(3) 0.0438(12) Uani 1 1 d . . . . .
H14A H 0.293624 0.344009 0.203321 0.053 Uiso 1 1 calc R U . . .
H14B H 0.257592 0.331273 0.305430 0.053 Uiso 1 1 calc R U . . .
C30 C 0.0800(6) 0.8047(3) 0.7464(4) 0.0462(12) Uani 1 1 d . . . . .
H30A H 0.072370 0.807192 0.686751 0.055 Uiso 1 1 calc R U . . .
H30B H -0.019147 0.812286 0.784348 0.055 Uiso 1 1 calc R U . . .
C19 C 0.2218(7) 0.9844(4) 0.4824(3) 0.0518(14) Uani 1 1 d . . . . .
H19A H 0.184443 0.933624 0.474832 0.062 Uiso 1 1 calc R U . . .
H19B H 0.152207 1.035307 0.470610 0.062 Uiso 1 1 calc R U . . .
C27 C -0.2705(6) 0.9844(4) 0.9292(4) 0.0558(15) Uani 1 1 d . . . . .
H27A H -0.317943 1.040995 0.910307 0.067 Uiso 1 1 calc R U . . .
H27B H -0.313122 0.940811 0.911059 0.067 Uiso 1 1 calc R U . . .
C7 C 0.4518(7) 0.7171(4) 0.2572(4) 0.0516(13) Uani 1 1 d . . . . .
H7A H 0.494588 0.702700 0.306736 0.062 Uiso 1 1 calc R U . . .
H7B H 0.530889 0.707873 0.204472 0.062 Uiso 1 1 calc R U . . .
C12 C 0.2700(8) 0.4782(4) 0.5961(4) 0.0626(17) Uani 1 1 d . . . . .
H12A H 0.319956 0.526048 0.593336 0.094 Uiso 1 1 calc R U . . .
H12B H 0.340565 0.425153 0.589736 0.094 Uiso 1 1 calc R U . . .
H12C H 0.198826 0.475155 0.651331 0.094 Uiso 1 1 calc R U . . .
C23 C 0.1936(7) 1.1857(4) 0.7619(4) 0.0579(15) Uani 1 1 d . . . . .
H23A H 0.207753 1.170988 0.820116 0.069 Uiso 1 1 calc R U . . .
H23B H 0.289772 1.175447 0.720784 0.069 Uiso 1 1 calc R U . . .
C11 C 0.1920(7) 0.4911(4) 0.5232(3) 0.0515(14) Uani 1 1 d . . . . .
H11A H 0.139477 0.443374 0.527207 0.062 Uiso 1 1 calc R U . . .
H11B H 0.119869 0.544302 0.530350 0.062 Uiso 1 1 calc R U . . .
C32 C 0.0904(8) 0.6432(4) 0.7586(4) 0.0664(17) Uani 1 1 d . . . . .
H32A H 0.092883 0.641377 0.698259 0.100 Uiso 1 1 calc R U . . .
H32B H -0.010277 0.652880 0.792480 0.100 Uiso 1 1 calc R U . . .
H32C H 0.141321 0.589088 0.778488 0.100 Uiso 1 1 calc R U . . .
C3 C 0.1712(7) 0.5289(4) 0.0615(4) 0.0580(15) Uani 1 1 d . . . . .
H3A H 0.115511 0.481753 0.078497 0.070 Uiso 1 1 calc R U . . .
H3B H 0.103060 0.582753 0.076034 0.070 Uiso 1 1 calc R U . . .
C20 C 0.3681(8) 0.9864(4) 0.4174(4) 0.0678(18) Uani 1 1 d . . . . .
H20A H 0.356274 0.986440 0.359510 0.102 Uiso 1 1 calc R U . . .
H20B H 0.437553 0.936140 0.428454 0.102 Uiso 1 1 calc R U . . .
H20C H 0.403773 1.037890 0.422672 0.102 Uiso 1 1 calc R U . . .
C16 C 0.3689(8) 0.1732(4) 0.2418(4) 0.0664(17) Uani 1 1 d . . . . .
H16A H 0.318329 0.185863 0.196187 0.100 Uiso 1 1 calc R U . . .
H16B H 0.299300 0.164215 0.296577 0.100 Uiso 1 1 calc R U . . .
H16C H 0.442157 0.121732 0.230049 0.100 Uiso 1 1 calc R U . . .
C28 C -0.3014(7) 0.9776(5) 1.0277(4) 0.0683(18) Uani 1 1 d . . . . .
H28A H -0.236480 0.928570 1.045858 0.103 Uiso 1 1 calc R U . . .
H28B H -0.402007 0.970368 1.052632 0.103 Uiso 1 1 calc R U . . .
H28C H -0.285389 1.029598 1.047009 0.103 Uiso 1 1 calc R U . . .
C24 C 0.1274(8) 1.2803(4) 0.7541(4) 0.0691(18) Uani 1 1 d . . . . .
H24A H 0.127202 1.297336 0.694427 0.104 Uiso 1 1 calc R U . . .
H24B H 0.184860 1.314224 0.773105 0.104 Uiso 1 1 calc R U . . .
H24C H 0.027967 1.289650 0.789868 0.104 Uiso 1 1 calc R U . . .
C8 C 0.3776(8) 0.8116(4) 0.2571(5) 0.0720(19) Uani 1 1 d . . . . .
H8A H 0.337383 0.826216 0.207243 0.108 Uiso 1 1 calc R U . . .
H8B H 0.448798 0.847720 0.254717 0.108 Uiso 1 1 calc R U . . .
H8C H 0.299586 0.820763 0.309395 0.108 Uiso 1 1 calc R U . . .
C4 C 0.2377(9) 0.5312(5) -0.0357(4) 0.075(2) Uani 1 1 d . . . . .
H4A H 0.161031 0.535718 -0.065259 0.112 Uiso 1 1 calc R U . . .
H4B H 0.307679 0.478827 -0.050236 0.112 Uiso 1 1 calc R U . . .
H4C H 0.286796 0.580326 -0.053529 0.112 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I5 I4 2.9070(6) . ?
I5 I6 2.9371(6) . ?
I2 I1 2.9491(6) . ?
I2 I3 2.8848(6) . ?
N007 C25 1.515(6) . ?
N007 C21 1.513(6) . ?
N007 C17 1.522(6) . ?
N007 C29 1.526(6) . ?
N008 C9 1.525(6) . ?
N008 C1 1.514(6) . ?
N008 C5 1.514(6) . ?
N008 C13 1.527(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.511(7) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.514(7) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.521(7) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C22 1.513(7) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.504(7) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.518(7) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.509(7) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C30 1.505(7) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 C27 1.518(8) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.511(8) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.514(7) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.513(8) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.523(8) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C19 1.521(7) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C14 1.509(7) . ?
C15 C16 1.522(8) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C30 1.522(7) . ?
C31 C32 1.514(8) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.503(8) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.515(8) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.517(8) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C12 C11 1.518(8) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.504(8) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.509(8) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I4 I5 I6 174.726(18) . . ?
I3 I2 I1 178.450(19) . . ?
C25 N007 C17 107.2(4) . . ?
C25 N007 C29 109.9(4) . . ?
C21 N007 C25 110.7(4) . . ?
C21 N007 C17 110.7(4) . . ?
C21 N007 C29 107.9(4) . . ?
C17 N007 C29 110.5(4) . . ?
C9 N008 C13 110.1(4) . . ?
C1 N008 C9 106.9(4) . . ?
C1 N008 C13 110.9(4) . . ?
C5 N008 C9 110.7(4) . . ?
C5 N008 C1 110.9(4) . . ?
C5 N008 C13 107.3(4) . . ?
N008 C9 H9A 108.2 . . ?
N008 C9 H9B 108.2 . . ?
H9A C9 H9B 107.4 . . ?
C10 C9 N008 116.3(4) . . ?
C10 C9 H9A 108.2 . . ?
C10 C9 H9B 108.2 . . ?
N007 C25 H25A 108.4 . . ?
N007 C25 H25B 108.4 . . ?
H25A C25 H25B 107.4 . . ?
C26 C25 N007 115.6(4) . . ?
C26 C25 H25A 108.4 . . ?
C26 C25 H25B 108.4 . . ?
N008 C1 H1A 108.4 . . ?
N008 C1 H1B 108.4 . . ?
N008 C1 C2 115.7(4) . . ?
H1A C1 H1B 107.4 . . ?
C2 C1 H1A 108.4 . . ?
C2 C1 H1B 108.4 . . ?
N007 C21 H21A 108.4 . . ?
N007 C21 H21B 108.4 . . ?
N007 C21 C22 115.6(4) . . ?
H21A C21 H21B 107.4 . . ?
C22 C21 H21A 108.4 . . ?
C22 C21 H21B 108.4 . . ?
N007 C17 H17A 108.4 . . ?
N007 C17 H17B 108.4 . . ?
H17A C17 H17B 107.4 . . ?
C18 C17 N007 115.7(4) . . ?
C18 C17 H17A 108.4 . . ?
C18 C17 H17B 108.4 . . ?
N008 C5 H5A 108.4 . . ?
N008 C5 H5B 108.4 . . ?
N008 C5 C6 115.5(4) . . ?
H5A C5 H5B 107.5 . . ?
C6 C5 H5A 108.4 . . ?
C6 C5 H5B 108.4 . . ?
N008 C13 H13A 108.1 . . ?
N008 C13 H13B 108.1 . . ?
H13A C13 H13B 107.3 . . ?
C14 C13 N008 116.9(4) . . ?
C14 C13 H13A 108.1 . . ?
C14 C13 H13B 108.1 . . ?
N007 C29 H29A 108.3 . . ?
N007 C29 H29B 108.3 . . ?
H29A C29 H29B 107.4 . . ?
C30 C29 N007 115.7(4) . . ?
C30 C29 H29A 108.3 . . ?
C30 C29 H29B 108.3 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 C27 110.7(4) . . ?
H26A C26 H26B 108.1 . . ?
C27 C26 H26A 109.5 . . ?
C27 C26 H26B 109.5 . . ?
C21 C22 H22A 109.2 . . ?
C21 C22 H22B 109.2 . . ?
H22A C22 H22B 107.9 . . ?
C23 C22 C21 112.1(5) . . ?
C23 C22 H22A 109.2 . . ?
C23 C22 H22B 109.2 . . ?
C9 C10 H10A 109.4 . . ?
C9 C10 H10B 109.4 . . ?
C9 C10 C11 111.0(4) . . ?
H10A C10 H10B 108.0 . . ?
C11 C10 H10A 109.4 . . ?
C11 C10 H10B 109.4 . . ?
C1 C2 H2A 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
C3 C2 C1 109.8(5) . . ?
C3 C2 H2A 109.7 . . ?
C3 C2 H2B 109.7 . . ?
C5 C6 H6A 109.4 . . ?
C5 C6 H6B 109.4 . . ?
C5 C6 C7 111.2(5) . . ?
H6A C6 H6B 108.0 . . ?
C7 C6 H6A 109.4 . . ?
C7 C6 H6B 109.4 . . ?
C17 C18 H18A 109.3 . . ?
C17 C18 H18B 109.3 . . ?
C17 C18 C19 111.4(5) . . ?
H18A C18 H18B 108.0 . . ?
C19 C18 H18A 109.3 . . ?
C19 C18 H18B 109.3 . . ?
H15A C15 H15B 107.9 . . ?
C14 C15 H15A 109.2 . . ?
C14 C15 H15B 109.2 . . ?
C14 C15 C16 112.0(5) . . ?
C16 C15 H15A 109.2 . . ?
C16 C15 H15B 109.2 . . ?
H31A C31 H31B 108.0 . . ?
C30 C31 H31A 109.3 . . ?
C30 C31 H31B 109.3 . . ?
C32 C31 H31A 109.3 . . ?
C32 C31 H31B 109.3 . . ?
C32 C31 C30 111.7(5) . . ?
C13 C14 C15 111.2(4) . . ?
C13 C14 H14A 109.4 . . ?
C13 C14 H14B 109.4 . . ?
C15 C14 H14A 109.4 . . ?
C15 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C29 C30 C31 111.3(4) . . ?
C29 C30 H30A 109.4 . . ?
C29 C30 H30B 109.4 . . ?
C31 C30 H30A 109.4 . . ?
C31 C30 H30B 109.4 . . ?
H30A C30 H30B 108.0 . . ?
C18 C19 H19A 108.9 . . ?
C18 C19 H19B 108.9 . . ?
H19A C19 H19B 107.7 . . ?
C20 C19 C18 113.4(5) . . ?
C20 C19 H19A 108.9 . . ?
C20 C19 H19B 108.9 . . ?
C26 C27 H27A 109.1 . . ?
C26 C27 H27B 109.1 . . ?
H27A C27 H27B 107.8 . . ?
C28 C27 C26 112.4(5) . . ?
C28 C27 H27A 109.1 . . ?
C28 C27 H27B 109.1 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
C8 C7 C6 110.8(5) . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
C22 C23 H23A 109.1 . . ?
C22 C23 H23B 109.1 . . ?
H23A C23 H23B 107.8 . . ?
C24 C23 C22 112.6(5) . . ?
C24 C23 H23A 109.1 . . ?
C24 C23 H23B 109.1 . . ?
C10 C11 C12 112.3(5) . . ?
C10 C11 H11A 109.1 . . ?
C10 C11 H11B 109.1 . . ?
C12 C11 H11A 109.1 . . ?
C12 C11 H11B 109.1 . . ?
H11A C11 H11B 107.9 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C2 C3 H3A 109.1 . . ?
C2 C3 H3B 109.1 . . ?
H3A C3 H3B 107.9 . . ?
C4 C3 C2 112.4(5) . . ?
C4 C3 H3A 109.1 . . ?
C4 C3 H3B 109.1 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 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
N007 C25 C26 C27 -177.7(5) . . . . ?
N007 C21 C22 C23 -175.1(5) . . . . ?
N007 C17 C18 C19 173.1(4) . . . . ?
N007 C29 C30 C31 179.7(4) . . . . ?
N008 C9 C10 C11 -175.2(4) . . . . ?
N008 C1 C2 C3 174.9(5) . . . . ?
N008 C5 C6 C7 171.0(4) . . . . ?
N008 C13 C14 C15 -175.2(4) . . . . ?
C9 N008 C1 C2 -179.3(4) . . . . ?
C9 N008 C5 C6 -60.5(5) . . . . ?
C9 N008 C13 C14 70.1(5) . . . . ?
C9 C10 C11 C12 174.8(5) . . . . ?
C25 N007 C21 C22 -57.7(5) . . . . ?
C25 N007 C17 C18 171.8(4) . . . . ?
C25 N007 C29 C30 53.3(5) . . . . ?
C25 C26 C27 C28 -177.9(5) . . . . ?
C1 N008 C9 C10 -171.4(4) . . . . ?
C1 N008 C5 C6 58.0(5) . . . . ?
C1 N008 C13 C14 -47.9(5) . . . . ?
C1 C2 C3 C4 178.8(5) . . . . ?
C21 N007 C25 C26 -59.8(5) . . . . ?
C21 N007 C17 C18 51.0(6) . . . . ?
C21 N007 C29 C30 174.1(4) . . . . ?
C21 C22 C23 C24 -176.2(5) . . . . ?
C17 N007 C25 C26 179.4(4) . . . . ?
C17 N007 C21 C22 61.1(5) . . . . ?
C17 N007 C29 C30 -64.8(5) . . . . ?
C17 C18 C19 C20 179.5(5) . . . . ?
C5 N008 C9 C10 -50.5(6) . . . . ?
C5 N008 C1 C2 59.9(6) . . . . ?
C5 N008 C13 C14 -169.3(4) . . . . ?
C5 C6 C7 C8 173.8(5) . . . . ?
C13 N008 C9 C10 68.0(5) . . . . ?
C13 N008 C1 C2 -59.3(6) . . . . ?
C13 N008 C5 C6 179.3(4) . . . . ?
C29 N007 C25 C26 59.3(5) . . . . ?
C29 N007 C21 C22 -177.9(4) . . . . ?
C29 N007 C17 C18 -68.5(5) . . . . ?
C32 C31 C30 C29 -179.9(5) . . . . ?
C16 C15 C14 C13 -178.9(4) . . . . ?

_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 1.677
_oxdiff_exptl_absorpt_empirical_full_min 0.581
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Ethanol'
_chemical_properties_physical    Light-sensitive,Photo-sensitive
####################################################################### 
# 
# 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_ethac_autored
_database_code_depnum_ccdc_archive 'CCDC 2350026'
loop_
_audit_author_name
_audit_author_address
'Toshio Naito'
;Ehime University
Japan
;
_audit_update_record             
;
2024-04-22 deposited with the CCDC.	2025-05-30 downloaded from the CCDC.
;
_audit_creation_date             2024-04-22
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        (EtHAC)2I3
_chemical_formula_moiety         'I3, 2(C50 H52 N6)'
_chemical_formula_sum            'C100 H104 I3 N12'
_chemical_formula_weight         1854.65
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C100 H104 N14 I3'
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'
I I -0.4742 1.8119 '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      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                   9.6300(2)
_cell_length_b                   14.6686(4)
_cell_length_c                   15.6386(4)
_cell_angle_alpha                105.469(2)
_cell_angle_beta                 99.439(2)
_cell_angle_gamma                104.391(2)
_cell_volume                     1998.52(9)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    21552
_cell_measurement_temperature    90
_cell_measurement_theta_max      31.3310
_cell_measurement_theta_min      1.7480
_shelx_estimated_absorpt_T_max   0.913
_shelx_estimated_absorpt_T_min   0.625
_exptl_absorpt_coefficient_mu    1.233
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             947
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.075
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33728
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         2.253
_diffrn_ambient_temperature      90
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 7.111
_diffrn_detector_type            'Rigaku Saturn724+ area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50    1.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50    1.00    --  -20.00  45.00  90.00  360
  3  ω   -110.00  70.00   0.50    1.00    --  -20.00  45.00 180.00  360
  4  ω   -110.00  70.00   0.50    1.00    --  -20.00  45.00 270.00  360
;
_diffrn_measurement_device       'AFC11 SATURN724+ Right'
_diffrn_measurement_device_type  'Rigaku Varimax with Saturn'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0371325000
_diffrn_orient_matrix_UB_12      -0.0299244000
_diffrn_orient_matrix_UB_13      -0.0247465000
_diffrn_orient_matrix_UB_21      0.0470748000
_diffrn_orient_matrix_UB_22      0.0427969000
_diffrn_orient_matrix_UB_23      -0.0051030000
_diffrn_orient_matrix_UB_31      0.0506163000
_diffrn_orient_matrix_UB_32      0.0072775000
_diffrn_orient_matrix_UB_33      0.0414701000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'MicroMax 007'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7650
_reflns_number_total             9640
_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 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b46 (Rigaku, 2016)'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.413
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         9640
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0477
_refine_ls_restrained_S_all      1.076
_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)+(0.0525P)²+2.9046P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1119
_refine_ls_wR_factor_ref         0.1186
_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 Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C33(H33A,H33B), C35(H35A,H35B), C37(H37A,H37B), C39(H39A,
 H39B), C41(H41A,H41B), C43(H43A,H43B), C45(H45A,H45B), C47(H47A,H47B),
 C49(H49A,H49B)
2.b Aromatic/amide H refined with riding coordinates:
 C28(H28), C29(H29)
2.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C38(H38A,H38B,
 H38C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C46(H46A,
 H46B,H46C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C)
;
_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
I1 I 1.000000 0.000000 0.000000 0.03601(11) Uani 1 2 d S . P . .
I2 I 0.96503(3) 0.16559(2) -0.06350(2) 0.04270(10) Uani 1 1 d . . . . .
N1 N 0.6419(3) 0.65294(16) 0.52854(15) 0.0108(4) Uani 1 1 d . . . . .
N2 N 0.5304(3) 0.51489(16) 0.35784(15) 0.0106(4) Uani 1 1 d . . . . .
N3 N 0.6327(2) 0.35416(16) 0.31227(15) 0.0096(4) Uani 1 1 d . . . . .
N4 N 0.8359(3) 0.32783(16) 0.44053(15) 0.0098(4) Uani 1 1 d . . . . .
N5 N 0.9402(2) 0.46357(16) 0.61242(15) 0.0098(4) Uani 1 1 d . . . . .
N6 N 0.8455(3) 0.62674(16) 0.65481(15) 0.0097(4) Uani 1 1 d . . . . .
C1 C 0.6885(3) 0.57145(19) 0.50642(18) 0.0099(5) Uani 1 1 d . . . . .
C2 C 0.6345(3) 0.50263(19) 0.42035(18) 0.0100(5) Uani 1 1 d . . . . .
C3 C 0.6860(3) 0.42255(19) 0.39760(17) 0.0092(5) Uani 1 1 d . . . . .
C4 C 0.7883(3) 0.40935(19) 0.46166(18) 0.0099(5) Uani 1 1 d . . . . .
C5 C 0.8408(3) 0.47710(19) 0.54777(18) 0.0104(5) Uani 1 1 d . . . . .
C6 C 0.7921(3) 0.55853(19) 0.56980(18) 0.0098(5) Uani 1 1 d . . . . .
C7 C 0.6934(3) 0.72515(19) 0.61435(18) 0.0117(5) Uani 1 1 d . . . . .
C8 C 0.6196(3) 0.7948(2) 0.60911(19) 0.0126(5) Uani 1 1 d . . . . .
C9 C 0.5249(3) 0.7638(2) 0.51987(19) 0.0138(6) Uani 1 1 d . . . . .
C10 C 0.5392(3) 0.6729(2) 0.46791(19) 0.0115(5) Uani 1 1 d . . . . .
C11 C 0.4796(3) 0.59838(19) 0.37496(19) 0.0117(5) Uani 1 1 d . . . . .
C12 C 0.3839(3) 0.5841(2) 0.29156(19) 0.0131(5) Uani 1 1 d . . . . .
C13 C 0.3788(3) 0.4928(2) 0.22682(19) 0.0132(5) Uani 1 1 d . . . . .
C14 C 0.4718(3) 0.44881(19) 0.26853(18) 0.0113(5) Uani 1 1 d . . . . .
C15 C 0.5209(3) 0.35938(19) 0.24565(18) 0.0113(5) Uani 1 1 d . . . . .
C16 C 0.4887(3) 0.2704(2) 0.17376(19) 0.0141(6) Uani 1 1 d . . . . .
C17 C 0.5800(3) 0.2141(2) 0.19867(19) 0.0144(6) Uani 1 1 d . . . . .
C18 C 0.6718(3) 0.26671(19) 0.28667(18) 0.0111(5) Uani 1 1 d . . . . .
C19 C 0.7832(3) 0.25356(19) 0.35555(18) 0.0119(5) Uani 1 1 d . . . . .
C20 C 0.8560(3) 0.1837(2) 0.36359(19) 0.0126(5) Uani 1 1 d . . . . .
C21 C 0.9502(3) 0.21753(19) 0.45378(19) 0.0121(5) Uani 1 1 d . . . . .
C22 C 0.9381(3) 0.30892(19) 0.50351(18) 0.0101(5) Uani 1 1 d . . . . .
C23 C 0.9963(3) 0.38296(19) 0.59617(18) 0.0102(5) Uani 1 1 d . . . . .
C24 C 1.0982(3) 0.4018(2) 0.67996(19) 0.0122(5) Uani 1 1 d . . . . .
C25 C 1.0993(3) 0.4930(2) 0.74300(18) 0.0124(5) Uani 1 1 d . . . . .
C26 C 0.9998(3) 0.53121(19) 0.69997(18) 0.0114(5) Uani 1 1 d . . . . .
C27 C 0.9488(3) 0.6184(2) 0.72313(18) 0.0112(5) Uani 1 1 d . . . . .
C28 C 0.9718(3) 0.7024(2) 0.79827(19) 0.0148(6) Uani 1 1 d . . . . .
H28 H 1.036764 0.718777 0.856617 0.018 Uiso 1 1 calc R U . . .
C29 C 0.8828(3) 0.7587(2) 0.77319(19) 0.0153(6) Uani 1 1 d . . . . .
H29 H 0.878292 0.819393 0.812061 0.018 Uiso 1 1 calc R U . . .
C30 C 0.8028(3) 0.71165(19) 0.68268(19) 0.0127(5) Uani 1 1 d . . . . .
C31 C 0.6412(3) 0.8886(2) 0.6858(2) 0.0164(6) Uani 1 1 d . . . . .
H31A H 0.674232 0.878173 0.744799 0.020 Uiso 1 1 calc R U . . .
H31B H 0.544751 0.901253 0.684491 0.020 Uiso 1 1 calc R U . . .
C32 C 0.7530(3) 0.9804(2) 0.6815(2) 0.0198(6) Uani 1 1 d . . . . .
H32A H 0.721328 0.991685 0.623456 0.030 Uiso 1 1 calc R U . . .
H32B H 0.850339 0.970080 0.685925 0.030 Uiso 1 1 calc R U . . .
H32C H 0.759281 1.038382 0.732548 0.030 Uiso 1 1 calc R U . . .
C33 C 0.4340(4) 0.8241(2) 0.4892(2) 0.0190(6) Uani 1 1 d . . . . .
H33A H 0.422072 0.871750 0.543579 0.023 Uiso 1 1 calc R U . . .
H33B H 0.334402 0.779386 0.453218 0.023 Uiso 1 1 calc R U . . .
C34 C 0.5061(4) 0.8813(2) 0.4306(2) 0.0221(7) Uani 1 1 d . . . . .
H34A H 0.529983 0.835486 0.381237 0.033 Uiso 1 1 calc R U . . .
H34B H 0.596917 0.933473 0.468963 0.033 Uiso 1 1 calc R U . . .
H34C H 0.437307 0.911656 0.404276 0.033 Uiso 1 1 calc R U . . .
C35 C 0.2984(3) 0.6513(2) 0.2686(2) 0.0183(6) Uani 1 1 d . . . . .
H35A H 0.300095 0.700805 0.326237 0.022 Uiso 1 1 calc R U . . .
H35B H 0.194000 0.610958 0.239079 0.022 Uiso 1 1 calc R U . . .
C36 C 0.3581(4) 0.7064(2) 0.2052(2) 0.0281(8) Uani 1 1 d . . . . .
H36A H 0.346155 0.658279 0.145286 0.042 Uiso 1 1 calc R U . . .
H36B H 0.463254 0.743238 0.231962 0.042 Uiso 1 1 calc R U . . .
H36C H 0.303170 0.752901 0.197786 0.042 Uiso 1 1 calc R U . . .
C37 C 0.2891(3) 0.4568(2) 0.12920(19) 0.0168(6) Uani 1 1 d . . . . .
H37A H 0.220416 0.496275 0.123286 0.020 Uiso 1 1 calc R U . . .
H37B H 0.229057 0.386500 0.113393 0.020 Uiso 1 1 calc R U . . .
C38 C 0.3861(4) 0.4654(3) 0.0619(2) 0.0226(7) Uani 1 1 d . . . . .
H38A H 0.323861 0.436962 -0.000843 0.034 Uiso 1 1 calc R U . . .
H38B H 0.457647 0.429192 0.069606 0.034 Uiso 1 1 calc R U . . .
H38C H 0.439033 0.535584 0.073723 0.034 Uiso 1 1 calc R U . . .
C39 C 0.3690(3) 0.2325(2) 0.0862(2) 0.0198(6) Uani 1 1 d . . . . .
H39A H 0.307033 0.277425 0.090328 0.024 Uiso 1 1 calc R U . . .
H39B H 0.305089 0.166193 0.081527 0.024 Uiso 1 1 calc R U . . .
C40 C 0.4213(4) 0.2235(3) -0.0022(2) 0.0311(8) Uani 1 1 d . . . . .
H40A H 0.340161 0.218948 -0.051613 0.047 Uiso 1 1 calc R U . . .
H40B H 0.452280 0.163691 -0.018807 0.047 Uiso 1 1 calc R U . . .
H40C H 0.505017 0.282193 0.007225 0.047 Uiso 1 1 calc R U . . .
C41 C 0.5653(3) 0.1106(2) 0.1409(2) 0.0191(6) Uani 1 1 d . . . . .
H41A H 0.462779 0.079503 0.102396 0.023 Uiso 1 1 calc R U . . .
H41B H 0.581311 0.071100 0.181934 0.023 Uiso 1 1 calc R U . . .
C42 C 0.6719(4) 0.1047(3) 0.0789(2) 0.0256(7) Uani 1 1 d . . . . .
H42A H 0.651579 0.138831 0.034489 0.038 Uiso 1 1 calc R U . . .
H42B H 0.658607 0.034901 0.046346 0.038 Uiso 1 1 calc R U . . .
H42C H 0.773822 0.136710 0.116065 0.038 Uiso 1 1 calc R U . . .
C43 C 0.8435(3) 0.0882(2) 0.2920(2) 0.0166(6) Uani 1 1 d . . . . .
H43A H 0.943082 0.080032 0.295944 0.020 Uiso 1 1 calc R U . . .
H43B H 0.808343 0.093136 0.230763 0.020 Uiso 1 1 calc R U . . .
C44 C 0.7386(4) -0.0045(2) 0.3010(2) 0.0233(7) Uani 1 1 d . . . . .
H44A H 0.732209 -0.063071 0.250610 0.035 Uiso 1 1 calc R U . . .
H44B H 0.640101 0.003473 0.298617 0.035 Uiso 1 1 calc R U . . .
H44C H 0.776535 -0.012968 0.359519 0.035 Uiso 1 1 calc R U . . .
C45 C 1.0392(3) 0.1585(2) 0.4896(2) 0.0158(6) Uani 1 1 d . . . . .
H45A H 1.141073 0.202396 0.521612 0.019 Uiso 1 1 calc R U . . .
H45B H 1.045174 0.104749 0.437763 0.019 Uiso 1 1 calc R U . . .
C46 C 0.9687(4) 0.1132(2) 0.5559(2) 0.0203(6) Uani 1 1 d . . . . .
H46A H 0.875394 0.061058 0.521914 0.030 Uiso 1 1 calc R U . . .
H46B H 0.949483 0.165117 0.602338 0.030 Uiso 1 1 calc R U . . .
H46C H 1.036248 0.084528 0.585852 0.030 Uiso 1 1 calc R U . . .
C47 C 1.1948(3) 0.3421(2) 0.70512(19) 0.0152(6) Uani 1 1 d . . . . .
H47A H 1.298160 0.386361 0.730201 0.018 Uiso 1 1 calc R U . . .
H47B H 1.191964 0.290062 0.648913 0.018 Uiso 1 1 calc R U . . .
C48 C 1.1499(4) 0.2926(2) 0.7751(2) 0.0228(7) Uani 1 1 d . . . . .
H48A H 1.046725 0.250238 0.751799 0.034 Uiso 1 1 calc R U . . .
H48B H 1.160543 0.343822 0.832868 0.034 Uiso 1 1 calc R U . . .
H48C H 1.213785 0.251992 0.785542 0.034 Uiso 1 1 calc R U . . .
C49 C 1.1939(3) 0.5435(2) 0.83912(19) 0.0153(6) Uani 1 1 d . . . . .
H49A H 1.240841 0.614330 0.847017 0.018 Uiso 1 1 calc R U . . .
H49B H 1.273868 0.513009 0.847769 0.018 Uiso 1 1 calc R U . . .
C50 C 1.1095(3) 0.5373(2) 0.9139(2) 0.0201(6) Uani 1 1 d . . . . .
H50A H 1.061101 0.467461 0.906169 0.030 Uiso 1 1 calc R U . . .
H50B H 1.034617 0.571539 0.908790 0.030 Uiso 1 1 calc R U . . .
H50C H 1.179009 0.569090 0.974281 0.030 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 I2 2.9296(3) 2_755 ?
I1 I2 2.9296(3) . ?
N1 C1 1.359(3) . ?
N1 C7 1.390(3) . ?
N1 C10 1.395(3) . ?
N2 C2 1.362(3) . ?
N2 C11 1.406(3) . ?
N2 C14 1.399(3) . ?
N3 C3 1.362(3) . ?
N3 C15 1.402(3) . ?
N3 C18 1.401(3) . ?
N4 C4 1.364(3) . ?
N4 C19 1.394(3) . ?
N4 C22 1.407(3) . ?
N5 C5 1.365(3) . ?
N5 C23 1.399(3) . ?
N5 C26 1.387(3) . ?
N6 C6 1.358(3) . ?
N6 C27 1.389(3) . ?
N6 C30 1.391(3) . ?
C1 C2 1.373(4) . ?
C1 C6 1.372(4) . ?
C2 C3 1.370(4) . ?
C3 C4 1.374(4) . ?
C4 C5 1.367(4) . ?
C5 C6 1.370(4) . ?
C7 C8 1.393(4) . ?
C7 C30 1.463(4) . ?
C8 C9 1.423(4) . ?
C8 C31 1.507(4) . ?
C9 C10 1.417(4) . ?
C9 C33 1.501(4) . ?
C10 C11 1.484(4) . ?
C11 C12 1.400(4) . ?
C12 C13 1.432(4) . ?
C12 C35 1.507(4) . ?
C13 C14 1.401(4) . ?
C13 C37 1.506(4) . ?
C14 C15 1.479(4) . ?
C15 C16 1.402(4) . ?
C16 C17 1.424(4) . ?
C16 C39 1.507(4) . ?
C17 C18 1.402(4) . ?
C17 C41 1.503(4) . ?
C18 C19 1.477(4) . ?
C19 C20 1.398(4) . ?
C20 C21 1.429(4) . ?
C20 C43 1.505(4) . ?
C21 C22 1.402(4) . ?
C21 C45 1.506(4) . ?
C22 C23 1.478(4) . ?
C23 C24 1.416(4) . ?
C24 C25 1.431(4) . ?
C24 C47 1.502(4) . ?
C25 C26 1.393(4) . ?
C25 C49 1.503(4) . ?
C26 C27 1.459(4) . ?
C27 C28 1.398(4) . ?
C28 H28 0.9500 . ?
C28 C29 1.410(4) . ?
C29 H29 0.9500 . ?
C29 C30 1.389(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.525(4) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.535(4) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.534(4) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.527(4) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.532(4) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.526(4) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.534(4) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.533(4) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C47 C48 1.528(4) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C49 C50 1.538(4) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?

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
I2 I1 I2 180.0 2_755 . ?
C1 N1 C7 122.8(2) . . ?
C1 N1 C10 123.7(2) . . ?
C7 N1 C10 113.4(2) . . ?
C2 N2 C11 123.2(2) . . ?
C2 N2 C14 122.9(2) . . ?
C14 N2 C11 113.8(2) . . ?
C3 N3 C15 122.7(2) . . ?
C3 N3 C18 123.1(2) . . ?
C18 N3 C15 113.8(2) . . ?
C4 N4 C19 123.0(2) . . ?
C4 N4 C22 123.2(2) . . ?
C19 N4 C22 113.8(2) . . ?
C5 N5 C23 123.7(2) . . ?
C5 N5 C26 122.7(2) . . ?
C26 N5 C23 113.5(2) . . ?
C6 N6 C27 123.1(2) . . ?
C6 N6 C30 123.9(2) . . ?
C27 N6 C30 113.1(2) . . ?
N1 C1 C2 120.4(2) . . ?
N1 C1 C6 120.0(2) . . ?
C6 C1 C2 119.7(2) . . ?
N2 C2 C1 119.6(2) . . ?
N2 C2 C3 120.4(2) . . ?
C3 C2 C1 120.0(2) . . ?
N3 C3 C2 120.2(2) . . ?
N3 C3 C4 119.7(2) . . ?
C2 C3 C4 120.1(2) . . ?
N4 C4 C3 120.4(2) . . ?
N4 C4 C5 119.6(2) . . ?
C5 C4 C3 120.0(2) . . ?
N5 C5 C4 120.4(2) . . ?
N5 C5 C6 119.7(2) . . ?
C4 C5 C6 119.9(2) . . ?
N6 C6 C1 119.5(2) . . ?
N6 C6 C5 120.1(2) . . ?
C5 C6 C1 120.3(2) . . ?
N1 C7 C8 105.0(2) . . ?
N1 C7 C30 117.7(2) . . ?
C8 C7 C30 137.3(3) . . ?
C7 C8 C9 109.0(2) . . ?
C7 C8 C31 124.7(3) . . ?
C9 C8 C31 126.3(2) . . ?
C8 C9 C33 123.1(2) . . ?
C10 C9 C8 108.6(2) . . ?
C10 C9 C33 128.2(3) . . ?
N1 C10 C9 104.0(2) . . ?
N1 C10 C11 116.1(2) . . ?
C9 C10 C11 139.9(3) . . ?
N2 C11 C10 116.9(2) . . ?
C12 C11 N2 104.0(2) . . ?
C12 C11 C10 139.1(2) . . ?
C11 C12 C13 108.9(2) . . ?
C11 C12 C35 127.9(3) . . ?
C13 C12 C35 123.2(2) . . ?
C12 C13 C37 122.4(2) . . ?
C14 C13 C12 109.3(2) . . ?
C14 C13 C37 128.2(3) . . ?
N2 C14 C13 104.0(2) . . ?
N2 C14 C15 116.7(2) . . ?
C13 C14 C15 139.4(3) . . ?
N3 C15 C14 116.8(2) . . ?
N3 C15 C16 103.9(2) . . ?
C16 C15 C14 139.3(3) . . ?
C15 C16 C17 109.3(2) . . ?
C15 C16 C39 127.3(3) . . ?
C17 C16 C39 123.2(2) . . ?
C16 C17 C41 123.4(3) . . ?
C18 C17 C16 109.2(2) . . ?
C18 C17 C41 127.2(3) . . ?
N3 C18 C17 103.9(2) . . ?
N3 C18 C19 116.8(2) . . ?
C17 C18 C19 139.2(2) . . ?
N4 C19 C18 116.9(2) . . ?
N4 C19 C20 104.6(2) . . ?
C20 C19 C18 138.5(2) . . ?
C19 C20 C21 108.6(2) . . ?
C19 C20 C43 128.0(3) . . ?
C21 C20 C43 123.3(2) . . ?
C20 C21 C45 123.9(2) . . ?
C22 C21 C20 109.6(2) . . ?
C22 C21 C45 126.4(2) . . ?
N4 C22 C23 117.1(2) . . ?
C21 C22 N4 103.4(2) . . ?
C21 C22 C23 139.5(2) . . ?
N5 C23 C22 116.0(2) . . ?
N5 C23 C24 104.0(2) . . ?
C24 C23 C22 140.1(2) . . ?
C23 C24 C25 108.5(2) . . ?
C23 C24 C47 129.4(3) . . ?
C25 C24 C47 122.1(2) . . ?
C24 C25 C49 127.0(3) . . ?
C26 C25 C24 108.8(2) . . ?
C26 C25 C49 124.2(2) . . ?
N5 C26 C25 105.2(2) . . ?
N5 C26 C27 117.5(2) . . ?
C25 C26 C27 137.3(2) . . ?
N6 C27 C26 116.9(2) . . ?
N6 C27 C28 104.4(2) . . ?
C28 C27 C26 138.7(3) . . ?
C27 C28 H28 125.6 . . ?
C27 C28 C29 108.8(2) . . ?
C29 C28 H28 125.6 . . ?
C28 C29 H29 125.4 . . ?
C30 C29 C28 109.3(2) . . ?
C30 C29 H29 125.4 . . ?
N6 C30 C7 116.1(2) . . ?
C29 C30 N6 104.5(2) . . ?
C29 C30 C7 139.4(2) . . ?
C8 C31 H31A 108.7 . . ?
C8 C31 H31B 108.7 . . ?
C8 C31 C32 114.3(2) . . ?
H31A C31 H31B 107.6 . . ?
C32 C31 H31A 108.7 . . ?
C32 C31 H31B 108.7 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C9 C33 H33A 109.3 . . ?
C9 C33 H33B 109.3 . . ?
C9 C33 C34 111.7(2) . . ?
H33A C33 H33B 107.9 . . ?
C34 C33 H33A 109.3 . . ?
C34 C33 H33B 109.3 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C12 C35 H35A 108.7 . . ?
C12 C35 H35B 108.7 . . ?
C12 C35 C36 114.0(3) . . ?
H35A C35 H35B 107.6 . . ?
C36 C35 H35A 108.7 . . ?
C36 C35 H35B 108.7 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C13 C37 H37A 109.1 . . ?
C13 C37 H37B 109.1 . . ?
C13 C37 C38 112.3(2) . . ?
H37A C37 H37B 107.9 . . ?
C38 C37 H37A 109.1 . . ?
C38 C37 H37B 109.1 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C16 C39 H39A 108.3 . . ?
C16 C39 H39B 108.3 . . ?
C16 C39 C40 116.1(3) . . ?
H39A C39 H39B 107.4 . . ?
C40 C39 H39A 108.3 . . ?
C40 C39 H39B 108.3 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C17 C41 H41A 108.6 . . ?
C17 C41 H41B 108.6 . . ?
C17 C41 C42 114.8(3) . . ?
H41A C41 H41B 107.6 . . ?
C42 C41 H41A 108.6 . . ?
C42 C41 H41B 108.6 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C20 C43 H43A 108.7 . . ?
C20 C43 H43B 108.7 . . ?
C20 C43 C44 114.0(2) . . ?
H43A C43 H43B 107.6 . . ?
C44 C43 H43A 108.7 . . ?
C44 C43 H43B 108.7 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C21 C45 H45A 109.4 . . ?
C21 C45 H45B 109.4 . . ?
C21 C45 C46 110.9(2) . . ?
H45A C45 H45B 108.0 . . ?
C46 C45 H45A 109.4 . . ?
C46 C45 H45B 109.4 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C24 C47 H47A 108.8 . . ?
C24 C47 H47B 108.8 . . ?
C24 C47 C48 113.9(2) . . ?
H47A C47 H47B 107.7 . . ?
C48 C47 H47A 108.8 . . ?
C48 C47 H47B 108.8 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C25 C49 H49A 108.7 . . ?
C25 C49 H49B 108.7 . . ?
C25 C49 C50 114.3(2) . . ?
H49A C49 H49B 107.6 . . ?
C50 C49 H49A 108.7 . . ?
C50 C49 H49B 108.7 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 N2 -1.9(4) . . . . ?
N1 C1 C2 C3 177.7(2) . . . . ?
N1 C1 C6 N6 1.0(4) . . . . ?
N1 C1 C6 C5 -179.4(2) . . . . ?
N1 C7 C8 C9 -0.3(3) . . . . ?
N1 C7 C8 C31 -178.9(2) . . . . ?
N1 C7 C30 N6 0.0(4) . . . . ?
N1 C7 C30 C29 -179.0(3) . . . . ?
N1 C10 C11 N2 1.0(4) . . . . ?
N1 C10 C11 C12 -177.1(3) . . . . ?
N2 C2 C3 N3 -0.4(4) . . . . ?
N2 C2 C3 C4 -178.4(2) . . . . ?
N2 C11 C12 C13 0.3(3) . . . . ?
N2 C11 C12 C35 -179.0(3) . . . . ?
N2 C14 C15 N3 -6.4(4) . . . . ?
N2 C14 C15 C16 172.6(3) . . . . ?
N3 C3 C4 N4 -0.5(4) . . . . ?
N3 C3 C4 C5 -179.2(2) . . . . ?
N3 C15 C16 C17 0.3(3) . . . . ?
N3 C15 C16 C39 175.4(3) . . . . ?
N3 C18 C19 N4 1.9(4) . . . . ?
N3 C18 C19 C20 -179.9(3) . . . . ?
N4 C4 C5 N5 0.0(4) . . . . ?
N4 C4 C5 C6 -179.2(2) . . . . ?
N4 C19 C20 C21 0.4(3) . . . . ?
N4 C19 C20 C43 -179.1(3) . . . . ?
N4 C22 C23 N5 1.6(3) . . . . ?
N4 C22 C23 C24 -177.5(3) . . . . ?
N5 C5 C6 N6 1.7(4) . . . . ?
N5 C5 C6 C1 -177.9(2) . . . . ?
N5 C23 C24 C25 -0.1(3) . . . . ?
N5 C23 C24 C47 -179.4(3) . . . . ?
N5 C26 C27 N6 -0.7(4) . . . . ?
N5 C26 C27 C28 178.7(3) . . . . ?
N6 C27 C28 C29 -0.2(3) . . . . ?
C1 N1 C7 C8 -180.0(2) . . . . ?
C1 N1 C7 C30 0.2(4) . . . . ?
C1 N1 C10 C9 -180.0(2) . . . . ?
C1 N1 C10 C11 0.5(4) . . . . ?
C1 C2 C3 N3 -180.0(2) . . . . ?
C1 C2 C3 C4 2.0(4) . . . . ?
C2 N2 C11 C10 -3.1(4) . . . . ?
C2 N2 C11 C12 175.7(2) . . . . ?
C2 N2 C14 C13 -175.9(2) . . . . ?
C2 N2 C14 C15 3.9(4) . . . . ?
C2 C1 C6 N6 179.9(2) . . . . ?
C2 C1 C6 C5 -0.5(4) . . . . ?
C2 C3 C4 N4 177.5(2) . . . . ?
C2 C3 C4 C5 -1.1(4) . . . . ?
C3 N3 C15 C14 5.9(4) . . . . ?
C3 N3 C15 C16 -173.5(2) . . . . ?
C3 N3 C18 C17 173.4(2) . . . . ?
C3 N3 C18 C19 -3.8(4) . . . . ?
C3 C4 C5 N5 178.7(2) . . . . ?
C3 C4 C5 C6 -0.5(4) . . . . ?
C4 N4 C19 C18 0.5(4) . . . . ?
C4 N4 C19 C20 -178.3(2) . . . . ?
C4 N4 C22 C21 178.2(2) . . . . ?
C4 N4 C22 C23 -0.8(4) . . . . ?
C4 C5 C6 N6 -179.1(2) . . . . ?
C4 C5 C6 C1 1.3(4) . . . . ?
C5 N5 C23 C22 -1.7(4) . . . . ?
C5 N5 C23 C24 177.7(2) . . . . ?
C5 N5 C26 C25 -177.7(2) . . . . ?
C5 N5 C26 C27 1.9(4) . . . . ?
C6 N6 C27 C26 0.0(4) . . . . ?
C6 N6 C27 C28 -179.6(2) . . . . ?
C6 N6 C30 C7 0.2(4) . . . . ?
C6 N6 C30 C29 179.6(2) . . . . ?
C6 C1 C2 N2 179.2(2) . . . . ?
C6 C1 C2 C3 -1.2(4) . . . . ?
C7 N1 C1 C2 -179.7(2) . . . . ?
C7 N1 C1 C6 -0.8(4) . . . . ?
C7 N1 C10 C9 -0.4(3) . . . . ?
C7 N1 C10 C11 -179.9(2) . . . . ?
C7 C8 C9 C10 0.1(3) . . . . ?
C7 C8 C9 C33 -177.1(3) . . . . ?
C7 C8 C31 C32 94.9(3) . . . . ?
C8 C7 C30 N6 -179.6(3) . . . . ?
C8 C7 C30 C29 1.3(6) . . . . ?
C8 C9 C10 N1 0.2(3) . . . . ?
C8 C9 C10 C11 179.5(3) . . . . ?
C8 C9 C33 C34 100.7(3) . . . . ?
C9 C8 C31 C32 -83.4(4) . . . . ?
C9 C10 C11 N2 -178.3(3) . . . . ?
C9 C10 C11 C12 3.5(6) . . . . ?
C10 N1 C1 C2 -0.1(4) . . . . ?
C10 N1 C1 C6 178.8(2) . . . . ?
C10 N1 C7 C8 0.4(3) . . . . ?
C10 N1 C7 C30 -179.4(2) . . . . ?
C10 C9 C33 C34 -75.9(4) . . . . ?
C10 C11 C12 C13 178.6(3) . . . . ?
C10 C11 C12 C35 -0.7(5) . . . . ?
C11 N2 C2 C1 3.6(4) . . . . ?
C11 N2 C2 C3 -176.0(2) . . . . ?
C11 N2 C14 C13 0.0(3) . . . . ?
C11 N2 C14 C15 179.8(2) . . . . ?
C11 C12 C13 C14 -0.3(3) . . . . ?
C11 C12 C13 C37 -178.2(2) . . . . ?
C11 C12 C35 C36 107.7(3) . . . . ?
C12 C13 C14 N2 0.2(3) . . . . ?
C12 C13 C14 C15 -179.6(3) . . . . ?
C12 C13 C37 C38 107.9(3) . . . . ?
C13 C12 C35 C36 -71.4(4) . . . . ?
C13 C14 C15 N3 173.4(3) . . . . ?
C13 C14 C15 C16 -7.6(6) . . . . ?
C14 N2 C2 C1 179.0(2) . . . . ?
C14 N2 C2 C3 -0.5(4) . . . . ?
C14 N2 C11 C10 -178.9(2) . . . . ?
C14 N2 C11 C12 -0.2(3) . . . . ?
C14 C13 C37 C38 -69.6(4) . . . . ?
C14 C15 C16 C17 -178.8(3) . . . . ?
C14 C15 C16 C39 -3.7(6) . . . . ?
C15 N3 C3 C2 -2.5(4) . . . . ?
C15 N3 C3 C4 175.5(2) . . . . ?
C15 N3 C18 C17 0.4(3) . . . . ?
C15 N3 C18 C19 -176.8(2) . . . . ?
C15 C16 C17 C18 -0.1(3) . . . . ?
C15 C16 C17 C41 174.4(3) . . . . ?
C15 C16 C39 C40 115.1(3) . . . . ?
C16 C17 C18 N3 -0.1(3) . . . . ?
C16 C17 C18 C19 175.9(3) . . . . ?
C16 C17 C41 C42 96.8(3) . . . . ?
C17 C16 C39 C40 -70.4(4) . . . . ?
C17 C18 C19 N4 -173.9(3) . . . . ?
C17 C18 C19 C20 4.4(6) . . . . ?
C18 N3 C3 C2 -174.9(2) . . . . ?
C18 N3 C3 C4 3.2(4) . . . . ?
C18 N3 C15 C14 178.9(2) . . . . ?
C18 N3 C15 C16 -0.4(3) . . . . ?
C18 C17 C41 C42 -89.7(4) . . . . ?
C18 C19 C20 C21 -178.0(3) . . . . ?
C18 C19 C20 C43 2.5(5) . . . . ?
C19 N4 C4 C3 -1.3(4) . . . . ?
C19 N4 C4 C5 177.4(2) . . . . ?
C19 N4 C22 C21 0.6(3) . . . . ?
C19 N4 C22 C23 -178.4(2) . . . . ?
C19 C20 C21 C22 -0.1(3) . . . . ?
C19 C20 C21 C45 176.0(3) . . . . ?
C19 C20 C43 C44 -98.7(3) . . . . ?
C20 C21 C22 N4 -0.3(3) . . . . ?
C20 C21 C22 C23 178.3(3) . . . . ?
C20 C21 C45 C46 -104.6(3) . . . . ?
C21 C20 C43 C44 81.9(3) . . . . ?
C21 C22 C23 N5 -176.9(3) . . . . ?
C21 C22 C23 C24 4.0(6) . . . . ?
C22 N4 C4 C3 -178.7(2) . . . . ?
C22 N4 C4 C5 0.0(4) . . . . ?
C22 N4 C19 C18 178.2(2) . . . . ?
C22 N4 C19 C20 -0.6(3) . . . . ?
C22 C21 C45 C46 70.8(4) . . . . ?
C22 C23 C24 C25 179.1(3) . . . . ?
C22 C23 C24 C47 -0.2(6) . . . . ?
C23 N5 C5 C4 0.9(4) . . . . ?
C23 N5 C5 C6 -179.8(2) . . . . ?
C23 N5 C26 C25 -0.1(3) . . . . ?
C23 N5 C26 C27 179.5(2) . . . . ?
C23 C24 C25 C26 0.1(3) . . . . ?
C23 C24 C25 C49 -178.1(3) . . . . ?
C23 C24 C47 C48 -111.1(3) . . . . ?
C24 C25 C26 N5 0.0(3) . . . . ?
C24 C25 C26 C27 -179.5(3) . . . . ?
C24 C25 C49 C50 -107.6(3) . . . . ?
C25 C24 C47 C48 69.7(3) . . . . ?
C25 C26 C27 N6 178.8(3) . . . . ?
C25 C26 C27 C28 -1.8(6) . . . . ?
C26 N5 C5 C4 178.3(2) . . . . ?
C26 N5 C5 C6 -2.5(4) . . . . ?
C26 N5 C23 C22 -179.3(2) . . . . ?
C26 N5 C23 C24 0.1(3) . . . . ?
C26 C25 C49 C50 74.5(4) . . . . ?
C26 C27 C28 C29 -179.6(3) . . . . ?
C27 N6 C6 C1 179.1(2) . . . . ?
C27 N6 C6 C5 -0.5(4) . . . . ?
C27 N6 C30 C7 -179.6(2) . . . . ?
C27 N6 C30 C29 -0.3(3) . . . . ?
C27 C28 C29 C30 0.1(3) . . . . ?
C28 C29 C30 N6 0.1(3) . . . . ?
C28 C29 C30 C7 179.3(3) . . . . ?
C30 N6 C6 C1 -0.8(4) . . . . ?
C30 N6 C6 C5 179.6(3) . . . . ?
C30 N6 C27 C26 179.9(2) . . . . ?
C30 N6 C27 C28 0.3(3) . . . . ?
C30 C7 C8 C9 179.4(3) . . . . ?
C30 C7 C8 C31 0.9(5) . . . . ?
C31 C8 C9 C10 178.6(3) . . . . ?
C31 C8 C9 C33 1.5(4) . . . . ?
C33 C9 C10 N1 177.2(3) . . . . ?
C33 C9 C10 C11 -3.5(6) . . . . ?
C35 C12 C13 C14 179.0(3) . . . . ?
C35 C12 C13 C37 1.1(4) . . . . ?
C37 C13 C14 N2 177.9(3) . . . . ?
C37 C13 C14 C15 -1.9(5) . . . . ?
C39 C16 C17 C18 -175.5(3) . . . . ?
C39 C16 C17 C41 -0.9(4) . . . . ?
C41 C17 C18 N3 -174.4(3) . . . . ?
C41 C17 C18 C19 1.6(6) . . . . ?
C43 C20 C21 C22 179.4(2) . . . . ?
C43 C20 C21 C45 -4.4(4) . . . . ?
C45 C21 C22 N4 -176.3(3) . . . . ?
C45 C21 C22 C23 2.3(5) . . . . ?
C47 C24 C25 C26 179.4(2) . . . . ?
C47 C24 C25 C49 1.3(4) . . . . ?
C49 C25 C26 N5 178.2(2) . . . . ?
C49 C25 C26 C27 -1.3(5) . . . . ?

_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 1.370
_oxdiff_exptl_absorpt_empirical_full_min 0.648
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: C6H5Cl'
_exptl_crystal_preparation       'Magnetic properties,Conducting properties'
####################################################################### 
# 
# 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_ethac2i3_autored
_database_code_depnum_ccdc_archive 'CCDC 2394976'
loop_
_audit_author_name
_audit_author_address
'Toshio Naito'
;Ehime University
Japan
;
_audit_update_record             
;
2024-10-31 deposited with the CCDC.	2025-05-30 downloaded from the CCDC.
;
_audit_creation_date             2024-10-23
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        (EtHAC)2I3
_chemical_formula_moiety         'I3, 2(C50 H52 N6)'
_chemical_formula_sum            'C100 H104 I3 N12'
_chemical_formula_weight         1854.65
_chemical_melting_point          ?
_chemical_oxdiff_formula         C100H104N12I3
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'
I I -0.4742 1.8119 '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      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                   9.7835(4)
_cell_length_b                   15.0398(5)
_cell_length_c                   15.5308(6)
_cell_angle_alpha                107.211(3)
_cell_angle_beta                 98.244(3)
_cell_angle_gamma                103.056(3)
_cell_volume                     2071.49(14)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    15343
_cell_measurement_temperature    300
_cell_measurement_theta_max      31.1490
_cell_measurement_theta_min      2.1860
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.189
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             947
_exptl_crystal_size_max          0.389
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.038
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35248
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         2.194
_diffrn_ambient_temperature      300
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 7.111
_diffrn_detector_type            'Rigaku Saturn724+ area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50    6.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50    6.00    --  -20.00  45.00  90.00  360
  3  ω   -110.00  70.00   0.50    6.00    --  -20.00  45.00 180.00  360
  4  ω   -110.00  70.00   0.50    6.00    --  -20.00  45.00 270.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Rigaku Varimax with Saturn'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0268125000
_diffrn_orient_matrix_UB_12      0.0486058000
_diffrn_orient_matrix_UB_13      0.0308921000
_diffrn_orient_matrix_UB_21      0.0683957000
_diffrn_orient_matrix_UB_22      -0.0074169000
_diffrn_orient_matrix_UB_23      0.0114330000
_diffrn_orient_matrix_UB_31      0.0209736000
_diffrn_orient_matrix_UB_32      0.0152868000
_diffrn_orient_matrix_UB_33      -0.0363848000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'MicroMax 007'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5807
_reflns_number_total             9971
_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 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b46 (Rigaku, 2016)'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.923
_refine_diff_density_min         -0.944
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         9971
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.1083
_refine_ls_R_factor_gt           0.0679
_refine_ls_restrained_S_all      1.120
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1326P)²+0.2045P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2114
_refine_ls_wR_factor_ref         0.2371
_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
 I1-I2 = I2-I1
 2.8 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
I1 \\sim I2: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Uanis(C39) \\sim Ueq, Uanis(C52) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C51) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 I2, I1, I3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=1-FVAR(1)
 Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(C51)=Sof(H51A)=Sof(H51B)=FVAR(1)
 Fixed Sof: I1(0.5) I2(0.5) I3(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C33(H33A,H33B), C49(H49A,H49B), C37(H37A,H37B), C35(H35A,
 H35B), C43(H43A,H43B), C47(H47A,H47B), C45(H45A,H45B), C39(H39A,H39B),
 C41(H41A,H41B), C51(H51A,H51B)
6.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9)
6.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C50(H50A,H50B,H50C), C38(H38A,H38B,H38C), C36(H36A,H36B,
 H36C), C48(H48A,H48B,H48C), C44(H44A,H44B,H44C), C34(H34A,H34B,H34C), C46(H46A,
 H46B,H46C), C42(H42A,H42B,H42C), C40(H40A,H40B,H40C), C52(H52A,H52B,H52C)
;
_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
I1 I 0.03352(8) 0.98595(8) 0.00554(7) 0.1127(4) Uani 0.5 1 d D . P A -1
I2 I 0.05213(19) 0.82793(10) 0.07464(10) 0.1625(6) Uani 0.5 1 d D . P A -1
N1 N 0.1613(2) 0.37042(14) 0.34928(13) 0.0473(5) Uani 1 1 d . . . . .
N6 N 0.3643(2) 0.35515(14) 0.47974(15) 0.0491(5) Uani 1 1 d . . . . .
N2 N 0.0602(2) 0.52981(15) 0.38672(13) 0.0467(5) Uani 1 1 d . . . . .
N5 N 0.4687(2) 0.49915(15) 0.64776(14) 0.0480(5) Uani 1 1 d . . . . .
N4 N 0.3609(2) 0.65665(14) 0.68787(13) 0.0470(5) Uani 1 1 d . . . . .
N3 N 0.1560(2) 0.67105(14) 0.55654(15) 0.0480(5) Uani 1 1 d . . . . .
C1 C 0.2110(2) 0.44212(16) 0.43326(15) 0.0422(5) Uani 1 1 d . . . . .
C2 C 0.1593(2) 0.52099(16) 0.45241(15) 0.0419(5) Uani 1 1 d . . . . .
C5 C 0.3651(2) 0.50726(17) 0.58320(15) 0.0428(5) Uani 1 1 d . . . . .
C6 C 0.3140(2) 0.43509(16) 0.49921(16) 0.0433(5) Uani 1 1 d . . . . .
C30 C 0.3167(3) 0.28003(18) 0.39461(19) 0.0534(6) Uani 1 1 d . . . . .
C10 C 0.0595(3) 0.37475(19) 0.27945(16) 0.0511(6) Uani 1 1 d . . . . .
C4 C 0.3108(2) 0.58501(15) 0.60325(15) 0.0418(5) Uani 1 1 d . . . . .
C3 C 0.2076(2) 0.59205(15) 0.53784(16) 0.0410(5) Uani 1 1 d . . . . .
C7 C 0.2086(3) 0.28838(18) 0.32476(18) 0.0525(6) Uani 1 1 d . . . . .
C14 C 0.0018(3) 0.60829(19) 0.40047(19) 0.0497(6) Uani 1 1 d . . . . .
C27 C 0.4675(3) 0.3411(2) 0.5424(2) 0.0528(6) Uani 1 1 d . . . . .
C11 C 0.0048(3) 0.45879(19) 0.29982(17) 0.0508(6) Uani 1 1 d . . . . .
C29 C 0.3928(3) 0.2143(2) 0.4029(2) 0.0628(7) Uani 1 1 d . . . . .
C26 C 0.5223(3) 0.4192(2) 0.63406(19) 0.0525(6) Uani 1 1 d . . . . .
C23 C 0.5226(3) 0.5691(2) 0.73641(17) 0.0535(6) Uani 1 1 d . . . . .
C19 C 0.3145(3) 0.73945(18) 0.71121(18) 0.0548(6) Uani 1 1 d . . . . .
C15 C 0.0571(3) 0.68545(19) 0.49124(19) 0.0504(6) Uani 1 1 d . . . . .
C22 C 0.4685(3) 0.65485(19) 0.75621(17) 0.0544(6) Uani 1 1 d . . . . .
C8 C 0.1318(3) 0.2377(2) 0.2343(2) 0.0670(8) Uani 1 1 d . . . . .
H8 H 0.139205 0.178456 0.197471 0.080 Uiso 1 1 calc R U . . .
C18 C 0.2061(3) 0.74872(17) 0.64011(19) 0.0527(6) Uani 1 1 d . . . . .
C13 C -0.0981(3) 0.5844(2) 0.3153(2) 0.0585(7) Uani 1 1 d . . . . .
C25 C 0.6168(3) 0.4383(3) 0.7178(2) 0.0642(8) Uani 1 1 d . . . . .
C12 C -0.0951(3) 0.4936(2) 0.25467(19) 0.0582(7) Uani 1 1 d . . . . .
C9 C 0.0416(3) 0.2891(2) 0.20699(19) 0.0658(8) Uani 1 1 d . . . . .
H9 H -0.020773 0.269190 0.149374 0.079 Uiso 1 1 calc R U . . .
C24 C 0.6166(3) 0.5297(3) 0.7801(2) 0.0652(8) Uani 1 1 d . . . . .
C17 C 0.1338(3) 0.8157(2) 0.6281(2) 0.0620(7) Uani 1 1 d . . . . .
C16 C 0.0451(3) 0.7785(2) 0.5383(2) 0.0628(7) Uani 1 1 d . . . . .
C31 C -0.1849(3) 0.4392(3) 0.1583(2) 0.0753(9) Uani 1 1 d . . . . .
H31A H -0.267348 0.464043 0.150136 0.090 Uiso 1 1 calc R U . . .
H31B H -0.221038 0.371429 0.151813 0.090 Uiso 1 1 calc R U . . .
C28 C 0.4856(3) 0.2507(2) 0.4930(3) 0.0651(8) Uani 1 1 d . . . . .
C21 C 0.4924(4) 0.7431(2) 0.8281(2) 0.0712(8) Uani 1 1 d . . . . .
C20 C 0.3987(4) 0.7942(2) 0.8011(2) 0.0742(9) Uani 1 1 d . . . . .
C33 C -0.1975(3) 0.6390(3) 0.2883(3) 0.0807(10) Uani 1 1 d . . . . .
H33A H -0.203443 0.687540 0.343814 0.097 Uiso 1 1 calc R U . . .
H33B H -0.293057 0.594172 0.260872 0.097 Uiso 1 1 calc R U . . .
C49 C 0.3789(4) 0.1204(2) 0.3281(3) 0.0808(10) Uani 1 1 d . . . . .
H49A H 0.359555 0.129270 0.268657 0.097 Uiso 1 1 calc R U . . .
H49B H 0.470339 0.105463 0.335362 0.097 Uiso 1 1 calc R U . . .
C32 C -0.1056(4) 0.4457(4) 0.0812(2) 0.0994(13) Uani 1 1 d . . . . .
H32A H -0.171717 0.412405 0.022179 0.149 Uiso 1 1 calc R U . . .
H32B H -0.028782 0.416063 0.085209 0.149 Uiso 1 1 calc R U . . .
H32C H -0.066715 0.512573 0.087961 0.149 Uiso 1 1 calc R U . . .
C37 C 0.1453(4) 0.9137(2) 0.6967(3) 0.0881(11) Uani 1 1 d . . . . .
H37A H 0.174673 0.912900 0.758766 0.106 Uiso 1 1 calc R U . . .
H37B H 0.050870 0.924446 0.690664 0.106 Uiso 1 1 calc R U . . .
C50 C 0.2636(4) 0.0354(3) 0.3271(3) 0.0908(11) Uani 1 1 d . . . . .
H50A H 0.270493 -0.022809 0.283295 0.136 Uiso 1 1 calc R U . . .
H50B H 0.170855 0.044489 0.309693 0.136 Uiso 1 1 calc R U . . .
H50C H 0.275309 0.030023 0.387608 0.136 Uiso 1 1 calc R U . . .
C35 C -0.0406(4) 0.8341(3) 0.4982(3) 0.0879(11) Uani 1 1 d . . . . .
H35A H -0.055268 0.885018 0.548249 0.105 Uiso 1 1 calc R U . . .
H35B H -0.134451 0.790643 0.463217 0.105 Uiso 1 1 calc R U . . .
C43 C 0.7026(3) 0.5693(3) 0.8776(2) 0.0918(12) Uani 1 1 d . . . . .
H43A H 0.782353 0.541189 0.881194 0.110 Uiso 1 1 calc R U . . .
H43B H 0.742705 0.638910 0.894563 0.110 Uiso 1 1 calc R U . . .
C47 C 0.5778(5) 0.1944(3) 0.5238(3) 0.0943(13) Uani 1 1 d . . . . .
H47A H 0.665822 0.239371 0.565968 0.113 Uiso 1 1 calc R U . . .
H47B H 0.603970 0.155161 0.470443 0.113 Uiso 1 1 calc R U . . .
C38 C 0.2517(5) 0.9984(3) 0.6846(4) 0.1175(16) Uani 1 1 d . . . . .
H38A H 0.232363 0.994225 0.620986 0.176 Uiso 1 1 calc R U . . .
H38B H 0.348212 0.995508 0.702668 0.176 Uiso 1 1 calc R U . . .
H38C H 0.241286 1.058566 0.722712 0.176 Uiso 1 1 calc R U . . .
C45 C 0.7058(4) 0.3773(3) 0.7438(3) 0.0949(12) Uani 1 1 d . . . . .
H45A H 0.721987 0.335423 0.687640 0.114 Uiso 1 1 calc R U . . .
H45B H 0.798958 0.419804 0.781022 0.114 Uiso 1 1 calc R U . . .
C36 C 0.0333(6) 0.8787(3) 0.4358(4) 0.1121(15) Uani 1 1 d . . . . .
H36A H 0.056447 0.829503 0.389664 0.168 Uiso 1 1 calc R U . . .
H36B H 0.120190 0.928273 0.471923 0.168 Uiso 1 1 calc R U . . .
H36C H -0.029659 0.906869 0.406217 0.168 Uiso 1 1 calc R U . . .
C48 C 0.5054(6) 0.1293(3) 0.5712(4) 0.1118(15) Uani 1 1 d . . . . .
H48A H 0.428063 0.077454 0.526818 0.168 Uiso 1 1 calc R U . . .
H48B H 0.467876 0.166156 0.619048 0.168 Uiso 1 1 calc R U . . .
H48C H 0.574182 0.102828 0.597817 0.168 Uiso 1 1 calc R U . . .
C39 C 0.4111(7) 0.8973(4) 0.8578(4) 0.0862(19) Uani 0.761(10) 1 d . U P B 2
H39A H 0.508985 0.928800 0.894131 0.103 Uiso 0.761(10) 1 calc R U P B 2
H39B H 0.390076 0.932695 0.816984 0.103 Uiso 0.761(10) 1 calc R U P B 2
C41 C 0.6024(6) 0.7847(3) 0.9188(3) 0.1179(16) Uani 1 1 d . . . . .
H41A H 0.646834 0.852825 0.929916 0.141 Uiso 1 1 calc R U . . .
H41B H 0.677295 0.752012 0.913682 0.141 Uiso 1 1 calc R U . . .
C44 C 0.6182(5) 0.5498(4) 0.9454(3) 0.1143(15) Uani 1 1 d . . . . .
H44A H 0.578542 0.481012 0.929441 0.171 Uiso 1 1 calc R U . . .
H44B H 0.541426 0.579804 0.944310 0.171 Uiso 1 1 calc R U . . .
H44C H 0.679860 0.575951 1.006239 0.171 Uiso 1 1 calc R U . . .
C34 C -0.1534(6) 0.6890(4) 0.2209(4) 0.1181(17) Uani 1 1 d . . . . .
H34A H -0.152707 0.641292 0.164139 0.177 Uiso 1 1 calc R U . . .
H34B H -0.058900 0.733598 0.247153 0.177 Uiso 1 1 calc R U . . .
H34C H -0.220799 0.723731 0.208700 0.177 Uiso 1 1 calc R U . . .
C46 C 0.6424(7) 0.3154(4) 0.7959(4) 0.1298(19) Uani 1 1 d . . . . .
H46A H 0.549362 0.273539 0.760354 0.195 Uiso 1 1 calc R U . . .
H46B H 0.632760 0.356132 0.854031 0.195 Uiso 1 1 calc R U . . .
H46C H 0.704448 0.276851 0.806927 0.195 Uiso 1 1 calc R U . . .
C42 C 0.5410(10) 0.7757(6) 1.0030(3) 0.184(3) Uani 1 1 d . . . . .
H42A H 0.462687 0.717335 0.983859 0.276 Uiso 1 1 calc R U . . .
H42B H 0.506973 0.830760 1.028271 0.276 Uiso 1 1 calc R U . . .
H42C H 0.615193 0.773226 1.049240 0.276 Uiso 1 1 calc R U . . .
C40 C 0.3104(7) 0.8999(4) 0.9203(5) 0.115(2) Uani 0.761(10) 1 d . . P B 2
H40A H 0.213194 0.873092 0.884187 0.172 Uiso 0.761(10) 1 calc R U P B 2
H40B H 0.324189 0.965849 0.958328 0.172 Uiso 0.761(10) 1 calc R U P B 2
H40C H 0.328451 0.862422 0.958812 0.172 Uiso 0.761(10) 1 calc R U P B 2
I3 I 0.01110(17) 1.13689(11) -0.07421(10) 0.1536(5) Uani 0.5 1 d . . P A -1
C52 C 0.4534(15) 0.9744(8) 0.8694(8) 0.066(4) Uani 0.239(10) 1 d . U P B 1
H52A H 0.392127 1.005074 0.841950 0.099 Uiso 0.239(10) 1 calc R U P B 1
H52B H 0.520939 0.959768 0.832069 0.099 Uiso 0.239(10) 1 calc R U P B 1
H52C H 0.504658 1.017370 0.930408 0.099 Uiso 0.239(10) 1 calc R U P B 1
C51 C 0.3592(19) 0.8779(11) 0.8756(9) 0.060(4) Uani 0.239(10) 1 d . U P B 1
H51A H 0.257370 0.872759 0.860263 0.072 Uiso 0.239(10) 1 calc R U P B 1
H51B H 0.383588 0.874636 0.937180 0.072 Uiso 0.239(10) 1 calc R U P B 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
I1 I2 2.9124(18) . ?
I1 I3 2.9235(19) . ?
N1 C1 1.360(3) . ?
N1 C10 1.391(3) . ?
N1 C7 1.383(3) . ?
N6 C6 1.369(3) . ?
N6 C30 1.394(3) . ?
N6 C27 1.396(3) . ?
N2 C2 1.361(3) . ?
N2 C14 1.399(3) . ?
N2 C11 1.390(3) . ?
N5 C5 1.372(3) . ?
N5 C26 1.390(3) . ?
N5 C23 1.402(3) . ?
N4 C4 1.366(3) . ?
N4 C19 1.387(3) . ?
N4 C22 1.395(3) . ?
N3 C3 1.364(3) . ?
N3 C15 1.398(3) . ?
N3 C18 1.397(3) . ?
C1 C2 1.363(3) . ?
C1 C6 1.375(3) . ?
C2 C3 1.371(3) . ?
C5 C6 1.364(3) . ?
C5 C4 1.364(3) . ?
C30 C7 1.457(4) . ?
C30 C29 1.388(4) . ?
C10 C11 1.450(4) . ?
C10 C9 1.393(4) . ?
C4 C3 1.371(3) . ?
C7 C8 1.387(4) . ?
C14 C15 1.468(4) . ?
C14 C13 1.422(4) . ?
C27 C26 1.484(4) . ?
C27 C28 1.413(4) . ?
C11 C12 1.405(4) . ?
C29 C28 1.428(5) . ?
C29 C49 1.504(4) . ?
C26 C25 1.394(4) . ?
C23 C22 1.469(4) . ?
C23 C24 1.401(4) . ?
C19 C18 1.478(4) . ?
C19 C20 1.410(4) . ?
C15 C16 1.415(4) . ?
C22 C21 1.403(4) . ?
C8 H8 0.9300 . ?
C8 C9 1.397(5) . ?
C18 C17 1.395(4) . ?
C13 C12 1.420(5) . ?
C13 C33 1.499(4) . ?
C25 C24 1.428(5) . ?
C25 C45 1.498(4) . ?
C12 C31 1.501(4) . ?
C9 H9 0.9300 . ?
C24 C43 1.494(4) . ?
C17 C16 1.408(5) . ?
C17 C37 1.510(4) . ?
C16 C35 1.504(4) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.532(5) . ?
C28 C47 1.491(4) . ?
C21 C20 1.417(5) . ?
C21 C41 1.508(5) . ?
C20 C39 1.507(6) . ?
C20 C51 1.600(16) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C34 1.515(5) . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C49 C50 1.496(5) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 C38 1.529(6) . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C35 C36 1.510(6) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C43 C44 1.483(6) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C47 C48 1.504(6) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C45 C46 1.496(6) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 C40 1.477(10) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C41 C42 1.543(8) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C52 C51 1.572(19) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?

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
I2 I1 I3 176.84(6) . . ?
C1 N1 C10 122.3(2) . . ?
C1 N1 C7 123.6(2) . . ?
C7 N1 C10 114.1(2) . . ?
C6 N6 C30 122.7(2) . . ?
C6 N6 C27 123.6(2) . . ?
C30 N6 C27 113.7(2) . . ?
C2 N2 C14 123.9(2) . . ?
C2 N2 C11 122.1(2) . . ?
C11 N2 C14 113.9(2) . . ?
C5 N5 C26 123.7(2) . . ?
C5 N5 C23 122.1(2) . . ?
C26 N5 C23 114.0(2) . . ?
C4 N4 C19 122.9(2) . . ?
C4 N4 C22 122.6(2) . . ?
C19 N4 C22 114.4(2) . . ?
C3 N3 C15 123.1(2) . . ?
C3 N3 C18 122.9(2) . . ?
C18 N3 C15 113.8(2) . . ?
N1 C1 C2 120.3(2) . . ?
N1 C1 C6 119.9(2) . . ?
C2 C1 C6 119.8(2) . . ?
N2 C2 C1 120.2(2) . . ?
N2 C2 C3 119.8(2) . . ?
C1 C2 C3 120.0(2) . . ?
C6 C5 N5 119.1(2) . . ?
C6 C5 C4 120.1(2) . . ?
C4 C5 N5 120.7(2) . . ?
N6 C6 C1 119.4(2) . . ?
C5 C6 N6 120.5(2) . . ?
C5 C6 C1 120.1(2) . . ?
N6 C30 C7 117.6(2) . . ?
C29 C30 N6 104.7(2) . . ?
C29 C30 C7 137.7(3) . . ?
N1 C10 C11 117.3(2) . . ?
N1 C10 C9 103.3(2) . . ?
C9 C10 C11 139.4(2) . . ?
N4 C4 C3 120.0(2) . . ?
C5 C4 N4 120.0(2) . . ?
C5 C4 C3 119.9(2) . . ?
N3 C3 C2 119.8(2) . . ?
N3 C3 C4 120.2(2) . . ?
C2 C3 C4 120.0(2) . . ?
N1 C7 C30 116.8(2) . . ?
N1 C7 C8 103.6(2) . . ?
C8 C7 C30 139.6(3) . . ?
N2 C14 C15 116.0(2) . . ?
N2 C14 C13 103.7(2) . . ?
C13 C14 C15 140.3(2) . . ?
N6 C27 C26 115.9(2) . . ?
N6 C27 C28 103.7(3) . . ?
C28 C27 C26 140.3(3) . . ?
N2 C11 C10 117.7(2) . . ?
N2 C11 C12 104.5(2) . . ?
C12 C11 C10 137.8(2) . . ?
C30 C29 C28 109.1(3) . . ?
C30 C29 C49 124.8(3) . . ?
C28 C29 C49 126.1(3) . . ?
N5 C26 C27 117.0(2) . . ?
N5 C26 C25 104.7(3) . . ?
C25 C26 C27 138.3(3) . . ?
N5 C23 C22 116.9(2) . . ?
C24 C23 N5 103.1(3) . . ?
C24 C23 C22 139.9(3) . . ?
N4 C19 C18 117.4(2) . . ?
N4 C19 C20 103.5(2) . . ?
C20 C19 C18 139.0(3) . . ?
N3 C15 C14 117.4(2) . . ?
N3 C15 C16 103.0(3) . . ?
C16 C15 C14 139.6(2) . . ?
N4 C22 C23 117.4(2) . . ?
N4 C22 C21 103.9(2) . . ?
C21 C22 C23 138.7(3) . . ?
C7 C8 H8 125.2 . . ?
C7 C8 C9 109.6(2) . . ?
C9 C8 H8 125.2 . . ?
N3 C18 C19 116.6(2) . . ?
C17 C18 N3 104.4(2) . . ?
C17 C18 C19 139.0(2) . . ?
C14 C13 C33 129.2(3) . . ?
C12 C13 C14 108.7(2) . . ?
C12 C13 C33 122.1(3) . . ?
C26 C25 C24 108.3(2) . . ?
C26 C25 C45 128.6(3) . . ?
C24 C25 C45 123.0(3) . . ?
C11 C12 C13 109.1(2) . . ?
C11 C12 C31 123.6(3) . . ?
C13 C12 C31 127.3(3) . . ?
C10 C9 C8 109.4(2) . . ?
C10 C9 H9 125.3 . . ?
C8 C9 H9 125.3 . . ?
C23 C24 C25 109.8(3) . . ?
C23 C24 C43 128.5(3) . . ?
C25 C24 C43 121.6(3) . . ?
C18 C17 C16 109.0(2) . . ?
C18 C17 C37 127.8(3) . . ?
C16 C17 C37 123.2(3) . . ?
C15 C16 C35 126.2(3) . . ?
C17 C16 C15 109.8(2) . . ?
C17 C16 C35 124.0(3) . . ?
C12 C31 H31A 108.6 . . ?
C12 C31 H31B 108.6 . . ?
C12 C31 C32 114.8(3) . . ?
H31A C31 H31B 107.6 . . ?
C32 C31 H31A 108.6 . . ?
C32 C31 H31B 108.6 . . ?
C27 C28 C29 108.8(2) . . ?
C27 C28 C47 129.6(4) . . ?
C29 C28 C47 121.6(3) . . ?
C22 C21 C20 108.9(3) . . ?
C22 C21 C41 128.6(3) . . ?
C20 C21 C41 122.5(3) . . ?
C19 C20 C21 109.3(3) . . ?
C19 C20 C39 128.2(4) . . ?
C19 C20 C51 125.5(6) . . ?
C21 C20 C39 121.8(3) . . ?
C21 C20 C51 121.5(5) . . ?
C13 C33 H33A 108.6 . . ?
C13 C33 H33B 108.6 . . ?
C13 C33 C34 114.8(3) . . ?
H33A C33 H33B 107.6 . . ?
C34 C33 H33A 108.6 . . ?
C34 C33 H33B 108.6 . . ?
C29 C49 H49A 108.6 . . ?
C29 C49 H49B 108.6 . . ?
H49A C49 H49B 107.5 . . ?
C50 C49 C29 114.8(3) . . ?
C50 C49 H49A 108.6 . . ?
C50 C49 H49B 108.6 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C17 C37 H37A 108.7 . . ?
C17 C37 H37B 108.7 . . ?
C17 C37 C38 114.0(3) . . ?
H37A C37 H37B 107.6 . . ?
C38 C37 H37A 108.7 . . ?
C38 C37 H37B 108.7 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C16 C35 H35A 109.2 . . ?
C16 C35 H35B 109.2 . . ?
C16 C35 C36 112.2(3) . . ?
H35A C35 H35B 107.9 . . ?
C36 C35 H35A 109.2 . . ?
C36 C35 H35B 109.2 . . ?
C24 C43 H43A 108.8 . . ?
C24 C43 H43B 108.8 . . ?
H43A C43 H43B 107.7 . . ?
C44 C43 C24 113.7(3) . . ?
C44 C43 H43A 108.8 . . ?
C44 C43 H43B 108.8 . . ?
C28 C47 H47A 108.9 . . ?
C28 C47 H47B 108.9 . . ?
C28 C47 C48 113.2(3) . . ?
H47A C47 H47B 107.8 . . ?
C48 C47 H47A 108.9 . . ?
C48 C47 H47B 108.9 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C25 C45 H45A 108.4 . . ?
C25 C45 H45B 108.4 . . ?
H45A C45 H45B 107.5 . . ?
C46 C45 C25 115.4(4) . . ?
C46 C45 H45A 108.4 . . ?
C46 C45 H45B 108.4 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C20 C39 H39A 109.5 . . ?
C20 C39 H39B 109.5 . . ?
H39A C39 H39B 108.1 . . ?
C40 C39 C20 110.9(6) . . ?
C40 C39 H39A 109.5 . . ?
C40 C39 H39B 109.5 . . ?
C21 C41 H41A 108.7 . . ?
C21 C41 H41B 108.7 . . ?
C21 C41 C42 114.4(5) . . ?
H41A C41 H41B 107.6 . . ?
C42 C41 H41A 108.7 . . ?
C42 C41 H41B 108.7 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
C20 C51 H51A 111.0 . . ?
C20 C51 H51B 111.0 . . ?
C52 C51 C20 103.9(11) . . ?
C52 C51 H51A 111.0 . . ?
C52 C51 H51B 111.0 . . ?
H51A C51 H51B 109.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 N2 -1.8(3) . . . . ?
N1 C1 C2 C3 178.7(2) . . . . ?
N1 C1 C6 N6 -0.7(3) . . . . ?
N1 C1 C6 C5 179.4(2) . . . . ?
N1 C10 C11 N2 1.4(3) . . . . ?
N1 C10 C11 C12 -179.0(3) . . . . ?
N1 C10 C9 C8 -0.6(3) . . . . ?
N1 C7 C8 C9 -0.1(3) . . . . ?
N6 C30 C7 N1 -0.4(3) . . . . ?
N6 C30 C7 C8 178.9(3) . . . . ?
N6 C30 C29 C28 -0.1(3) . . . . ?
N6 C30 C29 C49 -179.8(3) . . . . ?
N6 C27 C26 N5 -1.5(3) . . . . ?
N6 C27 C26 C25 177.2(3) . . . . ?
N6 C27 C28 C29 0.0(3) . . . . ?
N6 C27 C28 C47 -177.6(3) . . . . ?
N2 C2 C3 N3 0.1(3) . . . . ?
N2 C2 C3 C4 -177.9(2) . . . . ?
N2 C14 C15 N3 -3.4(3) . . . . ?
N2 C14 C15 C16 174.7(3) . . . . ?
N2 C14 C13 C12 -0.1(3) . . . . ?
N2 C14 C13 C33 178.1(3) . . . . ?
N2 C11 C12 C13 -0.2(3) . . . . ?
N2 C11 C12 C31 -178.7(2) . . . . ?
N5 C5 C6 N6 0.6(3) . . . . ?
N5 C5 C6 C1 -179.5(2) . . . . ?
N5 C5 C4 N4 1.0(3) . . . . ?
N5 C5 C4 C3 179.8(2) . . . . ?
N5 C26 C25 C24 0.3(3) . . . . ?
N5 C26 C25 C45 179.9(3) . . . . ?
N5 C23 C22 N4 4.4(3) . . . . ?
N5 C23 C22 C21 -175.7(3) . . . . ?
N5 C23 C24 C25 -0.1(3) . . . . ?
N5 C23 C24 C43 -177.5(3) . . . . ?
N4 C4 C3 N3 0.8(3) . . . . ?
N4 C4 C3 C2 178.9(2) . . . . ?
N4 C19 C18 N3 2.3(3) . . . . ?
N4 C19 C18 C17 -176.3(3) . . . . ?
N4 C19 C20 C21 0.3(3) . . . . ?
N4 C19 C20 C39 171.1(5) . . . . ?
N4 C19 C20 C51 -158.4(7) . . . . ?
N4 C22 C21 C20 0.3(3) . . . . ?
N4 C22 C21 C41 -176.4(4) . . . . ?
N3 C15 C16 C17 -0.4(3) . . . . ?
N3 C15 C16 C35 175.7(3) . . . . ?
N3 C18 C17 C16 -1.1(3) . . . . ?
N3 C18 C17 C37 179.6(3) . . . . ?
C1 N1 C10 C11 -1.2(3) . . . . ?
C1 N1 C10 C9 179.3(2) . . . . ?
C1 N1 C7 C30 0.6(3) . . . . ?
C1 N1 C7 C8 -179.0(2) . . . . ?
C1 C2 C3 N3 179.7(2) . . . . ?
C1 C2 C3 C4 1.6(3) . . . . ?
C2 N2 C14 C15 2.0(3) . . . . ?
C2 N2 C14 C13 -178.2(2) . . . . ?
C2 N2 C11 C10 -1.9(3) . . . . ?
C2 N2 C11 C12 178.4(2) . . . . ?
C2 C1 C6 N6 179.3(2) . . . . ?
C2 C1 C6 C5 -0.6(3) . . . . ?
C5 N5 C26 C27 2.8(3) . . . . ?
C5 N5 C26 C25 -176.3(2) . . . . ?
C5 N5 C23 C22 -3.0(3) . . . . ?
C5 N5 C23 C24 176.3(2) . . . . ?
C5 C4 C3 N3 -178.0(2) . . . . ?
C5 C4 C3 C2 0.0(3) . . . . ?
C6 N6 C30 C7 -0.3(3) . . . . ?
C6 N6 C30 C29 179.9(2) . . . . ?
C6 N6 C27 C26 0.0(3) . . . . ?
C6 N6 C27 C28 -179.9(2) . . . . ?
C6 C1 C2 N2 178.2(2) . . . . ?
C6 C1 C2 C3 -1.4(3) . . . . ?
C6 C5 C4 N4 179.2(2) . . . . ?
C6 C5 C4 C3 -2.0(3) . . . . ?
C30 N6 C6 C1 0.9(3) . . . . ?
C30 N6 C6 C5 -179.2(2) . . . . ?
C30 N6 C27 C26 179.8(2) . . . . ?
C30 N6 C27 C28 -0.1(3) . . . . ?
C30 C7 C8 C9 -179.5(3) . . . . ?
C30 C29 C28 C27 0.0(3) . . . . ?
C30 C29 C28 C47 177.9(3) . . . . ?
C30 C29 C49 C50 -88.3(4) . . . . ?
C10 N1 C1 C2 1.4(3) . . . . ?
C10 N1 C1 C6 -178.6(2) . . . . ?
C10 N1 C7 C30 179.3(2) . . . . ?
C10 N1 C7 C8 -0.3(3) . . . . ?
C10 C11 C12 C13 -179.9(3) . . . . ?
C10 C11 C12 C31 1.6(5) . . . . ?
C4 N4 C19 C18 0.0(3) . . . . ?
C4 N4 C19 C20 -176.9(2) . . . . ?
C4 N4 C22 C23 -3.4(3) . . . . ?
C4 N4 C22 C21 176.7(2) . . . . ?
C4 C5 C6 N6 -177.6(2) . . . . ?
C4 C5 C6 C1 2.3(3) . . . . ?
C3 N3 C15 C14 3.5(3) . . . . ?
C3 N3 C15 C16 -175.2(2) . . . . ?
C3 N3 C18 C19 -3.2(3) . . . . ?
C3 N3 C18 C17 175.8(2) . . . . ?
C7 N1 C1 C2 180.0(2) . . . . ?
C7 N1 C1 C6 0.0(4) . . . . ?
C7 N1 C10 C11 -179.9(2) . . . . ?
C7 N1 C10 C9 0.5(3) . . . . ?
C7 C30 C29 C28 -179.8(3) . . . . ?
C7 C30 C29 C49 0.4(5) . . . . ?
C7 C8 C9 C10 0.5(3) . . . . ?
C14 N2 C2 C1 -179.9(2) . . . . ?
C14 N2 C2 C3 -0.3(3) . . . . ?
C14 N2 C11 C10 179.9(2) . . . . ?
C14 N2 C11 C12 0.1(3) . . . . ?
C14 C15 C16 C17 -178.7(3) . . . . ?
C14 C15 C16 C35 -2.6(5) . . . . ?
C14 C13 C12 C11 0.2(3) . . . . ?
C14 C13 C12 C31 178.6(2) . . . . ?
C14 C13 C33 C34 106.9(4) . . . . ?
C27 N6 C6 C1 -179.4(2) . . . . ?
C27 N6 C6 C5 0.5(4) . . . . ?
C27 N6 C30 C7 179.9(2) . . . . ?
C27 N6 C30 C29 0.1(3) . . . . ?
C27 C26 C25 C24 -178.5(3) . . . . ?
C27 C26 C25 C45 1.0(5) . . . . ?
C27 C28 C47 C48 86.5(5) . . . . ?
C11 N2 C2 C1 2.1(3) . . . . ?
C11 N2 C2 C3 -178.3(2) . . . . ?
C11 N2 C14 C15 -179.9(2) . . . . ?
C11 N2 C14 C13 0.0(3) . . . . ?
C11 C10 C9 C8 180.0(3) . . . . ?
C11 C12 C31 C32 -78.6(4) . . . . ?
C29 C30 C7 N1 179.3(3) . . . . ?
C29 C30 C7 C8 -1.4(6) . . . . ?
C29 C28 C47 C48 -90.9(4) . . . . ?
C26 N5 C5 C6 -2.4(3) . . . . ?
C26 N5 C5 C4 175.9(2) . . . . ?
C26 N5 C23 C22 -178.9(2) . . . . ?
C26 N5 C23 C24 0.4(3) . . . . ?
C26 C27 C28 C29 -179.8(3) . . . . ?
C26 C27 C28 C47 2.6(6) . . . . ?
C26 C25 C24 C23 -0.1(3) . . . . ?
C26 C25 C24 C43 177.4(3) . . . . ?
C26 C25 C45 C46 -97.3(5) . . . . ?
C23 N5 C5 C6 -177.9(2) . . . . ?
C23 N5 C5 C4 0.3(3) . . . . ?
C23 N5 C26 C27 178.7(2) . . . . ?
C23 N5 C26 C25 -0.4(3) . . . . ?
C23 C22 C21 C20 -179.6(3) . . . . ?
C23 C22 C21 C41 3.6(6) . . . . ?
C23 C24 C43 C44 80.2(5) . . . . ?
C19 N4 C4 C5 177.2(2) . . . . ?
C19 N4 C4 C3 -1.6(3) . . . . ?
C19 N4 C22 C23 179.8(2) . . . . ?
C19 N4 C22 C21 -0.1(3) . . . . ?
C19 C18 C17 C16 177.6(3) . . . . ?
C19 C18 C17 C37 -1.7(5) . . . . ?
C19 C20 C39 C40 94.5(6) . . . . ?
C19 C20 C51 C52 -100.6(10) . . . . ?
C15 N3 C3 C2 -1.9(3) . . . . ?
C15 N3 C3 C4 176.2(2) . . . . ?
C15 N3 C18 C19 -178.2(2) . . . . ?
C15 N3 C18 C17 0.9(3) . . . . ?
C15 C14 C13 C12 179.7(3) . . . . ?
C15 C14 C13 C33 -2.1(5) . . . . ?
C15 C16 C35 C36 -76.4(4) . . . . ?
C22 N4 C4 C5 0.7(3) . . . . ?
C22 N4 C4 C3 -178.2(2) . . . . ?
C22 N4 C19 C18 176.8(2) . . . . ?
C22 N4 C19 C20 -0.1(3) . . . . ?
C22 C23 C24 C25 178.9(3) . . . . ?
C22 C23 C24 C43 1.6(5) . . . . ?
C22 C21 C20 C19 -0.4(4) . . . . ?
C22 C21 C20 C39 -171.9(4) . . . . ?
C22 C21 C20 C51 159.3(8) . . . . ?
C22 C21 C41 C42 -103.2(5) . . . . ?
C18 N3 C3 C2 -176.3(2) . . . . ?
C18 N3 C3 C4 1.7(3) . . . . ?
C18 N3 C15 C14 178.5(2) . . . . ?
C18 N3 C15 C16 -0.3(3) . . . . ?
C18 C19 C20 C21 -175.5(3) . . . . ?
C18 C19 C20 C39 -4.7(7) . . . . ?
C18 C19 C20 C51 25.8(9) . . . . ?
C18 C17 C16 C15 1.0(3) . . . . ?
C18 C17 C16 C35 -175.2(3) . . . . ?
C18 C17 C37 C38 95.7(4) . . . . ?
C13 C14 C15 N3 176.8(3) . . . . ?
C13 C14 C15 C16 -5.0(6) . . . . ?
C13 C12 C31 C32 103.2(4) . . . . ?
C25 C24 C43 C44 -96.9(4) . . . . ?
C12 C13 C33 C34 -75.0(4) . . . . ?
C9 C10 C11 N2 -179.3(3) . . . . ?
C9 C10 C11 C12 0.4(6) . . . . ?
C24 C23 C22 N4 -174.6(3) . . . . ?
C24 C23 C22 C21 5.4(6) . . . . ?
C24 C25 C45 C46 82.2(5) . . . . ?
C17 C16 C35 C36 99.2(4) . . . . ?
C16 C17 C37 C38 -83.5(4) . . . . ?
C28 C27 C26 N5 178.3(3) . . . . ?
C28 C27 C26 C25 -3.0(6) . . . . ?
C28 C29 C49 C50 92.1(4) . . . . ?
C21 C20 C39 C40 -95.7(5) . . . . ?
C21 C20 C51 C52 103.2(8) . . . . ?
C20 C19 C18 N3 177.7(3) . . . . ?
C20 C19 C18 C17 -0.9(6) . . . . ?
C20 C21 C41 C42 80.5(5) . . . . ?
C33 C13 C12 C11 -178.2(2) . . . . ?
C33 C13 C12 C31 0.2(4) . . . . ?
C49 C29 C28 C27 179.8(3) . . . . ?
C49 C29 C28 C47 -2.4(5) . . . . ?
C37 C17 C16 C15 -179.7(3) . . . . ?
C37 C17 C16 C35 4.1(5) . . . . ?
C45 C25 C24 C23 -179.7(3) . . . . ?
C45 C25 C24 C43 -2.2(4) . . . . ?
C41 C21 C20 C19 176.6(4) . . . . ?
C41 C21 C20 C39 5.1(6) . . . . ?
C41 C21 C20 C51 -23.7(9) . . . . ?

_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 1.308
_oxdiff_exptl_absorpt_empirical_full_min 0.688
_exptl_crystal_recrystallization_method 
'Slow reaction in chlorobenzene solution'
_exptl_crystal_preparation       'Magnetic properties,Conducting properties'
####################################################################### 
# 
# 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_ethac2i3_autored_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2394981'
loop_
_audit_author_name
_audit_author_address
'Toshio Naito'
;Ehime University
Japan
;
_audit_update_record             
;
2024-10-31 deposited with the CCDC.	2025-05-30 downloaded from the CCDC.
;
_audit_creation_date             2024-10-31
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        (EtHAC)2I3
_chemical_formula_moiety         'I3, 2(C50 H52 N6)'
_chemical_formula_sum            'C100 H104 I3 N12'
_chemical_formula_weight         1854.65
_chemical_melting_point          ?
_chemical_oxdiff_formula         C100H104N12I3
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'
I I -0.4742 1.8119 '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                   9.6360(2)
_cell_length_b                   14.7064(3)
_cell_length_c                   15.6387(3)
_cell_angle_alpha                105.686(2)
_cell_angle_beta                 99.166(2)
_cell_angle_gamma                104.270(2)
_cell_volume                     2006.26(8)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    29247
_cell_measurement_temperature    90
_cell_measurement_theta_max      31.3150
_cell_measurement_theta_min      2.2760
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.228
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83443
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic black'
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             947
_exptl_crystal_size_max          0.389
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.038
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0171
_diffrn_reflns_av_unetI/netI     0.0119
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26694
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.248
_diffrn_ambient_temperature      90
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.111
_diffrn_detector_type            'Rigaku Saturn724+ area detector'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  70.00   0.50    6.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50    6.00    --  -20.00  45.00  90.00  360
  3  ω   -110.00  70.00   0.50    6.00    --  -20.00  45.00 180.00  360
  4  ω   -110.00  70.00   0.50    6.00    --  -20.00  45.00 270.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Rigaku Varimax with Saturn'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0334360000
_diffrn_orient_matrix_UB_12      -0.0487457000
_diffrn_orient_matrix_UB_13      -0.0312541000
_diffrn_orient_matrix_UB_21      -0.0676290000
_diffrn_orient_matrix_UB_22      0.0106851000
_diffrn_orient_matrix_UB_23      -0.0092739000
_diffrn_orient_matrix_UB_31      0.0208928000
_diffrn_orient_matrix_UB_32      0.0166169000
_diffrn_orient_matrix_UB_33      -0.0359827000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Enhance (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                6589
_reflns_number_total             7035
_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 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b46 (Rigaku, 2016)'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.228
_refine_diff_density_min         -1.109
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         7035
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0416
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0444P)²+6.6667P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1038
_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 Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C37(H37A,H37B), C35(H35A,H35B), C43(H43A,H43B), C33(H33A,
 H33B), C45(H45A,H45B), C39(H39A,H39B), C49(H49A,H49B), C47(H47A,H47B),
 C41(H41A,H41B)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C8(H8)
2.c Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C32(H32A,H32B,H32C), C38(H38A,H38B,H38C), C48(H48A,H48B,
 H48C), C50(H50A,H50B,H50C), C34(H34A,H34B,H34C), C46(H46A,H46B,H46C), C40(H40A,
 H40B,H40C), C44(H44A,H44B,H44C), C42(H42A,H42B,H42C)
;
_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
I1 I 1.000000 0.000000 1.000000 0.04306(13) Uani 1 2 d S . P . .
I2 I 0.96711(3) 0.16515(2) 0.93593(2) 0.05016(12) Uani 1 1 d . . . . .
N1 N 0.8457(3) 0.62716(17) 0.65509(16) 0.0114(5) Uani 1 1 d . . . . .
N6 N 0.6418(3) 0.65277(17) 0.52855(16) 0.0114(5) Uani 1 1 d . . . . .
N4 N 0.6329(3) 0.35335(17) 0.31223(16) 0.0104(5) Uani 1 1 d . . . . .
N5 N 0.5310(3) 0.51461(17) 0.35801(16) 0.0117(5) Uani 1 1 d . . . . .
N2 N 0.9406(3) 0.46361(17) 0.61219(16) 0.0102(5) Uani 1 1 d . . . . .
N3 N 0.8369(3) 0.32763(17) 0.44062(16) 0.0113(5) Uani 1 1 d . . . . .
C6 C 0.6888(3) 0.5710(2) 0.50620(19) 0.0116(6) Uani 1 1 d . . . . .
C10 C 0.9484(3) 0.6189(2) 0.72328(19) 0.0122(6) Uani 1 1 d . . . . .
C1 C 0.7920(3) 0.5586(2) 0.56956(19) 0.0102(5) Uani 1 1 d . . . . .
C11 C 0.9996(3) 0.5316(2) 0.69998(19) 0.0120(6) Uani 1 1 d . . . . .
C2 C 0.8412(3) 0.4772(2) 0.54803(19) 0.0104(5) Uani 1 1 d . . . . .
C7 C 0.8023(3) 0.7118(2) 0.6826(2) 0.0135(6) Uani 1 1 d . . . . .
C5 C 0.6344(3) 0.5020(2) 0.42044(19) 0.0106(5) Uani 1 1 d . . . . .
C30 C 0.6926(3) 0.7254(2) 0.6145(2) 0.0135(6) Uani 1 1 d . . . . .
C3 C 0.7889(3) 0.4091(2) 0.46164(19) 0.0104(5) Uani 1 1 d . . . . .
C17 C 0.8571(3) 0.1831(2) 0.3637(2) 0.0136(6) Uani 1 1 d . . . . .
C25 C 0.3840(3) 0.5833(2) 0.2920(2) 0.0148(6) Uani 1 1 d . . . . .
C16 C 0.9510(3) 0.2170(2) 0.4539(2) 0.0132(6) Uani 1 1 d . . . . .
C26 C 0.4803(3) 0.5979(2) 0.3752(2) 0.0129(6) Uani 1 1 d . . . . .
C13 C 1.0982(3) 0.4022(2) 0.6798(2) 0.0128(6) Uani 1 1 d . . . . .
C9 C 0.9711(3) 0.7029(2) 0.7980(2) 0.0153(6) Uani 1 1 d . . . . .
H9 H 1.035745 0.719444 0.856321 0.018 Uiso 1 1 calc R U . . .
C27 C 0.5391(3) 0.6725(2) 0.4680(2) 0.0127(6) Uani 1 1 d . . . . .
C22 C 0.5222(3) 0.3586(2) 0.24548(19) 0.0129(6) Uani 1 1 d . . . . .
C29 C 0.6200(3) 0.7950(2) 0.6095(2) 0.0148(6) Uani 1 1 d . . . . .
C12 C 1.0988(3) 0.4938(2) 0.74308(19) 0.0130(6) Uani 1 1 d . . . . .
C8 C 0.8824(3) 0.7592(2) 0.7731(2) 0.0170(6) Uani 1 1 d . . . . .
H8 H 0.878066 0.820009 0.811909 0.020 Uiso 1 1 calc R U . . .
C14 C 0.9971(3) 0.3832(2) 0.59637(19) 0.0115(6) Uani 1 1 d . . . . .
C19 C 0.6733(3) 0.2666(2) 0.2868(2) 0.0131(6) Uani 1 1 d . . . . .
C23 C 0.4722(3) 0.4481(2) 0.26872(19) 0.0127(6) Uani 1 1 d . . . . .
C18 C 0.7836(3) 0.2529(2) 0.35538(19) 0.0121(6) Uani 1 1 d . . . . .
C4 C 0.6867(3) 0.4218(2) 0.39753(19) 0.0112(6) Uani 1 1 d . . . . .
C15 C 0.9385(3) 0.3088(2) 0.50316(19) 0.0109(5) Uani 1 1 d . . . . .
C31 C 1.1934(3) 0.5440(2) 0.8394(2) 0.0158(6) Uani 1 1 d . . . . .
H31A H 1.240140 0.614739 0.847407 0.019 Uiso 1 1 calc R U . . .
H31B H 1.273308 0.513553 0.847619 0.019 Uiso 1 1 calc R U . . .
C24 C 0.3792(3) 0.4918(2) 0.2270(2) 0.0145(6) Uani 1 1 d . . . . .
C28 C 0.5247(3) 0.7635(2) 0.5200(2) 0.0154(6) Uani 1 1 d . . . . .
C37 C 0.8439(3) 0.0874(2) 0.2919(2) 0.0175(6) Uani 1 1 d . . . . .
H37A H 0.943143 0.078736 0.295384 0.021 Uiso 1 1 calc R U . . .
H37B H 0.808896 0.092303 0.230769 0.021 Uiso 1 1 calc R U . . .
C35 C 1.0388(3) 0.1583(2) 0.4896(2) 0.0169(6) Uani 1 1 d . . . . .
H35A H 1.140418 0.201915 0.521436 0.020 Uiso 1 1 calc R U . . .
H35B H 1.044914 0.104447 0.437735 0.020 Uiso 1 1 calc R U . . .
C20 C 0.5816(3) 0.2136(2) 0.1985(2) 0.0173(6) Uani 1 1 d . . . . .
C21 C 0.4905(3) 0.2694(2) 0.1733(2) 0.0170(6) Uani 1 1 d . . . . .
C36 C 0.9681(4) 0.1134(2) 0.5562(2) 0.0222(7) Uani 1 1 d . . . . .
H36A H 0.875037 0.061490 0.522401 0.033 Uiso 1 1 calc R U . . .
H36B H 0.948860 0.165396 0.602750 0.033 Uiso 1 1 calc R U . . .
H36C H 1.035421 0.084728 0.586023 0.033 Uiso 1 1 calc R U . . .
C43 C 0.2894(3) 0.4554(2) 0.1296(2) 0.0183(6) Uani 1 1 d . . . . .
H43A H 0.220227 0.494457 0.123868 0.022 Uiso 1 1 calc R U . . .
H43B H 0.230259 0.385188 0.113950 0.022 Uiso 1 1 calc R U . . .
C33 C 1.1950(3) 0.3423(2) 0.7050(2) 0.0157(6) Uani 1 1 d . . . . .
H33A H 1.298167 0.386255 0.729646 0.019 Uiso 1 1 calc R U . . .
H33B H 1.191970 0.289965 0.648857 0.019 Uiso 1 1 calc R U . . .
C45 C 0.2984(3) 0.6503(2) 0.2693(2) 0.0206(7) Uani 1 1 d . . . . .
H45A H 0.300684 0.700187 0.327034 0.025 Uiso 1 1 calc R U . . .
H45B H 0.194186 0.610233 0.240571 0.025 Uiso 1 1 calc R U . . .
C32 C 1.1091(4) 0.5379(3) 0.9144(2) 0.0216(7) Uani 1 1 d . . . . .
H32A H 1.060922 0.468201 0.906516 0.032 Uiso 1 1 calc R U . . .
H32B H 1.034232 0.572110 0.909644 0.032 Uiso 1 1 calc R U . . .
H32C H 1.178320 0.569485 0.974666 0.032 Uiso 1 1 calc R U . . .
C39 C 0.5672(4) 0.1102(2) 0.1406(2) 0.0240(7) Uani 1 1 d . . . . .
H39A H 0.465084 0.079321 0.102100 0.029 Uiso 1 1 calc R U . . .
H39B H 0.582879 0.070843 0.181535 0.029 Uiso 1 1 calc R U . . .
C38 C 0.7390(4) -0.0047(2) 0.3011(2) 0.0260(7) Uani 1 1 d . . . . .
H38A H 0.733633 -0.063468 0.251191 0.039 Uiso 1 1 calc R U . . .
H38B H 0.640432 0.003214 0.298079 0.039 Uiso 1 1 calc R U . . .
H38C H 0.775858 -0.012523 0.359975 0.039 Uiso 1 1 calc R U . . .
C48 C 0.5062(4) 0.8804(2) 0.4306(2) 0.0241(7) Uani 1 1 d . . . . .
H48A H 0.528396 0.834039 0.380612 0.036 Uiso 1 1 calc R U . . .
H48B H 0.597686 0.931769 0.468284 0.036 Uiso 1 1 calc R U . . .
H48C H 0.438031 0.911467 0.405146 0.036 Uiso 1 1 calc R U . . .
C50 C 0.7509(4) 0.9804(2) 0.6816(2) 0.0212(7) Uani 1 1 d . . . . .
H50A H 0.721813 0.989100 0.622040 0.032 Uiso 1 1 calc R U . . .
H50B H 0.849494 0.972082 0.689178 0.032 Uiso 1 1 calc R U . . .
H50C H 0.752466 1.038979 0.730455 0.032 Uiso 1 1 calc R U . . .
C49 C 0.6405(4) 0.8888(2) 0.6863(2) 0.0190(6) Uani 1 1 d . . . . .
H49A H 0.673945 0.878698 0.745316 0.023 Uiso 1 1 calc R U . . .
H49B H 0.543805 0.900986 0.685338 0.023 Uiso 1 1 calc R U . . .
C47 C 0.4347(4) 0.8242(2) 0.4899(2) 0.0207(7) Uani 1 1 d . . . . .
H47A H 0.423607 0.872248 0.544496 0.025 Uiso 1 1 calc R U . . .
H47B H 0.334915 0.779990 0.454533 0.025 Uiso 1 1 calc R U . . .
C41 C 0.3709(4) 0.2318(2) 0.0856(2) 0.0245(7) Uani 1 1 d . . . . .
H41A H 0.309103 0.276840 0.090002 0.029 Uiso 1 1 calc R U . . .
H41B H 0.306965 0.165711 0.080730 0.029 Uiso 1 1 calc R U . . .
C34 C 1.1503(4) 0.2937(3) 0.7756(2) 0.0252(7) Uani 1 1 d . . . . .
H34A H 1.046410 0.253213 0.753562 0.038 Uiso 1 1 calc R U . . .
H34B H 1.163839 0.345198 0.833844 0.038 Uiso 1 1 calc R U . . .
H34C H 1.211957 0.251499 0.784651 0.038 Uiso 1 1 calc R U . . .
C46 C 0.3564(4) 0.7046(3) 0.2053(2) 0.0287(8) Uani 1 1 d . . . . .
H46A H 0.341651 0.656381 0.144906 0.043 Uiso 1 1 calc R U . . .
H46B H 0.461846 0.740058 0.230530 0.043 Uiso 1 1 calc R U . . .
H46C H 0.302706 0.752047 0.199446 0.043 Uiso 1 1 calc R U . . .
C40 C 0.6738(4) 0.1042(3) 0.0787(2) 0.0315(8) Uani 1 1 d . . . . .
H40A H 0.652306 0.136781 0.033436 0.047 Uiso 1 1 calc R U . . .
H40B H 0.662475 0.034473 0.047216 0.047 Uiso 1 1 calc R U . . .
H40C H 0.775248 0.137410 0.115696 0.047 Uiso 1 1 calc R U . . .
C44 C 0.3865(4) 0.4642(3) 0.0619(2) 0.0242(7) Uani 1 1 d . . . . .
H44A H 0.324502 0.435567 -0.000771 0.036 Uiso 1 1 calc R U . . .
H44B H 0.458413 0.428289 0.069395 0.036 Uiso 1 1 calc R U . . .
H44C H 0.438627 0.534199 0.073659 0.036 Uiso 1 1 calc R U . . .
C42 C 0.4238(5) 0.2230(3) -0.0023(2) 0.0378(9) Uani 1 1 d . . . . .
H42A H 0.343290 0.218752 -0.051612 0.057 Uiso 1 1 calc R U . . .
H42B H 0.454709 0.163216 -0.019107 0.057 Uiso 1 1 calc R U . . .
H42C H 0.507483 0.281454 0.007431 0.057 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 I2 2.9321(3) . ?
I1 I2 2.9322(3) 2_757 ?
N1 C10 1.388(4) . ?
N1 C1 1.366(4) . ?
N1 C7 1.390(4) . ?
N6 C6 1.366(4) . ?
N6 C30 1.394(4) . ?
N6 C27 1.397(4) . ?
N4 C22 1.401(4) . ?
N4 C19 1.399(4) . ?
N4 C4 1.363(4) . ?
N5 C5 1.364(4) . ?
N5 C26 1.404(4) . ?
N5 C23 1.401(4) . ?
N2 C11 1.392(4) . ?
N2 C2 1.364(4) . ?
N2 C14 1.400(4) . ?
N3 C3 1.366(4) . ?
N3 C18 1.400(4) . ?
N3 C15 1.402(4) . ?
C6 C1 1.370(4) . ?
C6 C5 1.371(4) . ?
C10 C11 1.463(4) . ?
C10 C9 1.395(4) . ?
C1 C2 1.372(4) . ?
C11 C12 1.393(4) . ?
C2 C3 1.373(4) . ?
C7 C30 1.467(4) . ?
C7 C8 1.392(4) . ?
C5 C4 1.377(4) . ?
C30 C29 1.387(4) . ?
C3 C4 1.373(4) . ?
C17 C16 1.430(4) . ?
C17 C18 1.405(4) . ?
C17 C37 1.506(4) . ?
C25 C26 1.401(4) . ?
C25 C24 1.436(4) . ?
C25 C45 1.508(4) . ?
C16 C15 1.406(4) . ?
C16 C35 1.499(4) . ?
C26 C27 1.484(4) . ?
C13 C12 1.437(4) . ?
C13 C14 1.412(4) . ?
C13 C33 1.509(4) . ?
C9 H9 0.9500 . ?
C9 C8 1.409(4) . ?
C27 C28 1.419(4) . ?
C22 C23 1.486(4) . ?
C22 C21 1.407(4) . ?
C29 C28 1.431(4) . ?
C29 C49 1.509(4) . ?
C12 C31 1.508(4) . ?
C8 H8 0.9500 . ?
C14 C15 1.487(4) . ?
C19 C18 1.477(4) . ?
C19 C20 1.408(4) . ?
C23 C24 1.401(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.539(4) . ?
C24 C43 1.506(4) . ?
C28 C47 1.499(4) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.534(4) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.537(4) . ?
C20 C21 1.421(4) . ?
C20 C39 1.505(4) . ?
C21 C41 1.513(4) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.530(4) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.531(4) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.530(5) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.522(5) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C48 C47 1.535(4) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C50 C49 1.526(4) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.524(5) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?

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
I2 I1 I2 180.0 . 2_757 ?
C10 N1 C7 113.3(2) . . ?
C1 N1 C10 123.2(2) . . ?
C1 N1 C7 123.4(2) . . ?
C6 N6 C30 123.0(2) . . ?
C6 N6 C27 123.7(2) . . ?
C30 N6 C27 113.2(2) . . ?
C19 N4 C22 113.9(2) . . ?
C4 N4 C22 123.2(2) . . ?
C4 N4 C19 122.6(2) . . ?
C5 N5 C26 123.3(2) . . ?
C5 N5 C23 122.8(2) . . ?
C23 N5 C26 113.8(2) . . ?
C11 N2 C14 113.4(2) . . ?
C2 N2 C11 122.4(2) . . ?
C2 N2 C14 124.2(2) . . ?
C3 N3 C18 122.7(2) . . ?
C3 N3 C15 123.4(2) . . ?
C18 N3 C15 113.9(2) . . ?
N6 C6 C1 119.7(3) . . ?
N6 C6 C5 120.3(3) . . ?
C1 C6 C5 120.0(3) . . ?
N1 C10 C11 116.8(2) . . ?
N1 C10 C9 104.3(2) . . ?
C9 C10 C11 138.9(3) . . ?
N1 C1 C6 119.9(3) . . ?
N1 C1 C2 119.6(3) . . ?
C6 C1 C2 120.5(3) . . ?
N2 C11 C10 117.7(2) . . ?
N2 C11 C12 105.2(2) . . ?
C12 C11 C10 137.1(3) . . ?
N2 C2 C1 120.2(3) . . ?
N2 C2 C3 120.2(3) . . ?
C1 C2 C3 119.6(3) . . ?
N1 C7 C30 116.6(2) . . ?
N1 C7 C8 104.2(3) . . ?
C8 C7 C30 139.2(3) . . ?
N5 C5 C6 119.6(3) . . ?
N5 C5 C4 120.6(3) . . ?
C6 C5 C4 119.8(3) . . ?
N6 C30 C7 117.3(2) . . ?
C29 C30 N6 105.4(3) . . ?
C29 C30 C7 137.3(3) . . ?
N3 C3 C2 119.5(3) . . ?
N3 C3 C4 120.3(3) . . ?
C2 C3 C4 120.2(3) . . ?
C16 C17 C37 123.6(3) . . ?
C18 C17 C16 108.9(2) . . ?
C18 C17 C37 127.5(3) . . ?
C26 C25 C24 108.9(3) . . ?
C26 C25 C45 127.9(3) . . ?
C24 C25 C45 123.2(3) . . ?
C17 C16 C35 123.8(3) . . ?
C15 C16 C17 109.3(3) . . ?
C15 C16 C35 126.8(3) . . ?
N5 C26 C27 117.0(2) . . ?
C25 C26 N5 104.1(2) . . ?
C25 C26 C27 138.9(3) . . ?
C12 C13 C33 122.1(3) . . ?
C14 C13 C12 108.6(2) . . ?
C14 C13 C33 129.3(3) . . ?
C10 C9 H9 125.5 . . ?
C10 C9 C8 108.9(3) . . ?
C8 C9 H9 125.5 . . ?
N6 C27 C26 116.0(2) . . ?
N6 C27 C28 104.0(2) . . ?
C28 C27 C26 140.0(3) . . ?
N4 C22 C23 116.8(2) . . ?
N4 C22 C21 104.0(2) . . ?
C21 C22 C23 139.3(3) . . ?
C30 C29 C28 108.8(3) . . ?
C30 C29 C49 125.0(3) . . ?
C28 C29 C49 126.2(3) . . ?
C11 C12 C13 108.7(2) . . ?
C11 C12 C31 124.5(3) . . ?
C13 C12 C31 126.8(3) . . ?
C7 C8 C9 109.3(3) . . ?
C7 C8 H8 125.4 . . ?
C9 C8 H8 125.4 . . ?
N2 C14 C13 104.2(2) . . ?
N2 C14 C15 115.4(2) . . ?
C13 C14 C15 140.4(3) . . ?
N4 C19 C18 117.2(2) . . ?
N4 C19 C20 103.7(2) . . ?
C20 C19 C18 138.9(3) . . ?
N5 C23 C22 116.7(2) . . ?
N5 C23 C24 104.0(2) . . ?
C24 C23 C22 139.3(3) . . ?
N3 C18 C17 104.2(2) . . ?
N3 C18 C19 116.8(2) . . ?
C17 C18 C19 139.0(3) . . ?
N4 C4 C5 119.8(3) . . ?
N4 C4 C3 120.2(3) . . ?
C3 C4 C5 119.9(3) . . ?
N3 C15 C16 103.8(2) . . ?
N3 C15 C14 117.3(2) . . ?
C16 C15 C14 138.9(3) . . ?
C12 C31 H31A 108.7 . . ?
C12 C31 H31B 108.7 . . ?
C12 C31 C32 114.3(2) . . ?
H31A C31 H31B 107.6 . . ?
C32 C31 H31A 108.7 . . ?
C32 C31 H31B 108.7 . . ?
C25 C24 C43 122.5(3) . . ?
C23 C24 C25 109.2(3) . . ?
C23 C24 C43 128.2(3) . . ?
C27 C28 C29 108.6(3) . . ?
C27 C28 C47 128.5(3) . . ?
C29 C28 C47 122.8(3) . . ?
C17 C37 H37A 108.7 . . ?
C17 C37 H37B 108.7 . . ?
C17 C37 C38 114.1(3) . . ?
H37A C37 H37B 107.6 . . ?
C38 C37 H37A 108.7 . . ?
C38 C37 H37B 108.7 . . ?
C16 C35 H35A 109.4 . . ?
C16 C35 H35B 109.4 . . ?
C16 C35 C36 111.2(2) . . ?
H35A C35 H35B 108.0 . . ?
C36 C35 H35A 109.4 . . ?
C36 C35 H35B 109.4 . . ?
C19 C20 C21 109.4(3) . . ?
C19 C20 C39 127.3(3) . . ?
C21 C20 C39 123.1(3) . . ?
C22 C21 C20 109.0(3) . . ?
C22 C21 C41 127.1(3) . . ?
C20 C21 C41 123.8(3) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C24 C43 H43A 109.2 . . ?
C24 C43 H43B 109.2 . . ?
C24 C43 C44 112.1(2) . . ?
H43A C43 H43B 107.9 . . ?
C44 C43 H43A 109.2 . . ?
C44 C43 H43B 109.2 . . ?
C13 C33 H33A 108.8 . . ?
C13 C33 H33B 108.8 . . ?
C13 C33 C34 113.9(3) . . ?
H33A C33 H33B 107.7 . . ?
C34 C33 H33A 108.8 . . ?
C34 C33 H33B 108.8 . . ?
C25 C45 H45A 108.7 . . ?
C25 C45 H45B 108.7 . . ?
C25 C45 C46 114.4(3) . . ?
H45A C45 H45B 107.6 . . ?
C46 C45 H45A 108.7 . . ?
C46 C45 H45B 108.7 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C20 C39 H39A 108.6 . . ?
C20 C39 H39B 108.6 . . ?
C20 C39 C40 114.7(3) . . ?
H39A C39 H39B 107.6 . . ?
C40 C39 H39A 108.6 . . ?
C40 C39 H39B 108.6 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
C29 C49 C50 114.1(3) . . ?
C29 C49 H49A 108.7 . . ?
C29 C49 H49B 108.7 . . ?
C50 C49 H49A 108.7 . . ?
C50 C49 H49B 108.7 . . ?
H49A C49 H49B 107.6 . . ?
C28 C47 C48 111.8(3) . . ?
C28 C47 H47A 109.3 . . ?
C28 C47 H47B 109.3 . . ?
C48 C47 H47A 109.3 . . ?
C48 C47 H47B 109.3 . . ?
H47A C47 H47B 107.9 . . ?
C21 C41 H41A 108.3 . . ?
C21 C41 H41B 108.3 . . ?
C21 C41 C42 115.9(3) . . ?
H41A C41 H41B 107.4 . . ?
C42 C41 H41A 108.3 . . ?
C42 C41 H41B 108.3 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C10 C11 N2 -0.7(4) . . . . ?
N1 C10 C11 C12 178.7(3) . . . . ?
N1 C10 C9 C8 -0.1(3) . . . . ?
N1 C1 C2 N2 1.4(4) . . . . ?
N1 C1 C2 C3 -179.0(2) . . . . ?
N1 C7 C30 N6 -0.1(4) . . . . ?
N1 C7 C30 C29 -179.1(3) . . . . ?
N1 C7 C8 C9 -0.1(3) . . . . ?
N6 C6 C1 N1 1.0(4) . . . . ?
N6 C6 C1 C2 -179.6(3) . . . . ?
N6 C6 C5 N5 -1.2(4) . . . . ?
N6 C6 C5 C4 177.5(3) . . . . ?
N6 C30 C29 C28 0.2(3) . . . . ?
N6 C30 C29 C49 -179.3(3) . . . . ?
N6 C27 C28 C29 0.3(3) . . . . ?
N6 C27 C28 C47 176.9(3) . . . . ?
N4 C22 C23 N5 -5.4(4) . . . . ?
N4 C22 C23 C24 173.7(3) . . . . ?
N4 C22 C21 C20 0.2(3) . . . . ?
N4 C22 C21 C41 175.2(3) . . . . ?
N4 C19 C18 N3 0.8(4) . . . . ?
N4 C19 C18 C17 179.9(3) . . . . ?
N4 C19 C20 C21 0.4(3) . . . . ?
N4 C19 C20 C39 -174.2(3) . . . . ?
N5 C5 C4 N4 -1.1(4) . . . . ?
N5 C5 C4 C3 -178.8(3) . . . . ?
N5 C26 C27 N6 1.2(4) . . . . ?
N5 C26 C27 C28 -178.4(3) . . . . ?
N5 C23 C24 C25 -0.1(3) . . . . ?
N5 C23 C24 C43 177.9(3) . . . . ?
N2 C11 C12 C13 0.0(3) . . . . ?
N2 C11 C12 C31 178.2(3) . . . . ?
N2 C2 C3 N3 0.2(4) . . . . ?
N2 C2 C3 C4 178.8(3) . . . . ?
N2 C14 C15 N3 1.6(4) . . . . ?
N2 C14 C15 C16 -176.7(3) . . . . ?
N3 C3 C4 N4 -0.3(4) . . . . ?
N3 C3 C4 C5 177.4(3) . . . . ?
C6 N6 C30 C7 0.4(4) . . . . ?
C6 N6 C30 C29 179.7(3) . . . . ?
C6 N6 C27 C26 0.4(4) . . . . ?
C6 N6 C27 C28 -179.9(2) . . . . ?
C6 C1 C2 N2 -178.0(3) . . . . ?
C6 C1 C2 C3 1.5(4) . . . . ?
C6 C5 C4 N4 -179.8(3) . . . . ?
C6 C5 C4 C3 2.5(4) . . . . ?
C10 N1 C1 C6 178.9(3) . . . . ?
C10 N1 C1 C2 -0.5(4) . . . . ?
C10 N1 C7 C30 -179.4(2) . . . . ?
C10 N1 C7 C8 0.1(3) . . . . ?
C10 C11 C12 C13 -179.5(3) . . . . ?
C10 C11 C12 C31 -1.3(5) . . . . ?
C10 C9 C8 C7 0.2(3) . . . . ?
C1 N1 C10 C11 0.1(4) . . . . ?
C1 N1 C10 C9 -179.6(3) . . . . ?
C1 N1 C7 C30 0.3(4) . . . . ?
C1 N1 C7 C8 179.7(3) . . . . ?
C1 C6 C5 N5 179.6(3) . . . . ?
C1 C6 C5 C4 -1.7(4) . . . . ?
C1 C2 C3 N3 -179.4(3) . . . . ?
C1 C2 C3 C4 -0.8(4) . . . . ?
C11 N2 C2 C1 -2.0(4) . . . . ?
C11 N2 C2 C3 178.4(3) . . . . ?
C11 N2 C14 C13 0.0(3) . . . . ?
C11 N2 C14 C15 -179.5(2) . . . . ?
C11 C10 C9 C8 -179.8(3) . . . . ?
C11 C12 C31 C32 74.7(4) . . . . ?
C2 N2 C11 C10 1.6(4) . . . . ?
C2 N2 C11 C12 -178.0(2) . . . . ?
C2 N2 C14 C13 177.9(2) . . . . ?
C2 N2 C14 C15 -1.5(4) . . . . ?
C2 C3 C4 N4 -178.9(3) . . . . ?
C2 C3 C4 C5 -1.3(4) . . . . ?
C7 N1 C10 C11 179.8(2) . . . . ?
C7 N1 C10 C9 0.1(3) . . . . ?
C7 N1 C1 C6 -0.7(4) . . . . ?
C7 N1 C1 C2 179.8(3) . . . . ?
C7 C30 C29 C28 179.3(3) . . . . ?
C7 C30 C29 C49 -0.2(6) . . . . ?
C5 N5 C26 C25 176.4(3) . . . . ?
C5 N5 C26 C27 -2.9(4) . . . . ?
C5 N5 C23 C22 3.0(4) . . . . ?
C5 N5 C23 C24 -176.4(2) . . . . ?
C5 C6 C1 N1 -179.7(3) . . . . ?
C5 C6 C1 C2 -0.3(4) . . . . ?
C30 N6 C6 C1 -0.9(4) . . . . ?
C30 N6 C6 C5 179.9(3) . . . . ?
C30 N6 C27 C26 -179.9(2) . . . . ?
C30 N6 C27 C28 -0.2(3) . . . . ?
C30 C7 C8 C9 179.1(3) . . . . ?
C30 C29 C28 C27 -0.3(3) . . . . ?
C30 C29 C28 C47 -177.2(3) . . . . ?
C30 C29 C49 C50 95.9(4) . . . . ?
C3 N3 C18 C17 -178.1(2) . . . . ?
C3 N3 C18 C19 1.3(4) . . . . ?
C3 N3 C15 C16 177.9(2) . . . . ?
C3 N3 C15 C14 -0.9(4) . . . . ?
C17 C16 C15 N3 -0.2(3) . . . . ?
C17 C16 C15 C14 178.2(3) . . . . ?
C17 C16 C35 C36 -104.4(3) . . . . ?
C25 C26 C27 N6 -177.7(3) . . . . ?
C25 C26 C27 C28 2.7(7) . . . . ?
C25 C24 C43 C44 107.6(3) . . . . ?
C16 C17 C18 N3 0.7(3) . . . . ?
C16 C17 C18 C19 -178.5(3) . . . . ?
C16 C17 C37 C38 81.8(4) . . . . ?
C26 N5 C5 C6 2.9(4) . . . . ?
C26 N5 C5 C4 -175.8(3) . . . . ?
C26 N5 C23 C22 179.4(2) . . . . ?
C26 N5 C23 C24 0.1(3) . . . . ?
C26 C25 C24 C23 0.0(3) . . . . ?
C26 C25 C24 C43 -178.0(3) . . . . ?
C26 C25 C45 C46 107.8(4) . . . . ?
C26 C27 C28 C29 179.9(3) . . . . ?
C26 C27 C28 C47 -3.4(6) . . . . ?
C13 C12 C31 C32 -107.4(3) . . . . ?
C13 C14 C15 N3 -177.6(3) . . . . ?
C13 C14 C15 C16 4.2(6) . . . . ?
C9 C10 C11 N2 179.0(3) . . . . ?
C9 C10 C11 C12 -1.6(6) . . . . ?
C27 N6 C6 C1 178.8(3) . . . . ?
C27 N6 C6 C5 -0.4(4) . . . . ?
C27 N6 C30 C7 -179.3(2) . . . . ?
C27 N6 C30 C29 0.0(3) . . . . ?
C27 C28 C47 C48 -75.4(4) . . . . ?
C22 N4 C19 C18 -176.7(2) . . . . ?
C22 N4 C19 C20 -0.3(3) . . . . ?
C22 N4 C4 C5 -1.7(4) . . . . ?
C22 N4 C4 C3 176.0(3) . . . . ?
C22 C23 C24 C25 -179.2(3) . . . . ?
C22 C23 C24 C43 -1.3(6) . . . . ?
C22 C21 C41 C42 115.1(4) . . . . ?
C29 C28 C47 C48 100.8(3) . . . . ?
C12 C13 C14 N2 0.0(3) . . . . ?
C12 C13 C14 C15 179.2(3) . . . . ?
C12 C13 C33 C34 69.4(4) . . . . ?
C8 C7 C30 N6 -179.3(3) . . . . ?
C8 C7 C30 C29 1.7(7) . . . . ?
C14 N2 C11 C10 179.6(2) . . . . ?
C14 N2 C11 C12 0.0(3) . . . . ?
C14 N2 C2 C1 -179.8(3) . . . . ?
C14 N2 C2 C3 0.6(4) . . . . ?
C14 C13 C12 C11 0.0(3) . . . . ?
C14 C13 C12 C31 -178.1(3) . . . . ?
C14 C13 C33 C34 -111.3(3) . . . . ?
C19 N4 C22 C23 179.0(2) . . . . ?
C19 N4 C22 C21 0.1(3) . . . . ?
C19 N4 C4 C5 -175.2(3) . . . . ?
C19 N4 C4 C3 2.5(4) . . . . ?
C19 C20 C21 C22 -0.4(4) . . . . ?
C19 C20 C21 C41 -175.5(3) . . . . ?
C19 C20 C39 C40 -89.4(4) . . . . ?
C23 N5 C5 C6 179.0(3) . . . . ?
C23 N5 C5 C4 0.3(4) . . . . ?
C23 N5 C26 C25 0.0(3) . . . . ?
C23 N5 C26 C27 -179.3(2) . . . . ?
C23 C22 C21 C20 -178.3(3) . . . . ?
C23 C22 C21 C41 -3.3(6) . . . . ?
C23 C24 C43 C44 -70.0(4) . . . . ?
C18 N3 C3 C2 177.0(3) . . . . ?
C18 N3 C3 C4 -1.6(4) . . . . ?
C18 N3 C15 C16 0.6(3) . . . . ?
C18 N3 C15 C14 -178.2(2) . . . . ?
C18 C17 C16 C15 -0.3(3) . . . . ?
C18 C17 C16 C35 175.7(3) . . . . ?
C18 C17 C37 C38 -98.5(4) . . . . ?
C18 C19 C20 C21 175.6(3) . . . . ?
C18 C19 C20 C39 1.0(6) . . . . ?
C4 N4 C22 C23 4.9(4) . . . . ?
C4 N4 C22 C21 -174.0(3) . . . . ?
C4 N4 C19 C18 -2.7(4) . . . . ?
C4 N4 C19 C20 173.8(3) . . . . ?
C15 N3 C3 C2 0.0(4) . . . . ?
C15 N3 C3 C4 -178.6(3) . . . . ?
C15 N3 C18 C17 -0.8(3) . . . . ?
C15 N3 C18 C19 178.5(2) . . . . ?
C15 C16 C35 C36 70.9(4) . . . . ?
C24 C25 C26 N5 0.0(3) . . . . ?
C24 C25 C26 C27 179.0(3) . . . . ?
C24 C25 C45 C46 -71.0(4) . . . . ?
C28 C29 C49 C50 -83.5(4) . . . . ?
C37 C17 C16 C15 179.4(3) . . . . ?
C37 C17 C16 C35 -4.6(4) . . . . ?
C37 C17 C18 N3 -179.0(3) . . . . ?
C37 C17 C18 C19 1.8(6) . . . . ?
C35 C16 C15 N3 -176.1(3) . . . . ?
C35 C16 C15 C14 2.3(6) . . . . ?
C20 C19 C18 N3 -174.0(3) . . . . ?
C20 C19 C18 C17 5.1(7) . . . . ?
C20 C21 C41 C42 -70.6(4) . . . . ?
C21 C22 C23 N5 172.9(3) . . . . ?
C21 C22 C23 C24 -8.0(6) . . . . ?
C21 C20 C39 C40 96.7(4) . . . . ?
C33 C13 C12 C11 179.5(3) . . . . ?
C33 C13 C12 C31 1.3(4) . . . . ?
C33 C13 C14 N2 -179.4(3) . . . . ?
C33 C13 C14 C15 -0.2(6) . . . . ?
C45 C25 C26 N5 -178.9(3) . . . . ?
C45 C25 C26 C27 0.1(6) . . . . ?
C45 C25 C24 C23 179.0(3) . . . . ?
C45 C25 C24 C43 0.9(4) . . . . ?
C39 C20 C21 C22 174.5(3) . . . . ?
C39 C20 C21 C41 -0.7(5) . . . . ?
C49 C29 C28 C27 179.1(3) . . . . ?
C49 C29 C28 C47 2.3(5) . . . . ?

_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 1.341
_oxdiff_exptl_absorpt_empirical_full_min 0.711
_exptl_crystal_recrystallization_method 
'Slow reaction in chlorobenzene solution'
_exptl_crystal_preparation       'Magnetic properties,Conducting properties'
####################################################################### 
# 
# 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_ethac2i3_autored_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2394977'
loop_
_audit_author_name
_audit_author_address
'Toshio Naito'
;Ehime University
Japan
;
_audit_update_record             
;
2024-10-31 deposited with the CCDC.	2025-05-30 downloaded from the CCDC.
;
_audit_creation_date             2024-10-23
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        (EtHAC)2I3
_chemical_formula_moiety         'C50 H52 N6, 0.5(I3)'
_chemical_formula_sum            'C50 H52 I1.50 N6'
_chemical_formula_weight         927.32
_chemical_melting_point          ?
_chemical_oxdiff_formula         C100H104N12I3
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'
I I -0.4742 1.8119 '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      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                   9.7154(3)
_cell_length_b                   14.9261(5)
_cell_length_c                   15.5667(6)
_cell_angle_alpha                107.052(3)
_cell_angle_beta                 98.431(3)
_cell_angle_gamma                103.277(3)
_cell_volume                     2044.17(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    17714
_cell_measurement_temperature    250
_cell_measurement_theta_max      31.3100
_cell_measurement_theta_min      2.6700
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.205
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85237
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             947
_exptl_crystal_size_max          0.389
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.038
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34686
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         2.284
_diffrn_ambient_temperature      250
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 7.111
_diffrn_detector_type            'Rigaku Saturn724+ area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50    6.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50    6.00    --  -20.00  45.00  90.00  360
  3  ω   -110.00  70.00   0.50    6.00    --  -20.00  45.00 180.00  360
  4  ω   -110.00  70.00   0.50    6.00    --  -20.00  45.00 270.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Rigaku Varimax with Saturn'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0272578000
_diffrn_orient_matrix_UB_12      0.0489974000
_diffrn_orient_matrix_UB_13      0.0308120000
_diffrn_orient_matrix_UB_21      0.0689659000
_diffrn_orient_matrix_UB_22      -0.0073580000
_diffrn_orient_matrix_UB_23      0.0114703000
_diffrn_orient_matrix_UB_31      0.0210188000
_diffrn_orient_matrix_UB_32      0.0154855000
_diffrn_orient_matrix_UB_33      -0.0362961000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'MicroMax 007'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6585
_reflns_number_total             9853
_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 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b46 (Rigaku, 2016)'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.949
_refine_diff_density_min         -1.034
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         9853
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0622
_refine_ls_restrained_S_all      1.136
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1112P)²+0.5797P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1866
_refine_ls_wR_factor_ref         0.2045
_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
 I2-I1 = I1-I3
 2.98 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C41 \\sim C42: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
Uanis(I3) \\sim Ueq, Uanis(I1) \\sim Ueq, Uanis(I2) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 I3, I1, I2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
 C41, C42
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(C51)=Sof(H51A)=Sof(H51B)=1-FVAR(1)
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(1)
 Fixed Sof: I2(0.5) I1(0.5) I3(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C33(H33A,H33B), C49(H49A,H49B), C35(H35A,H35B), C37(H37A,
 H37B), C47(H47A,H47B), C43(H43A,H43B), C45(H45A,H45B), C41(H41A,H41B),
 C39(H39A,H39B), C51(H51A,H51B)
6.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C8(H8)
6.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C50(H50A,H50B,H50C), C38(H38A,H38B,H38C), C36(H36A,H36B,
 H36C), C34(H34A,H34B,H34C), C48(H48A,H48B,H48C), C44(H44A,H44B,H44C), C46(H46A,
 H46B,H46C), C42(H42A,H42B,H42C), C40(H40A,H40B,H40C), C52(H52A,H52B,H52C)
;
_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
N2 N 0.94047(19) 0.46804(13) 0.61288(12) 0.0370(4) Uani 1 1 d . . . . .
N1 N 0.8408(2) 0.62836(13) 0.65188(12) 0.0372(4) Uani 1 1 d . . . . .
N6 N 0.6375(2) 0.64674(13) 0.52302(13) 0.0388(4) Uani 1 1 d . . . . .
N4 N 0.6381(2) 0.34538(13) 0.31175(12) 0.0376(4) Uani 1 1 d . . . . .
N5 N 0.5317(2) 0.50409(14) 0.35382(13) 0.0390(4) Uani 1 1 d . . . . .
N3 N 0.8430(2) 0.32776(13) 0.44194(13) 0.0383(4) Uani 1 1 d . . . . .
C1 C 0.7901(2) 0.55773(15) 0.56753(14) 0.0341(4) Uani 1 1 d . . . . .
C2 C 0.8411(2) 0.47763(15) 0.54700(14) 0.0339(4) Uani 1 1 d . . . . .
C3 C 0.7922(2) 0.40778(15) 0.46182(14) 0.0332(4) Uani 1 1 d . . . . .
C4 C 0.6890(2) 0.41622(15) 0.39663(14) 0.0338(4) Uani 1 1 d . . . . .
C5 C 0.6353(2) 0.49507(16) 0.41792(14) 0.0346(4) Uani 1 1 d . . . . .
C10 C 0.9429(2) 0.62345(17) 0.72136(15) 0.0404(5) Uani 1 1 d . . . . .
C11 C 0.9965(2) 0.53796(17) 0.70003(15) 0.0395(5) Uani 1 1 d . . . . .
C6 C 0.6865(2) 0.56608(15) 0.50252(15) 0.0350(4) Uani 1 1 d . . . . .
C14 C 0.9987(2) 0.38891(17) 0.59857(16) 0.0378(5) Uani 1 1 d . . . . .
C30 C 0.6856(3) 0.72110(17) 0.60815(17) 0.0428(5) Uani 1 1 d . . . . .
C7 C 0.7944(3) 0.71152(16) 0.67774(16) 0.0422(5) Uani 1 1 d . . . . .
C12 C 1.0959(2) 0.5024(2) 0.74443(17) 0.0451(6) Uani 1 1 d . . . . .
C15 C 0.9420(2) 0.31200(17) 0.50636(17) 0.0398(5) Uani 1 1 d . . . . .
C13 C 1.0986(2) 0.4117(2) 0.68284(18) 0.0453(6) Uani 1 1 d . . . . .
C29 C 0.6105(3) 0.78813(19) 0.6013(2) 0.0518(6) Uani 1 1 d . . . . .
C19 C 0.6840(3) 0.26194(17) 0.28753(16) 0.0438(5) Uani 1 1 d . . . . .
C22 C 0.5296(3) 0.34822(18) 0.24352(15) 0.0438(5) Uani 1 1 d . . . . .
C27 C 0.5343(3) 0.66228(18) 0.46091(18) 0.0432(5) Uani 1 1 d . . . . .
C9 C 0.9617(3) 0.70895(19) 0.79453(17) 0.0520(6) Uani 1 1 d . . . . .
H9 H 1.025157 0.728111 0.852635 0.062 Uiso 1 1 calc R U . . .
C26 C 0.4788(2) 0.58520(19) 0.36935(18) 0.0432(5) Uani 1 1 d . . . . .
C23 C 0.4767(2) 0.43553(19) 0.26524(16) 0.0428(5) Uani 1 1 d . . . . .
C16 C 0.9547(3) 0.21953(18) 0.4592(2) 0.0483(6) Uani 1 1 d . . . . .
C8 C 0.8724(3) 0.76166(19) 0.76852(18) 0.0544(7) Uani 1 1 d . . . . .
H8 H 0.865788 0.821767 0.806340 0.065 Uiso 1 1 calc R U . . .
C18 C 0.7923(3) 0.25118(16) 0.35790(17) 0.0429(5) Uani 1 1 d . . . . .
C31 C 1.1869(3) 0.5556(3) 0.84097(19) 0.0585(7) Uani 1 1 d . . . . .
H31A H 1.226105 0.624704 0.848302 0.070 Uiso 1 1 calc R U . . .
H31B H 1.269358 0.529022 0.849005 0.070 Uiso 1 1 calc R U . . .
C25 C 0.3832(3) 0.5669(2) 0.2852(2) 0.0515(6) Uani 1 1 d . . . . .
C28 C 0.5175(3) 0.7532(2) 0.5116(2) 0.0520(6) Uani 1 1 d . . . . .
C17 C 0.8646(3) 0.18262(18) 0.3685(2) 0.0503(6) Uani 1 1 d . . . . .
C24 C 0.3823(3) 0.4762(2) 0.22257(19) 0.0530(7) Uani 1 1 d . . . . .
C33 C 1.1972(3) 0.3556(2) 0.7097(2) 0.0622(8) Uani 1 1 d . . . . .
H33A H 1.295548 0.400537 0.736182 0.075 Uiso 1 1 calc R U . . .
H33B H 1.200693 0.305394 0.653702 0.075 Uiso 1 1 calc R U . . .
C21 C 0.5050(3) 0.2604(2) 0.17189(18) 0.0588(7) Uani 1 1 d . . . . .
C32 C 1.1065(3) 0.5492(3) 0.9172(2) 0.0752(10) Uani 1 1 d . . . . .
H32A H 1.035103 0.585129 0.916697 0.113 Uiso 1 1 calc R U . . .
H32B H 1.175404 0.577160 0.976624 0.113 Uiso 1 1 calc R U . . .
H32C H 1.057870 0.481153 0.906847 0.113 Uiso 1 1 calc R U . . .
C49 C 0.6258(4) 0.8821(2) 0.6773(2) 0.0656(8) Uani 1 1 d . . . . .
H49A H 0.649776 0.872650 0.736807 0.079 Uiso 1 1 calc R U . . .
H49B H 0.531870 0.896117 0.672169 0.079 Uiso 1 1 calc R U . . .
C20 C 0.5986(4) 0.2078(2) 0.19752(18) 0.0615(7) Uani 1 1 d . . . . .
C35 C 1.0387(4) 0.1618(2) 0.4966(2) 0.0666(8) Uani 1 1 d . . . . .
H35A H 1.136745 0.204024 0.529681 0.080 Uiso 1 1 calc R U . . .
H35B H 1.047624 0.108320 0.445330 0.080 Uiso 1 1 calc R U . . .
C50 C 0.7400(4) 0.9699(2) 0.6770(3) 0.0724(8) Uani 1 1 d . . . . .
H50A H 0.834861 0.959119 0.687040 0.109 Uiso 1 1 calc R U . . .
H50B H 0.739412 1.027693 0.725770 0.109 Uiso 1 1 calc R U . . .
H50C H 0.718823 0.979167 0.617830 0.109 Uiso 1 1 calc R U . . .
C37 C 0.8525(3) 0.0851(2) 0.2996(2) 0.0668(8) Uani 1 1 d . . . . .
H37A H 0.948921 0.074767 0.304943 0.080 Uiso 1 1 calc R U . . .
H37B H 0.821360 0.086665 0.237395 0.080 Uiso 1 1 calc R U . . .
C47 C 0.4266(4) 0.8117(3) 0.4820(3) 0.0749(10) Uani 1 1 d . . . . .
H47A H 0.406817 0.854948 0.536713 0.090 Uiso 1 1 calc R U . . .
H47B H 0.333312 0.767296 0.442571 0.090 Uiso 1 1 calc R U . . .
C43 C 0.2952(3) 0.4376(3) 0.1248(2) 0.0715(9) Uani 1 1 d . . . . .
H43A H 0.249823 0.367099 0.107679 0.086 Uiso 1 1 calc R U . . .
H43B H 0.217227 0.468853 0.120897 0.086 Uiso 1 1 calc R U . . .
C38 C 0.7470(5) -0.0013(2) 0.3108(3) 0.0936(13) Uani 1 1 d . . . . .
H38A H 0.650004 0.006518 0.302603 0.140 Uiso 1 1 calc R U . . .
H38B H 0.776975 -0.003873 0.372032 0.140 Uiso 1 1 calc R U . . .
H38C H 0.746731 -0.061480 0.264832 0.140 Uiso 1 1 calc R U . . .
C36 C 0.9652(5) 0.1192(3) 0.5622(3) 0.0869(11) Uani 1 1 d . . . . .
H36A H 1.030815 0.093114 0.594092 0.130 Uiso 1 1 calc R U . . .
H36B H 0.877168 0.067301 0.527050 0.130 Uiso 1 1 calc R U . . .
H36C H 0.940956 0.170339 0.606876 0.130 Uiso 1 1 calc R U . . .
C45 C 0.2941(3) 0.6293(3) 0.2603(3) 0.0764(10) Uani 1 1 d . . . . .
H45A H 0.281433 0.673097 0.317377 0.092 Uiso 1 1 calc R U . . .
H45B H 0.197485 0.586610 0.224527 0.092 Uiso 1 1 calc R U . . .
C34 C 1.1551(5) 0.3066(3) 0.7777(3) 0.0878(12) Uani 1 1 d . . . . .
H34A H 1.162755 0.355989 0.836267 0.132 Uiso 1 1 calc R U . . .
H34B H 1.219660 0.267553 0.786516 0.132 Uiso 1 1 calc R U . . .
H34C H 1.055852 0.264668 0.754158 0.132 Uiso 1 1 calc R U . . .
C48 C 0.4988(5) 0.8729(3) 0.4299(3) 0.0901(12) Uani 1 1 d . . . . .
H48A H 0.529616 0.831742 0.380175 0.135 Uiso 1 1 calc R U . . .
H48B H 0.582748 0.924344 0.471721 0.135 Uiso 1 1 calc R U . . .
H48C H 0.430408 0.901945 0.404570 0.135 Uiso 1 1 calc R U . . .
C44 C 0.3839(4) 0.4549(4) 0.0571(3) 0.0852(11) Uani 1 1 d . . . . .
H44A H 0.427554 0.524665 0.072809 0.128 Uiso 1 1 calc R U . . .
H44B H 0.321840 0.428633 -0.004585 0.128 Uiso 1 1 calc R U . . .
H44C H 0.459766 0.422702 0.059349 0.128 Uiso 1 1 calc R U . . .
C41 C 0.3941(6) 0.2186(3) 0.0811(2) 0.1098(14) Uani 1 1 d . U . . .
H41A H 0.346034 0.150063 0.071831 0.132 Uiso 1 1 calc R U . . .
H41B H 0.320005 0.253494 0.086362 0.132 Uiso 1 1 calc R U . . .
C39 C 0.5828(6) 0.1031(4) 0.1417(4) 0.0698(18) Uani 0.715(10) 1 d . . P A 1
H39A H 0.482706 0.071163 0.105368 0.084 Uiso 0.715(10) 1 calc R U P A 1
H39B H 0.604745 0.067216 0.183005 0.084 Uiso 0.715(10) 1 calc R U P A 1
C46 C 0.3560(6) 0.6903(3) 0.2058(3) 0.1002(14) Uani 1 1 d . . . . .
H46A H 0.457583 0.724357 0.234751 0.150 Uiso 1 1 calc R U . . .
H46B H 0.302851 0.737655 0.204113 0.150 Uiso 1 1 calc R U . . .
H46C H 0.347400 0.648239 0.143307 0.150 Uiso 1 1 calc R U . . .
C42 C 0.4476(7) 0.2223(4) -0.0033(3) 0.1269(16) Uani 1 1 d . U . . .
H42A H 0.374514 0.232853 -0.045732 0.190 Uiso 1 1 calc R U . . .
H42B H 0.466613 0.160905 -0.032858 0.190 Uiso 1 1 calc R U . . .
H42C H 0.536512 0.275525 0.013913 0.190 Uiso 1 1 calc R U . . .
C40 C 0.6872(6) 0.1018(4) 0.0776(4) 0.0869(19) Uani 0.715(10) 1 d . . P A 1
H40A H 0.664179 0.136693 0.036334 0.130 Uiso 0.715(10) 1 calc R U P A 1
H40B H 0.677860 0.034614 0.041606 0.130 Uiso 0.715(10) 1 calc R U P A 1
H40C H 0.786086 0.133219 0.113904 0.130 Uiso 0.715(10) 1 calc R U P A 1
I2 I -0.05361(15) 0.17472(8) -0.07185(7) 0.1283(4) Uani 0.5 1 d D U P B -1
I1 I -0.03362(7) 0.01345(6) -0.00549(6) 0.0932(3) Uani 0.5 1 d D U P B -1
I3 I -0.00768(14) -0.14087(9) 0.07056(8) 0.1229(4) Uani 0.5 1 d D U P B -1
C52 C 0.5436(12) 0.0264(6) 0.1289(7) 0.061(3) Uani 0.285(10) 1 d . . P A 2
H52A H 0.504720 -0.020884 0.067052 0.091 Uiso 0.285(10) 1 calc R U P A 2
H52B H 0.464191 0.037103 0.157978 0.091 Uiso 0.285(10) 1 calc R U P A 2
H52C H 0.605909 0.001764 0.164950 0.091 Uiso 0.285(10) 1 calc R U P A 2
C51 C 0.634(2) 0.1254(10) 0.1238(7) 0.063(4) Uani 0.285(10) 1 d . . P A 2
H51A H 0.737869 0.131525 0.137343 0.076 Uiso 0.285(10) 1 calc R U P A 2
H51B H 0.605639 0.129060 0.062066 0.076 Uiso 0.285(10) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N2 C2 1.365(3) . ?
N2 C11 1.385(3) . ?
N2 C14 1.398(3) . ?
N1 C1 1.356(3) . ?
N1 C10 1.387(3) . ?
N1 C7 1.386(3) . ?
N6 C6 1.364(3) . ?
N6 C30 1.387(3) . ?
N6 C27 1.396(3) . ?
N4 C4 1.363(3) . ?
N4 C19 1.386(3) . ?
N4 C22 1.400(3) . ?
N5 C5 1.369(3) . ?
N5 C26 1.393(3) . ?
N5 C23 1.393(3) . ?
N3 C3 1.366(3) . ?
N3 C15 1.395(3) . ?
N3 C18 1.392(3) . ?
C1 C2 1.368(3) . ?
C1 C6 1.373(3) . ?
C2 C3 1.359(3) . ?
C3 C4 1.373(3) . ?
C4 C5 1.368(3) . ?
C5 C6 1.361(3) . ?
C10 C11 1.455(4) . ?
C10 C9 1.392(3) . ?
C11 C12 1.395(3) . ?
C14 C15 1.481(3) . ?
C14 C13 1.411(3) . ?
C30 C7 1.461(4) . ?
C30 C29 1.386(4) . ?
C7 C8 1.392(4) . ?
C12 C13 1.419(4) . ?
C12 C31 1.503(4) . ?
C15 C16 1.403(3) . ?
C13 C33 1.501(4) . ?
C29 C28 1.424(4) . ?
C29 C49 1.505(4) . ?
C19 C18 1.475(4) . ?
C19 C20 1.411(3) . ?
C22 C23 1.475(4) . ?
C22 C21 1.393(4) . ?
C27 C26 1.474(4) . ?
C27 C28 1.414(4) . ?
C9 H9 0.9400 . ?
C9 C8 1.390(4) . ?
C26 C25 1.403(4) . ?
C23 C24 1.402(4) . ?
C16 C17 1.423(4) . ?
C16 C35 1.492(4) . ?
C8 H8 0.9400 . ?
C18 C17 1.401(4) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 C32 1.528(4) . ?
C25 C24 1.414(5) . ?
C25 C45 1.501(4) . ?
C28 C47 1.493(4) . ?
C17 C37 1.500(4) . ?
C24 C43 1.500(4) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 C34 1.505(5) . ?
C21 C20 1.418(5) . ?
C21 C41 1.508(4) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 H32C 0.9700 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 C50 1.512(5) . ?
C20 C39 1.508(6) . ?
C20 C51 1.558(13) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 C36 1.529(5) . ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
C50 H50C 0.9700 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 C38 1.523(5) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 C48 1.514(5) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 C44 1.498(5) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 H38C 0.9700 . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C36 H36C 0.9700 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 C46 1.504(5) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 H34C 0.9700 . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C48 H48C 0.9700 . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C44 H44C 0.9700 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 C42 1.493(7) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 C40 1.523(9) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C46 H46C 0.9700 . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C42 H42C 0.9700 . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C40 H40C 0.9700 . ?
I2 I1 2.9178(15) . ?
I1 I3 2.9238(15) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C52 H52C 0.9700 . ?
C52 C51 1.566(17) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?

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
C2 N2 C11 122.76(19) . . ?
C2 N2 C14 123.73(19) . . ?
C11 N2 C14 113.48(18) . . ?
C1 N1 C10 123.00(19) . . ?
C1 N1 C7 123.56(19) . . ?
C7 N1 C10 113.44(19) . . ?
C6 N6 C30 122.88(19) . . ?
C6 N6 C27 123.5(2) . . ?
C30 N6 C27 113.66(19) . . ?
C4 N4 C19 122.72(19) . . ?
C4 N4 C22 122.84(19) . . ?
C19 N4 C22 114.36(19) . . ?
C5 N5 C26 123.1(2) . . ?
C5 N5 C23 122.7(2) . . ?
C26 N5 C23 114.11(19) . . ?
C3 N3 C15 123.0(2) . . ?
C3 N3 C18 122.87(19) . . ?
C18 N3 C15 113.97(19) . . ?
N1 C1 C2 120.23(19) . . ?
N1 C1 C6 120.0(2) . . ?
C2 C1 C6 119.7(2) . . ?
N2 C2 C1 119.5(2) . . ?
C3 C2 N2 120.30(19) . . ?
C3 C2 C1 120.18(19) . . ?
N3 C3 C4 119.97(19) . . ?
C2 C3 N3 119.88(19) . . ?
C2 C3 C4 120.13(19) . . ?
N4 C4 C3 120.17(19) . . ?
N4 C4 C5 120.13(19) . . ?
C5 C4 C3 119.69(19) . . ?
C4 C5 N5 120.3(2) . . ?
C6 C5 N5 119.5(2) . . ?
C6 C5 C4 120.17(19) . . ?
N1 C10 C11 116.9(2) . . ?
N1 C10 C9 103.7(2) . . ?
C9 C10 C11 139.4(2) . . ?
N2 C11 C10 117.53(19) . . ?
N2 C11 C12 104.9(2) . . ?
C12 C11 C10 137.6(2) . . ?
N6 C6 C1 119.4(2) . . ?
C5 C6 N6 120.49(19) . . ?
C5 C6 C1 120.1(2) . . ?
N2 C14 C15 115.56(18) . . ?
N2 C14 C13 103.9(2) . . ?
C13 C14 C15 140.6(2) . . ?
N6 C30 C7 117.65(19) . . ?
C29 C30 N6 105.1(2) . . ?
C29 C30 C7 137.2(2) . . ?
N1 C7 C30 116.4(2) . . ?
N1 C7 C8 103.9(2) . . ?
C8 C7 C30 139.7(2) . . ?
C11 C12 C13 108.9(2) . . ?
C11 C12 C31 124.0(3) . . ?
C13 C12 C31 127.0(2) . . ?
N3 C15 C14 117.48(19) . . ?
N3 C15 C16 103.6(2) . . ?
C16 C15 C14 138.9(2) . . ?
C14 C13 C12 108.8(2) . . ?
C14 C13 C33 129.3(3) . . ?
C12 C13 C33 121.8(2) . . ?
C30 C29 C28 108.8(2) . . ?
C30 C29 C49 124.9(3) . . ?
C28 C29 C49 126.3(2) . . ?
N4 C19 C18 117.4(2) . . ?
N4 C19 C20 103.5(2) . . ?
C20 C19 C18 139.0(2) . . ?
N4 C22 C23 116.8(2) . . ?
C21 C22 N4 103.7(2) . . ?
C21 C22 C23 139.5(2) . . ?
N6 C27 C26 115.9(2) . . ?
N6 C27 C28 103.5(2) . . ?
C28 C27 C26 140.6(2) . . ?
C10 C9 H9 125.2 . . ?
C8 C9 C10 109.6(2) . . ?
C8 C9 H9 125.2 . . ?
N5 C26 C27 117.47(19) . . ?
N5 C26 C25 104.0(2) . . ?
C25 C26 C27 138.5(2) . . ?
N5 C23 C22 117.06(19) . . ?
N5 C23 C24 103.4(2) . . ?
C24 C23 C22 139.5(2) . . ?
C15 C16 C17 109.5(2) . . ?
C15 C16 C35 127.5(3) . . ?
C17 C16 C35 122.8(2) . . ?
C7 C8 H8 125.3 . . ?
C9 C8 C7 109.4(2) . . ?
C9 C8 H8 125.3 . . ?
N3 C18 C19 116.8(2) . . ?
N3 C18 C17 104.4(2) . . ?
C17 C18 C19 138.8(2) . . ?
C12 C31 H31A 108.6 . . ?
C12 C31 H31B 108.6 . . ?
C12 C31 C32 114.8(2) . . ?
H31A C31 H31B 107.5 . . ?
C32 C31 H31A 108.6 . . ?
C32 C31 H31B 108.6 . . ?
C26 C25 C24 108.6(2) . . ?
C26 C25 C45 128.4(3) . . ?
C24 C25 C45 122.9(3) . . ?
C29 C28 C47 121.3(3) . . ?
C27 C28 C29 108.9(2) . . ?
C27 C28 C47 129.7(3) . . ?
C16 C17 C37 123.4(2) . . ?
C18 C17 C16 108.5(2) . . ?
C18 C17 C37 128.1(3) . . ?
C23 C24 C25 109.8(2) . . ?
C23 C24 C43 128.4(3) . . ?
C25 C24 C43 121.7(2) . . ?
C13 C33 H33A 108.4 . . ?
C13 C33 H33B 108.4 . . ?
C13 C33 C34 115.5(3) . . ?
H33A C33 H33B 107.5 . . ?
C34 C33 H33A 108.4 . . ?
C34 C33 H33B 108.4 . . ?
C22 C21 C20 109.5(2) . . ?
C22 C21 C41 128.9(3) . . ?
C20 C21 C41 121.5(3) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C29 C49 H49A 108.6 . . ?
C29 C49 H49B 108.6 . . ?
C29 C49 C50 114.7(3) . . ?
H49A C49 H49B 107.6 . . ?
C50 C49 H49A 108.6 . . ?
C50 C49 H49B 108.6 . . ?
C19 C20 C21 109.0(2) . . ?
C19 C20 C39 127.5(3) . . ?
C19 C20 C51 126.3(6) . . ?
C21 C20 C39 122.5(3) . . ?
C21 C20 C51 121.4(4) . . ?
C16 C35 H35A 109.3 . . ?
C16 C35 H35B 109.3 . . ?
C16 C35 C36 111.6(3) . . ?
H35A C35 H35B 108.0 . . ?
C36 C35 H35A 109.3 . . ?
C36 C35 H35B 109.3 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C17 C37 H37A 108.7 . . ?
C17 C37 H37B 108.7 . . ?
C17 C37 C38 114.4(3) . . ?
H37A C37 H37B 107.6 . . ?
C38 C37 H37A 108.7 . . ?
C38 C37 H37B 108.7 . . ?
C28 C47 H47A 109.1 . . ?
C28 C47 H47B 109.1 . . ?
C28 C47 C48 112.6(3) . . ?
H47A C47 H47B 107.8 . . ?
C48 C47 H47A 109.1 . . ?
C48 C47 H47B 109.1 . . ?
C24 C43 H43A 108.9 . . ?
C24 C43 H43B 108.9 . . ?
H43A C43 H43B 107.7 . . ?
C44 C43 C24 113.3(3) . . ?
C44 C43 H43A 108.9 . . ?
C44 C43 H43B 108.9 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C25 C45 H45A 108.4 . . ?
C25 C45 H45B 108.4 . . ?
C25 C45 C46 115.5(3) . . ?
H45A C45 H45B 107.5 . . ?
C46 C45 H45A 108.4 . . ?
C46 C45 H45B 108.4 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C21 C41 H41A 108.0 . . ?
C21 C41 H41B 108.0 . . ?
H41A C41 H41B 107.2 . . ?
C42 C41 C21 117.3(5) . . ?
C42 C41 H41A 108.0 . . ?
C42 C41 H41B 108.0 . . ?
C20 C39 H39A 109.9 . . ?
C20 C39 H39B 109.9 . . ?
C20 C39 C40 109.1(5) . . ?
H39A C39 H39B 108.3 . . ?
C40 C39 H39A 109.9 . . ?
C40 C39 H39B 109.9 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
I2 I1 I3 177.07(5) . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
C20 C51 C52 106.0(10) . . ?
C20 C51 H51A 110.5 . . ?
C20 C51 H51B 110.5 . . ?
C52 C51 H51A 110.5 . . ?
C52 C51 H51B 110.5 . . ?
H51A C51 H51B 108.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C2 C3 N3 -0.2(3) . . . . ?
N2 C2 C3 C4 178.04(19) . . . . ?
N2 C11 C12 C13 0.4(2) . . . . ?
N2 C11 C12 C31 178.5(2) . . . . ?
N2 C14 C15 N3 3.1(3) . . . . ?
N2 C14 C15 C16 -175.2(3) . . . . ?
N2 C14 C13 C12 0.5(2) . . . . ?
N2 C14 C13 C33 -178.9(2) . . . . ?
N1 C1 C2 N2 1.8(3) . . . . ?
N1 C1 C2 C3 -178.74(19) . . . . ?
N1 C1 C6 N6 1.2(3) . . . . ?
N1 C1 C6 C5 -179.8(2) . . . . ?
N1 C10 C11 N2 -0.7(3) . . . . ?
N1 C10 C11 C12 179.0(2) . . . . ?
N1 C10 C9 C8 0.4(3) . . . . ?
N1 C7 C8 C9 0.0(3) . . . . ?
N6 C30 C7 N1 0.4(3) . . . . ?
N6 C30 C7 C8 -179.1(3) . . . . ?
N6 C30 C29 C28 -0.1(3) . . . . ?
N6 C30 C29 C49 179.8(2) . . . . ?
N6 C27 C26 N5 1.1(3) . . . . ?
N6 C27 C26 C25 -177.4(3) . . . . ?
N6 C27 C28 C29 -0.1(3) . . . . ?
N6 C27 C28 C47 177.3(3) . . . . ?
N4 C4 C5 N5 -0.9(3) . . . . ?
N4 C4 C5 C6 -179.70(19) . . . . ?
N4 C19 C18 N3 -2.2(3) . . . . ?
N4 C19 C18 C17 176.6(3) . . . . ?
N4 C19 C20 C21 -0.3(3) . . . . ?
N4 C19 C20 C39 -169.1(4) . . . . ?
N4 C19 C20 C51 159.1(7) . . . . ?
N4 C22 C23 N5 -4.4(3) . . . . ?
N4 C22 C23 C24 174.9(3) . . . . ?
N4 C22 C21 C20 -0.6(3) . . . . ?
N4 C22 C21 C41 176.3(4) . . . . ?
N5 C5 C6 N6 -1.3(3) . . . . ?
N5 C5 C6 C1 179.8(2) . . . . ?
N5 C26 C25 C24 -0.1(3) . . . . ?
N5 C26 C25 C45 -179.7(3) . . . . ?
N5 C23 C24 C25 0.2(3) . . . . ?
N5 C23 C24 C43 177.4(3) . . . . ?
N3 C3 C4 N4 -0.6(3) . . . . ?
N3 C3 C4 C5 177.99(19) . . . . ?
N3 C15 C16 C17 0.3(3) . . . . ?
N3 C15 C16 C35 -175.4(2) . . . . ?
N3 C18 C17 C16 1.0(3) . . . . ?
N3 C18 C17 C37 -179.9(3) . . . . ?
C1 N1 C10 C11 0.5(3) . . . . ?
C1 N1 C10 C9 -179.4(2) . . . . ?
C1 N1 C7 C30 -0.4(3) . . . . ?
C1 N1 C7 C8 179.3(2) . . . . ?
C1 C2 C3 N3 -179.66(19) . . . . ?
C1 C2 C3 C4 -1.5(3) . . . . ?
C2 N2 C11 C10 1.5(3) . . . . ?
C2 N2 C11 C12 -178.3(2) . . . . ?
C2 N2 C14 C15 -1.9(3) . . . . ?
C2 N2 C14 C13 177.9(2) . . . . ?
C2 C1 C6 N6 -179.2(2) . . . . ?
C2 C1 C6 C5 -0.2(3) . . . . ?
C2 C3 C4 N4 -178.84(19) . . . . ?
C2 C3 C4 C5 -0.2(3) . . . . ?
C3 N3 C15 C14 -3.1(3) . . . . ?
C3 N3 C15 C16 175.7(2) . . . . ?
C3 N3 C18 C19 3.0(3) . . . . ?
C3 N3 C18 C17 -176.2(2) . . . . ?
C3 C4 C5 N5 -179.58(19) . . . . ?
C3 C4 C5 C6 1.7(3) . . . . ?
C4 N4 C19 C18 0.1(3) . . . . ?
C4 N4 C19 C20 176.7(2) . . . . ?
C4 N4 C22 C23 3.5(3) . . . . ?
C4 N4 C22 C21 -176.3(2) . . . . ?
C4 C5 C6 N6 177.5(2) . . . . ?
C4 C5 C6 C1 -1.5(3) . . . . ?
C5 N5 C26 C27 -2.4(3) . . . . ?
C5 N5 C26 C25 176.5(2) . . . . ?
C5 N5 C23 C22 3.0(3) . . . . ?
C5 N5 C23 C24 -176.6(2) . . . . ?
C10 N1 C1 C2 -1.1(3) . . . . ?
C10 N1 C1 C6 178.5(2) . . . . ?
C10 N1 C7 C30 -179.43(19) . . . . ?
C10 N1 C7 C8 0.2(3) . . . . ?
C10 C11 C12 C13 -179.4(3) . . . . ?
C10 C11 C12 C31 -1.3(4) . . . . ?
C10 C9 C8 C7 -0.3(3) . . . . ?
C11 N2 C2 C1 -2.1(3) . . . . ?
C11 N2 C2 C3 178.44(19) . . . . ?
C11 N2 C14 C15 179.92(18) . . . . ?
C11 N2 C14 C13 -0.3(2) . . . . ?
C11 C10 C9 C8 -179.6(3) . . . . ?
C11 C12 C13 C14 -0.6(3) . . . . ?
C11 C12 C13 C33 178.9(2) . . . . ?
C11 C12 C31 C32 77.7(4) . . . . ?
C6 N6 C30 C7 0.4(3) . . . . ?
C6 N6 C30 C29 -179.8(2) . . . . ?
C6 N6 C27 C26 0.1(3) . . . . ?
C6 N6 C27 C28 179.9(2) . . . . ?
C6 C1 C2 N2 -177.8(2) . . . . ?
C6 C1 C2 C3 1.7(3) . . . . ?
C14 N2 C2 C1 179.89(19) . . . . ?
C14 N2 C2 C3 0.4(3) . . . . ?
C14 N2 C11 C10 179.77(18) . . . . ?
C14 N2 C11 C12 0.0(2) . . . . ?
C14 C15 C16 C17 178.7(3) . . . . ?
C14 C15 C16 C35 3.0(5) . . . . ?
C14 C13 C33 C34 -108.1(4) . . . . ?
C30 N6 C6 C1 -1.2(3) . . . . ?
C30 N6 C6 C5 179.8(2) . . . . ?
C30 N6 C27 C26 -179.74(19) . . . . ?
C30 N6 C27 C28 0.0(3) . . . . ?
C30 C7 C8 C9 179.6(3) . . . . ?
C30 C29 C28 C27 0.1(3) . . . . ?
C30 C29 C28 C47 -177.5(2) . . . . ?
C30 C29 C49 C50 90.9(4) . . . . ?
C7 N1 C1 C2 180.0(2) . . . . ?
C7 N1 C1 C6 -0.4(3) . . . . ?
C7 N1 C10 C11 179.59(19) . . . . ?
C7 N1 C10 C9 -0.4(3) . . . . ?
C7 C30 C29 C28 179.6(3) . . . . ?
C7 C30 C29 C49 -0.5(5) . . . . ?
C12 C13 C33 C34 72.6(4) . . . . ?
C15 N3 C3 C2 1.7(3) . . . . ?
C15 N3 C3 C4 -176.55(19) . . . . ?
C15 N3 C18 C19 178.33(19) . . . . ?
C15 N3 C18 C17 -0.8(3) . . . . ?
C15 C14 C13 C12 -179.8(3) . . . . ?
C15 C14 C13 C33 0.8(5) . . . . ?
C15 C16 C17 C18 -0.8(3) . . . . ?
C15 C16 C17 C37 180.0(2) . . . . ?
C15 C16 C35 C36 72.8(4) . . . . ?
C13 C14 C15 N3 -176.6(3) . . . . ?
C13 C14 C15 C16 5.2(5) . . . . ?
C13 C12 C31 C32 -104.5(3) . . . . ?
C29 C30 C7 N1 -179.3(3) . . . . ?
C29 C30 C7 C8 1.2(5) . . . . ?
C29 C28 C47 C48 95.1(4) . . . . ?
C19 N4 C4 C3 1.3(3) . . . . ?
C19 N4 C4 C5 -177.3(2) . . . . ?
C19 N4 C22 C23 -179.78(19) . . . . ?
C19 N4 C22 C21 0.4(3) . . . . ?
C19 C18 C17 C16 -177.9(3) . . . . ?
C19 C18 C17 C37 1.2(5) . . . . ?
C19 C20 C39 C40 -96.1(5) . . . . ?
C19 C20 C51 C52 98.2(10) . . . . ?
C22 N4 C4 C3 177.8(2) . . . . ?
C22 N4 C4 C5 -0.8(3) . . . . ?
C22 N4 C19 C18 -176.64(19) . . . . ?
C22 N4 C19 C20 0.0(3) . . . . ?
C22 C23 C24 C25 -179.1(3) . . . . ?
C22 C23 C24 C43 -2.0(5) . . . . ?
C22 C21 C20 C19 0.6(3) . . . . ?
C22 C21 C20 C39 170.1(4) . . . . ?
C22 C21 C20 C51 -160.1(8) . . . . ?
C22 C21 C41 C42 105.4(5) . . . . ?
C27 N6 C6 C1 178.9(2) . . . . ?
C27 N6 C6 C5 0.0(3) . . . . ?
C27 N6 C30 C7 -179.75(19) . . . . ?
C27 N6 C30 C29 0.0(3) . . . . ?
C27 C26 C25 C24 178.5(3) . . . . ?
C27 C26 C25 C45 -1.1(5) . . . . ?
C27 C28 C47 C48 -81.9(4) . . . . ?
C9 C10 C11 N2 179.2(3) . . . . ?
C9 C10 C11 C12 -1.0(5) . . . . ?
C26 N5 C5 C4 -176.2(2) . . . . ?
C26 N5 C5 C6 2.6(3) . . . . ?
C26 N5 C23 C22 179.22(19) . . . . ?
C26 N5 C23 C24 -0.3(3) . . . . ?
C26 C27 C28 C29 179.6(3) . . . . ?
C26 C27 C28 C47 -3.0(5) . . . . ?
C26 C25 C24 C23 -0.1(3) . . . . ?
C26 C25 C24 C43 -177.4(2) . . . . ?
C26 C25 C45 C46 99.8(4) . . . . ?
C23 N5 C5 C4 -0.3(3) . . . . ?
C23 N5 C5 C6 178.5(2) . . . . ?
C23 N5 C26 C27 -178.69(19) . . . . ?
C23 N5 C26 C25 0.3(3) . . . . ?
C23 C22 C21 C20 179.6(3) . . . . ?
C23 C22 C21 C41 -3.4(6) . . . . ?
C23 C24 C43 C44 -77.2(4) . . . . ?
C16 C17 C37 C38 82.5(4) . . . . ?
C18 N3 C3 C2 176.6(2) . . . . ?
C18 N3 C3 C4 -1.6(3) . . . . ?
C18 N3 C15 C14 -178.49(19) . . . . ?
C18 N3 C15 C16 0.3(3) . . . . ?
C18 C19 C20 C21 175.1(3) . . . . ?
C18 C19 C20 C39 6.3(6) . . . . ?
C18 C19 C20 C51 -25.5(8) . . . . ?
C18 C17 C37 C38 -96.5(4) . . . . ?
C31 C12 C13 C14 -178.6(2) . . . . ?
C31 C12 C13 C33 0.8(4) . . . . ?
C25 C24 C43 C44 99.6(4) . . . . ?
C28 C29 C49 C50 -89.2(4) . . . . ?
C28 C27 C26 N5 -178.6(3) . . . . ?
C28 C27 C26 C25 3.0(5) . . . . ?
C17 C16 C35 C36 -102.4(3) . . . . ?
C24 C25 C45 C46 -79.8(4) . . . . ?
C21 C22 C23 N5 175.3(3) . . . . ?
C21 C22 C23 C24 -5.4(5) . . . . ?
C21 C20 C39 C40 96.5(5) . . . . ?
C21 C20 C51 C52 -104.6(6) . . . . ?
C49 C29 C28 C27 -179.8(2) . . . . ?
C49 C29 C28 C47 2.6(4) . . . . ?
C20 C19 C18 N3 -177.1(3) . . . . ?
C20 C19 C18 C17 1.6(6) . . . . ?
C20 C21 C41 C42 -78.0(5) . . . . ?
C35 C16 C17 C18 175.1(2) . . . . ?
C35 C16 C17 C37 -4.1(4) . . . . ?
C45 C25 C24 C23 179.6(2) . . . . ?
C45 C25 C24 C43 2.2(4) . . . . ?
C41 C21 C20 C19 -176.6(3) . . . . ?
C41 C21 C20 C39 -7.1(6) . . . . ?
C41 C21 C20 C51 22.8(9) . . . . ?

_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 1.313
_oxdiff_exptl_absorpt_empirical_full_min 0.678
_exptl_crystal_recrystallization_method 
'Slow reaction in chlorobenzene solution'
_exptl_crystal_preparation       'Magnetic properties,Conducting properties'
####################################################################### 
# 
# 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_ethac2i3_autored_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2394978'
loop_
_audit_author_name
_audit_author_address
'Toshio Naito'
;Ehime University
Japan
;
_audit_update_record             
;
2024-10-31 deposited with the CCDC.	2025-05-30 downloaded from the CCDC.
;
_audit_creation_date             2024-10-23
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        (EtHAC)2I3
_chemical_formula_moiety         'I3, 2(C50 H52 N6)'
_chemical_formula_sum            'C100 H104 I3 N12'
_chemical_formula_weight         1854.65
_chemical_melting_point          ?
_chemical_oxdiff_formula         C100H104N12I3
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'
I I -0.4742 1.8119 '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      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                   9.6767(3)
_cell_length_b                   14.8228(4)
_cell_length_c                   15.6099(5)
_cell_angle_alpha                106.658(2)
_cell_angle_beta                 98.703(2)
_cell_angle_gamma                103.675(2)
_cell_volume                     2025.70(11)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    20570
_cell_measurement_temperature    200
_cell_measurement_theta_max      31.3020
_cell_measurement_theta_min      2.2800
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.216
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             947
_exptl_crystal_preparation       'Magnetic properties,Conducting properties'
_exptl_crystal_size_max          0.389
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.038
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            38840
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.217
_diffrn_reflns_theta_min         2.229
_diffrn_ambient_temperature      200
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 7.111
_diffrn_detector_type            'Rigaku Saturn724+ area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.917
_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  70.00   0.50    6.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50    6.00    --  -20.00  45.00  90.00  360
  3  ω   -110.00  70.00   0.50    6.00    --  -20.00  45.00 180.00  360
  4  ω   -110.00  70.00   0.50    6.00    --  -20.00  45.00 270.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Rigaku Varimax with Saturn'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0280172000
_diffrn_orient_matrix_UB_12      0.0491478000
_diffrn_orient_matrix_UB_13      0.0309898000
_diffrn_orient_matrix_UB_21      0.0692453000
_diffrn_orient_matrix_UB_22      -0.0074979000
_diffrn_orient_matrix_UB_23      0.0112917000
_diffrn_orient_matrix_UB_31      0.0210917000
_diffrn_orient_matrix_UB_32      0.0161779000
_diffrn_orient_matrix_UB_33      -0.0359672000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'MicroMax 007'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8252
_reflns_number_total             12067
_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 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b46 (Rigaku, 2016)'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.963
_refine_diff_density_min         -1.215
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         12067
_refine_ls_number_restraints     50
_refine_ls_R_factor_all          0.0851
_refine_ls_R_factor_gt           0.0583
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0830P)²+1.2985P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1564
_refine_ls_wR_factor_ref         0.1753
_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
 I1-I2 = I1-I3
 2.8 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
I1 \\sim I2 \\sim I3: within 3A with sigma of 0.02 and sigma for terminal atoms
of 0.02 within 3A
Uanis(I1) \\sim Ueq, Uanis(I2) \\sim Ueq, Uanis(I3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 I1, I2, I3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(C51)=Sof(H51A)=Sof(H51B)=1-FVAR(1)
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(1)
 Fixed Sof: I1(0.5) I2(0.5) I3(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C37(H37A,H37B), C35(H35A,H35B), C33(H33A,H33B), C43(H43A,
 H43B), C45(H45A,H45B), C49(H49A,H49B), C47(H47A,H47B), C41(H41A,H41B),
 C39(H39A,H39B), C51(H51A,H51B)
6.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C8(H8)
6.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C38(H38A,H38B,H38C), C36(H36A,H36B,H36C), C50(H50A,H50B,
 H50C), C44(H44A,H44B,H44C), C34(H34A,H34B,H34C), C48(H48A,H48B,H48C), C46(H46A,
 H46B,H46C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C52(H52A,H52B,H52C)
;
_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
I1 I 0.02721(10) 0.98819(8) 0.00620(7) 0.0792(3) Uani 0.5 1 d D U P A -1
I2 I 0.05050(16) 0.82396(8) 0.06908(8) 0.1020(4) Uani 0.5 1 d D U P A -1
N1 N 0.15706(18) 0.37222(12) 0.34682(11) 0.0279(3) Uani 1 1 d . . . . .
N6 N 0.36062(19) 0.35093(12) 0.47465(12) 0.0300(3) Uani 1 1 d . . . . .
N4 N 0.36349(18) 0.65185(12) 0.68825(11) 0.0288(3) Uani 1 1 d . . . . .
N2 N 0.05951(17) 0.53399(12) 0.38772(11) 0.0270(3) Uani 1 1 d . . . . .
N5 N 0.46871(18) 0.49221(13) 0.64449(11) 0.0300(3) Uani 1 1 d . . . . .
N3 N 0.15933(18) 0.67242(12) 0.55906(11) 0.0282(3) Uani 1 1 d . . . . .
C1 C 0.2088(2) 0.44202(13) 0.43187(12) 0.0262(4) Uani 1 1 d . . . . .
C6 C 0.3120(2) 0.43205(13) 0.49596(13) 0.0265(4) Uani 1 1 d . . . . .
C2 C 0.1589(2) 0.52278(13) 0.45280(12) 0.0255(4) Uani 1 1 d . . . . .
C4 C 0.3121(2) 0.58192(13) 0.60322(12) 0.0264(4) Uani 1 1 d . . . . .
C19 C 0.3201(2) 0.73650(15) 0.71320(14) 0.0328(4) Uani 1 1 d . . . . .
C5 C 0.3648(2) 0.50232(14) 0.58099(12) 0.0264(4) Uani 1 1 d . . . . .
C17 C 0.1384(2) 0.81760(15) 0.63392(16) 0.0359(4) Uani 1 1 d . . . . .
C22 C 0.4728(2) 0.64790(16) 0.75574(13) 0.0330(4) Uani 1 1 d . . . . .
C3 C 0.2088(2) 0.59201(13) 0.53865(12) 0.0255(4) Uani 1 1 d . . . . .
C7 C 0.2029(2) 0.28880(14) 0.32050(14) 0.0317(4) Uani 1 1 d . . . . .
C10 C 0.0551(2) 0.37868(15) 0.27816(13) 0.0301(4) Uani 1 1 d . . . . .
C16 C 0.0468(2) 0.78180(15) 0.54333(16) 0.0346(4) Uani 1 1 d . . . . .
C26 C 0.5206(2) 0.40990(16) 0.62782(15) 0.0327(4) Uani 1 1 d . . . . .
C15 C 0.0590(2) 0.68959(14) 0.49543(14) 0.0282(4) Uani 1 1 d . . . . .
C30 C 0.3114(2) 0.27740(15) 0.38894(15) 0.0323(4) Uani 1 1 d . . . . .
C23 C 0.5247(2) 0.55970(16) 0.73331(14) 0.0323(4) Uani 1 1 d . . . . .
C18 C 0.2109(2) 0.74850(14) 0.64371(14) 0.0312(4) Uani 1 1 d . . . . .
C14 C 0.0023(2) 0.61371(14) 0.40280(14) 0.0282(4) Uani 1 1 d . . . . .
C11 C 0.0025(2) 0.46457(15) 0.30020(13) 0.0294(4) Uani 1 1 d . . . . .
C25 C 0.6165(2) 0.42672(19) 0.71164(17) 0.0388(5) Uani 1 1 d . . . . .
C24 C 0.6192(2) 0.51764(19) 0.77536(16) 0.0383(5) Uani 1 1 d . . . . .
C27 C 0.4636(2) 0.33383(16) 0.53604(15) 0.0327(4) Uani 1 1 d . . . . .
C12 C -0.0968(2) 0.50084(17) 0.25642(14) 0.0321(4) Uani 1 1 d . . . . .
C13 C -0.0983(2) 0.59226(17) 0.31870(15) 0.0327(4) Uani 1 1 d . . . . .
C29 C 0.3857(3) 0.20880(17) 0.39460(17) 0.0389(5) Uani 1 1 d . . . . .
C9 C 0.0346(3) 0.29352(16) 0.20364(14) 0.0387(5) Uani 1 1 d . . . . .
H9 H -0.029475 0.275492 0.145032 0.046 Uiso 1 1 calc R U . . .
C31 C -0.1894(2) 0.4493(2) 0.15996(15) 0.0412(5) Uani 1 1 d . . . . .
H31A H -0.271187 0.477864 0.152078 0.049 Uiso 1 1 calc R U . . .
H31B H -0.232327 0.378860 0.151772 0.049 Uiso 1 1 calc R U . . .
C37 C 0.1505(3) 0.91500(17) 0.7040(2) 0.0482(6) Uani 1 1 d . . . . .
H37A H 0.183089 0.912405 0.766280 0.058 Uiso 1 1 calc R U . . .
H37B H 0.052287 0.924763 0.699080 0.058 Uiso 1 1 calc R U . . .
C8 C 0.1237(3) 0.23900(16) 0.22926(15) 0.0401(5) Uani 1 1 d . . . . .
H8 H 0.129342 0.178011 0.190847 0.048 Uiso 1 1 calc R U . . .
C21 C 0.5008(3) 0.73613(18) 0.82796(15) 0.0448(6) Uani 1 1 d . . . . .
C28 C 0.4793(3) 0.24270(17) 0.48447(18) 0.0390(5) Uani 1 1 d . . . . .
C35 C -0.0389(3) 0.84016(18) 0.50679(19) 0.0457(6) Uani 1 1 d . . . . .
H35A H -0.045953 0.894611 0.558668 0.055 Uiso 1 1 calc R U . . .
H35B H -0.139321 0.797222 0.474361 0.055 Uiso 1 1 calc R U . . .
C33 C -0.1965(3) 0.6500(2) 0.29284(18) 0.0437(5) Uani 1 1 d . . . . .
H33A H -0.196865 0.701719 0.349310 0.052 Uiso 1 1 calc R U . . .
H33B H -0.297615 0.605148 0.267208 0.052 Uiso 1 1 calc R U . . .
C20 C 0.4075(3) 0.79009(18) 0.80233(16) 0.0471(6) Uani 1 1 d . . . . .
C32 C -0.1071(3) 0.4559(3) 0.08453(17) 0.0568(7) Uani 1 1 d . . . . .
H32A H -0.176949 0.429057 0.024519 0.085 Uiso 1 1 calc R U . . .
H32B H -0.036808 0.417977 0.084878 0.085 Uiso 1 1 calc R U . . .
H32C H -0.054760 0.525042 0.095914 0.085 Uiso 1 1 calc R U . . .
C43 C 0.7072(3) 0.5554(2) 0.87291(18) 0.0506(6) Uani 1 1 d . . . . .
H43A H 0.758291 0.626496 0.889775 0.061 Uiso 1 1 calc R U . . .
H43B H 0.782593 0.520858 0.877400 0.061 Uiso 1 1 calc R U . . .
C38 C 0.2561(4) 1.0034(2) 0.6936(3) 0.0698(9) Uani 1 1 d . . . . .
H38A H 0.221041 1.009595 0.633839 0.105 Uiso 1 1 calc R U . . .
H38B H 0.353457 0.994075 0.697266 0.105 Uiso 1 1 calc R U . . .
H38C H 0.261566 1.063487 0.742916 0.105 Uiso 1 1 calc R U . . .
C36 C 0.0334(4) 0.8827(2) 0.4405(2) 0.0598(7) Uani 1 1 d . . . . .
H36A H 0.052237 0.829956 0.393606 0.090 Uiso 1 1 calc R U . . .
H36B H 0.126096 0.933404 0.474761 0.090 Uiso 1 1 calc R U . . .
H36C H -0.031766 0.912079 0.410725 0.090 Uiso 1 1 calc R U . . .
C45 C 0.7044(3) 0.3623(2) 0.7353(2) 0.0550(7) Uani 1 1 d . . . . .
H45A H 0.709883 0.315180 0.677331 0.066 Uiso 1 1 calc R U . . .
H45B H 0.805340 0.404366 0.767628 0.066 Uiso 1 1 calc R U . . .
C49 C 0.3681(3) 0.11496(19) 0.3185(2) 0.0499(6) Uani 1 1 d . . . . .
H49A H 0.464044 0.101757 0.321776 0.060 Uiso 1 1 calc R U . . .
H49B H 0.339685 0.124575 0.258898 0.060 Uiso 1 1 calc R U . . .
C47 C 0.5697(3) 0.1828(2) 0.5143(2) 0.0547(7) Uani 1 1 d . . . . .
H47A H 0.666691 0.227274 0.552154 0.066 Uiso 1 1 calc R U . . .
H47B H 0.585351 0.136600 0.459345 0.066 Uiso 1 1 calc R U . . .
C50 C 0.2562(3) 0.0253(2) 0.3205(2) 0.0542(6) Uani 1 1 d . . . . .
H50A H 0.255488 -0.033021 0.270853 0.081 Uiso 1 1 calc R U . . .
H50B H 0.159054 0.035134 0.312131 0.081 Uiso 1 1 calc R U . . .
H50C H 0.281657 0.015863 0.379872 0.081 Uiso 1 1 calc R U . . .
C44 C 0.6152(3) 0.5410(3) 0.9404(2) 0.0626(8) Uani 1 1 d . . . . .
H44A H 0.566687 0.470557 0.925320 0.094 Uiso 1 1 calc R U . . .
H44B H 0.541213 0.575829 0.937029 0.094 Uiso 1 1 calc R U . . .
H44C H 0.677867 0.567355 1.002836 0.094 Uiso 1 1 calc R U . . .
C34 C -0.1532(4) 0.6985(3) 0.2233(2) 0.0631(8) Uani 1 1 d . . . . .
H34A H -0.161275 0.647559 0.165029 0.095 Uiso 1 1 calc R U . . .
H34B H -0.051947 0.741299 0.246907 0.095 Uiso 1 1 calc R U . . .
H34C H -0.218308 0.737903 0.213201 0.095 Uiso 1 1 calc R U . . .
C48 C 0.4969(4) 0.1246(2) 0.5697(2) 0.0649(8) Uani 1 1 d . . . . .
H48A H 0.407914 0.073673 0.529794 0.097 Uiso 1 1 calc R U . . .
H48B H 0.471272 0.169227 0.620407 0.097 Uiso 1 1 calc R U . . .
H48C H 0.564411 0.093543 0.594735 0.097 Uiso 1 1 calc R U . . .
C41 C 0.6155(4) 0.7767(2) 0.9171(2) 0.0754(11) Uani 1 1 d . . . . .
H41A H 0.668958 0.845629 0.925708 0.091 Uiso 1 1 calc R U . . .
H41B H 0.686765 0.738366 0.911927 0.091 Uiso 1 1 calc R U . . .
C39 C 0.4234(5) 0.8933(3) 0.8599(3) 0.0491(10) Uani 0.775(8) 1 d . . P B 1
H39A H 0.406410 0.931862 0.819203 0.059 Uiso 0.775(8) 1 calc R U P B 1
H39B H 0.524700 0.923911 0.898111 0.059 Uiso 0.775(8) 1 calc R U P B 1
C46 C 0.6467(5) 0.3050(3) 0.7940(3) 0.0734(10) Uani 1 1 d . . . . .
H46A H 0.541962 0.271401 0.768264 0.110 Uiso 1 1 calc R U . . .
H46B H 0.661665 0.350064 0.856678 0.110 Uiso 1 1 calc R U . . .
H46C H 0.698850 0.256049 0.795528 0.110 Uiso 1 1 calc R U . . .
C40 C 0.3181(5) 0.8976(3) 0.9217(3) 0.0638(13) Uani 0.775(8) 1 d . . P B 1
H40A H 0.217530 0.867644 0.884218 0.096 Uiso 0.775(8) 1 calc R U P B 1
H40B H 0.331241 0.966544 0.957369 0.096 Uiso 0.775(8) 1 calc R U P B 1
H40C H 0.336813 0.861563 0.963739 0.096 Uiso 0.775(8) 1 calc R U P B 1
C42 C 0.5584(7) 0.7752(4) 1.0026(2) 0.122(2) Uani 1 1 d . . . . .
H42A H 0.465552 0.722722 0.985095 0.182 Uiso 1 1 calc R U . . .
H42B H 0.542931 0.838873 1.031552 0.182 Uiso 1 1 calc R U . . .
H42C H 0.629975 0.763030 1.046096 0.182 Uiso 1 1 calc R U . . .
I3 I -0.00351(16) 1.14519(10) -0.06696(9) 0.1007(4) Uani 0.5 1 d D U P A -1
C52 C 0.4594(9) 0.9738(7) 0.8737(7) 0.044(3) Uani 0.225(8) 1 d . . P B 2
H52A H 0.399138 0.997625 0.834164 0.066 Uiso 0.225(8) 1 calc R U P B 2
H52B H 0.542352 0.962172 0.847767 0.066 Uiso 0.225(8) 1 calc R U P B 2
H52C H 0.495949 1.023190 0.935442 0.066 Uiso 0.225(8) 1 calc R U P B 2
C51 C 0.3603(14) 0.8702(8) 0.8799(7) 0.042(3) Uani 0.225(8) 1 d . . P B 2
H51A H 0.386861 0.865138 0.941800 0.051 Uiso 0.225(8) 1 calc R U P B 2
H51B H 0.254301 0.862698 0.863664 0.051 Uiso 0.225(8) 1 calc R U 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
I1 I2 2.9160(15) . ?
I1 I3 2.9250(16) . ?
N1 C1 1.360(2) . ?
N1 C7 1.385(3) . ?
N1 C10 1.384(3) . ?
N6 C6 1.365(2) . ?
N6 C30 1.389(3) . ?
N6 C27 1.395(3) . ?
N4 C4 1.361(2) . ?
N4 C19 1.386(3) . ?
N4 C22 1.400(3) . ?
N2 C2 1.365(2) . ?
N2 C14 1.395(3) . ?
N2 C11 1.388(2) . ?
N5 C5 1.368(2) . ?
N5 C26 1.398(3) . ?
N5 C23 1.392(3) . ?
N3 C3 1.360(2) . ?
N3 C15 1.401(3) . ?
N3 C18 1.395(2) . ?
C1 C6 1.368(3) . ?
C1 C2 1.367(3) . ?
C6 C5 1.363(3) . ?
C2 C3 1.365(2) . ?
C4 C5 1.370(3) . ?
C4 C3 1.375(3) . ?
C19 C18 1.476(3) . ?
C19 C20 1.405(3) . ?
C17 C16 1.426(3) . ?
C17 C18 1.401(3) . ?
C17 C37 1.507(3) . ?
C22 C23 1.478(3) . ?
C22 C21 1.396(3) . ?
C7 C30 1.456(3) . ?
C7 C8 1.400(3) . ?
C10 C11 1.452(3) . ?
C10 C9 1.398(3) . ?
C16 C15 1.400(3) . ?
C16 C35 1.497(3) . ?
C26 C25 1.404(3) . ?
C26 C27 1.473(3) . ?
C15 C14 1.481(3) . ?
C30 C29 1.392(3) . ?
C23 C24 1.406(3) . ?
C14 C13 1.414(3) . ?
C11 C12 1.391(3) . ?
C25 C24 1.419(4) . ?
C25 C45 1.505(3) . ?
C24 C43 1.500(3) . ?
C27 C28 1.416(3) . ?
C12 C13 1.428(3) . ?
C12 C31 1.504(3) . ?
C13 C33 1.505(3) . ?
C29 C28 1.427(4) . ?
C29 C49 1.501(3) . ?
C9 H9 0.9500 . ?
C9 C8 1.402(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.531(3) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.526(4) . ?
C8 H8 0.9500 . ?
C21 C20 1.425(4) . ?
C21 C41 1.506(3) . ?
C28 C47 1.501(3) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.531(4) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.521(4) . ?
C20 C39 1.493(4) . ?
C20 C51 1.638(12) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.507(4) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.500(4) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C49 C50 1.514(4) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C47 C48 1.521(4) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.523(6) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.505(7) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C52 C51 1.644(16) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?

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
I2 I1 I3 176.88(6) . . ?
C1 N1 C7 123.17(17) . . ?
C1 N1 C10 123.06(17) . . ?
C10 N1 C7 113.76(16) . . ?
C6 N6 C30 122.68(17) . . ?
C6 N6 C27 123.62(18) . . ?
C30 N6 C27 113.70(17) . . ?
C4 N4 C19 122.96(17) . . ?
C4 N4 C22 122.70(17) . . ?
C19 N4 C22 114.18(17) . . ?
C2 N2 C14 123.91(16) . . ?
C2 N2 C11 122.48(16) . . ?
C11 N2 C14 113.58(16) . . ?
C5 N5 C26 122.85(17) . . ?
C5 N5 C23 122.88(18) . . ?
C23 N5 C26 114.14(16) . . ?
C3 N3 C15 123.24(16) . . ?
C3 N3 C18 122.89(17) . . ?
C18 N3 C15 113.76(16) . . ?
N1 C1 C6 120.03(17) . . ?
N1 C1 C2 119.90(17) . . ?
C2 C1 C6 120.07(17) . . ?
N6 C6 C1 119.68(17) . . ?
C5 C6 N6 120.22(17) . . ?
C5 C6 C1 120.09(17) . . ?
N2 C2 C1 119.86(17) . . ?
N2 C2 C3 120.16(17) . . ?
C3 C2 C1 119.98(17) . . ?
N4 C4 C5 120.30(17) . . ?
N4 C4 C3 119.94(17) . . ?
C5 C4 C3 119.75(17) . . ?
N4 C19 C18 117.33(17) . . ?
N4 C19 C20 103.72(19) . . ?
C20 C19 C18 138.8(2) . . ?
N5 C5 C4 120.15(17) . . ?
C6 C5 N5 119.77(18) . . ?
C6 C5 C4 120.07(17) . . ?
C16 C17 C37 123.2(2) . . ?
C18 C17 C16 108.76(18) . . ?
C18 C17 C37 128.1(2) . . ?
N4 C22 C23 116.95(17) . . ?
C21 C22 N4 104.0(2) . . ?
C21 C22 C23 139.0(2) . . ?
N3 C3 C2 119.78(17) . . ?
N3 C3 C4 120.19(17) . . ?
C2 C3 C4 120.00(17) . . ?
N1 C7 C30 116.92(17) . . ?
N1 C7 C8 103.95(19) . . ?
C8 C7 C30 139.1(2) . . ?
N1 C10 C11 117.09(16) . . ?
N1 C10 C9 104.06(18) . . ?
C9 C10 C11 138.85(19) . . ?
C17 C16 C35 123.2(2) . . ?
C15 C16 C17 109.41(18) . . ?
C15 C16 C35 127.2(2) . . ?
N5 C26 C25 103.9(2) . . ?
N5 C26 C27 117.42(17) . . ?
C25 C26 C27 138.6(2) . . ?
N3 C15 C14 117.19(16) . . ?
C16 C15 N3 103.79(18) . . ?
C16 C15 C14 138.99(19) . . ?
N6 C30 C7 117.51(17) . . ?
N6 C30 C29 105.24(19) . . ?
C29 C30 C7 137.2(2) . . ?
N5 C23 C22 116.84(17) . . ?
N5 C23 C24 103.58(19) . . ?
C24 C23 C22 139.6(2) . . ?
N3 C18 C19 116.64(17) . . ?
N3 C18 C17 104.28(18) . . ?
C17 C18 C19 139.07(19) . . ?
N2 C14 C15 115.68(16) . . ?
N2 C14 C13 103.94(17) . . ?
C13 C14 C15 140.37(18) . . ?
N2 C11 C10 117.58(16) . . ?
N2 C11 C12 105.02(18) . . ?
C12 C11 C10 137.39(18) . . ?
C26 C25 C24 108.84(19) . . ?
C26 C25 C45 128.2(2) . . ?
C24 C25 C45 123.0(2) . . ?
C23 C24 C25 109.52(19) . . ?
C23 C24 C43 128.2(2) . . ?
C25 C24 C43 122.2(2) . . ?
N6 C27 C26 116.07(18) . . ?
N6 C27 C28 103.5(2) . . ?
C28 C27 C26 140.4(2) . . ?
C11 C12 C13 108.88(17) . . ?
C11 C12 C31 124.7(2) . . ?
C13 C12 C31 126.44(19) . . ?
C14 C13 C12 108.57(17) . . ?
C14 C13 C33 129.2(2) . . ?
C12 C13 C33 122.19(19) . . ?
C30 C29 C28 108.4(2) . . ?
C30 C29 C49 125.2(2) . . ?
C28 C29 C49 126.4(2) . . ?
C10 C9 H9 125.4 . . ?
C10 C9 C8 109.11(19) . . ?
C8 C9 H9 125.4 . . ?
C12 C31 H31A 108.6 . . ?
C12 C31 H31B 108.6 . . ?
C12 C31 C32 114.49(19) . . ?
H31A C31 H31B 107.6 . . ?
C32 C31 H31A 108.6 . . ?
C32 C31 H31B 108.6 . . ?
C17 C37 H37A 108.7 . . ?
C17 C37 H37B 108.7 . . ?
C17 C37 C38 114.1(2) . . ?
H37A C37 H37B 107.6 . . ?
C38 C37 H37A 108.7 . . ?
C38 C37 H37B 108.7 . . ?
C7 C8 C9 109.12(19) . . ?
C7 C8 H8 125.4 . . ?
C9 C8 H8 125.4 . . ?
C22 C21 C20 108.78(19) . . ?
C22 C21 C41 128.6(3) . . ?
C20 C21 C41 122.5(2) . . ?
C27 C28 C29 109.13(19) . . ?
C27 C28 C47 129.1(2) . . ?
C29 C28 C47 121.7(2) . . ?
C16 C35 H35A 109.4 . . ?
C16 C35 H35B 109.4 . . ?
C16 C35 C36 111.2(2) . . ?
H35A C35 H35B 108.0 . . ?
C36 C35 H35A 109.4 . . ?
C36 C35 H35B 109.4 . . ?
C13 C33 H33A 108.6 . . ?
C13 C33 H33B 108.6 . . ?
C13 C33 C34 114.5(2) . . ?
H33A C33 H33B 107.6 . . ?
C34 C33 H33A 108.6 . . ?
C34 C33 H33B 108.6 . . ?
C19 C20 C21 109.3(2) . . ?
C19 C20 C39 128.3(3) . . ?
C19 C20 C51 123.9(4) . . ?
C21 C20 C39 121.9(2) . . ?
C21 C20 C51 121.3(3) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C24 C43 H43A 109.0 . . ?
C24 C43 H43B 109.0 . . ?
C24 C43 C44 112.9(2) . . ?
H43A C43 H43B 107.8 . . ?
C44 C43 H43A 109.0 . . ?
C44 C43 H43B 109.0 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C25 C45 H45A 108.4 . . ?
C25 C45 H45B 108.4 . . ?
H45A C45 H45B 107.4 . . ?
C46 C45 C25 115.6(3) . . ?
C46 C45 H45A 108.4 . . ?
C46 C45 H45B 108.4 . . ?
C29 C49 H49A 108.6 . . ?
C29 C49 H49B 108.6 . . ?
C29 C49 C50 114.8(2) . . ?
H49A C49 H49B 107.5 . . ?
C50 C49 H49A 108.6 . . ?
C50 C49 H49B 108.6 . . ?
C28 C47 H47A 109.2 . . ?
C28 C47 H47B 109.2 . . ?
C28 C47 C48 111.9(2) . . ?
H47A C47 H47B 107.9 . . ?
C48 C47 H47A 109.2 . . ?
C48 C47 H47B 109.2 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C21 C41 H41A 108.4 . . ?
C21 C41 H41B 108.4 . . ?
C21 C41 C42 115.4(4) . . ?
H41A C41 H41B 107.5 . . ?
C42 C41 H41A 108.4 . . ?
C42 C41 H41B 108.4 . . ?
C20 C39 H39A 109.1 . . ?
C20 C39 H39B 109.1 . . ?
C20 C39 C40 112.3(4) . . ?
H39A C39 H39B 107.9 . . ?
C40 C39 H39A 109.1 . . ?
C40 C39 H39B 109.1 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
C20 C51 C52 100.3(8) . . ?
C20 C51 H51A 111.7 . . ?
C20 C51 H51B 111.7 . . ?
C52 C51 H51A 111.7 . . ?
C52 C51 H51B 111.7 . . ?
H51A C51 H51B 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C6 N6 -1.2(3) . . . . ?
N1 C1 C6 C5 179.50(18) . . . . ?
N1 C1 C2 N2 -1.2(3) . . . . ?
N1 C1 C2 C3 178.81(18) . . . . ?
N1 C7 C30 N6 -0.3(3) . . . . ?
N1 C7 C30 C29 179.1(2) . . . . ?
N1 C7 C8 C9 0.4(2) . . . . ?
N1 C10 C11 N2 0.8(3) . . . . ?
N1 C10 C11 C12 -178.7(2) . . . . ?
N1 C10 C9 C8 0.0(2) . . . . ?
N6 C6 C5 N5 1.2(3) . . . . ?
N6 C6 C5 C4 -177.75(18) . . . . ?
N6 C30 C29 C28 -0.1(2) . . . . ?
N6 C30 C29 C49 179.5(2) . . . . ?
N6 C27 C28 C29 0.0(2) . . . . ?
N6 C27 C28 C47 -176.8(2) . . . . ?
N4 C4 C5 N5 0.5(3) . . . . ?
N4 C4 C5 C6 179.45(18) . . . . ?
N4 C4 C3 N3 1.0(3) . . . . ?
N4 C4 C3 C2 178.86(18) . . . . ?
N4 C19 C18 N3 0.9(3) . . . . ?
N4 C19 C18 C17 -177.7(2) . . . . ?
N4 C19 C20 C21 0.2(3) . . . . ?
N4 C19 C20 C39 171.5(3) . . . . ?
N4 C19 C20 C51 -153.7(5) . . . . ?
N4 C22 C23 N5 5.0(3) . . . . ?
N4 C22 C23 C24 -174.7(2) . . . . ?
N4 C22 C21 C20 0.4(3) . . . . ?
N4 C22 C21 C41 -175.3(3) . . . . ?
N2 C2 C3 N3 -0.2(3) . . . . ?
N2 C2 C3 C4 -178.12(18) . . . . ?
N2 C14 C13 C12 -0.3(2) . . . . ?
N2 C14 C13 C33 178.8(2) . . . . ?
N2 C11 C12 C13 -0.1(2) . . . . ?
N2 C11 C12 C31 -178.47(19) . . . . ?
N5 C26 C25 C24 0.0(2) . . . . ?
N5 C26 C25 C45 179.6(2) . . . . ?
N5 C26 C27 N6 -1.0(3) . . . . ?
N5 C26 C27 C28 178.3(2) . . . . ?
N5 C23 C24 C25 -0.5(2) . . . . ?
N5 C23 C24 C43 -177.7(2) . . . . ?
N3 C15 C14 N2 -2.2(2) . . . . ?
N3 C15 C14 C13 176.8(2) . . . . ?
C1 N1 C7 C30 0.2(3) . . . . ?
C1 N1 C7 C8 -179.61(18) . . . . ?
C1 N1 C10 C11 -0.3(3) . . . . ?
C1 N1 C10 C9 179.48(18) . . . . ?
C1 C6 C5 N5 -179.52(18) . . . . ?
C1 C6 C5 C4 1.5(3) . . . . ?
C1 C2 C3 N3 179.74(18) . . . . ?
C1 C2 C3 C4 1.8(3) . . . . ?
C6 N6 C30 C7 -0.4(3) . . . . ?
C6 N6 C30 C29 -179.96(18) . . . . ?
C6 N6 C27 C26 -0.5(3) . . . . ?
C6 N6 C27 C28 179.98(18) . . . . ?
C6 C1 C2 N2 177.90(18) . . . . ?
C6 C1 C2 C3 -2.1(3) . . . . ?
C2 N2 C14 C15 1.4(3) . . . . ?
C2 N2 C14 C13 -177.95(17) . . . . ?
C2 N2 C11 C10 -1.5(3) . . . . ?
C2 N2 C11 C12 178.12(17) . . . . ?
C2 C1 C6 N6 179.66(18) . . . . ?
C2 C1 C6 C5 0.4(3) . . . . ?
C4 N4 C19 C18 1.3(3) . . . . ?
C4 N4 C19 C20 -175.46(19) . . . . ?
C4 N4 C22 C23 -4.2(3) . . . . ?
C4 N4 C22 C21 175.25(19) . . . . ?
C19 N4 C4 C5 176.54(19) . . . . ?
C19 N4 C4 C3 -2.2(3) . . . . ?
C19 N4 C22 C23 -179.68(17) . . . . ?
C19 N4 C22 C21 -0.3(2) . . . . ?
C19 C20 C39 C40 92.2(4) . . . . ?
C19 C20 C51 C52 -102.2(7) . . . . ?
C5 N5 C26 C25 -176.21(18) . . . . ?
C5 N5 C26 C27 2.6(3) . . . . ?
C5 N5 C23 C22 -3.4(3) . . . . ?
C5 N5 C23 C24 176.39(18) . . . . ?
C5 C4 C3 N3 -177.82(18) . . . . ?
C5 C4 C3 C2 0.1(3) . . . . ?
C17 C16 C15 N3 -0.3(2) . . . . ?
C17 C16 C15 C14 -178.1(2) . . . . ?
C17 C16 C35 C36 103.8(3) . . . . ?
C22 N4 C4 C5 1.4(3) . . . . ?
C22 N4 C4 C3 -177.37(18) . . . . ?
C22 N4 C19 C18 176.77(17) . . . . ?
C22 N4 C19 C20 0.0(2) . . . . ?
C22 C23 C24 C25 179.2(2) . . . . ?
C22 C23 C24 C43 2.0(4) . . . . ?
C22 C21 C20 C19 -0.4(3) . . . . ?
C22 C21 C20 C39 -172.3(3) . . . . ?
C22 C21 C20 C51 154.3(6) . . . . ?
C22 C21 C41 C42 -108.4(4) . . . . ?
C3 N3 C15 C16 -176.44(18) . . . . ?
C3 N3 C15 C14 2.0(3) . . . . ?
C3 N3 C18 C19 -2.1(3) . . . . ?
C3 N3 C18 C17 176.86(18) . . . . ?
C3 C4 C5 N5 179.31(18) . . . . ?
C3 C4 C5 C6 -1.8(3) . . . . ?
C7 N1 C1 C6 0.5(3) . . . . ?
C7 N1 C1 C2 179.67(18) . . . . ?
C7 N1 C10 C11 -179.52(17) . . . . ?
C7 N1 C10 C9 0.3(2) . . . . ?
C7 C30 C29 C28 -179.5(2) . . . . ?
C7 C30 C29 C49 0.1(4) . . . . ?
C10 N1 C1 C6 -178.59(18) . . . . ?
C10 N1 C1 C2 0.5(3) . . . . ?
C10 N1 C7 C30 179.39(17) . . . . ?
C10 N1 C7 C8 -0.4(2) . . . . ?
C10 C11 C12 C13 179.5(2) . . . . ?
C10 C11 C12 C31 1.1(4) . . . . ?
C10 C9 C8 C7 -0.2(3) . . . . ?
C16 C17 C18 N3 -0.8(2) . . . . ?
C16 C17 C18 C19 177.9(2) . . . . ?
C16 C17 C37 C38 -82.3(3) . . . . ?
C16 C15 C14 N2 175.5(2) . . . . ?
C16 C15 C14 C13 -5.5(4) . . . . ?
C26 N5 C5 C6 -2.8(3) . . . . ?
C26 N5 C5 C4 176.16(18) . . . . ?
C26 N5 C23 C22 -179.29(17) . . . . ?
C26 N5 C23 C24 0.5(2) . . . . ?
C26 C25 C24 C23 0.3(2) . . . . ?
C26 C25 C24 C43 177.7(2) . . . . ?
C26 C25 C45 C46 -104.0(3) . . . . ?
C26 C27 C28 C29 -179.3(2) . . . . ?
C26 C27 C28 C47 3.9(4) . . . . ?
C15 N3 C3 C2 -0.8(3) . . . . ?
C15 N3 C3 C4 177.14(18) . . . . ?
C15 N3 C18 C19 -178.37(17) . . . . ?
C15 N3 C18 C17 0.6(2) . . . . ?
C15 C16 C35 C36 -71.8(3) . . . . ?
C15 C14 C13 C12 -179.4(2) . . . . ?
C15 C14 C13 C33 -0.2(4) . . . . ?
C30 N6 C6 C1 1.2(3) . . . . ?
C30 N6 C6 C5 -179.54(18) . . . . ?
C30 N6 C27 C26 179.49(17) . . . . ?
C30 N6 C27 C28 -0.1(2) . . . . ?
C30 C7 C8 C9 -179.4(2) . . . . ?
C30 C29 C28 C27 0.0(3) . . . . ?
C30 C29 C28 C47 177.1(2) . . . . ?
C30 C29 C49 C50 -93.2(3) . . . . ?
C23 N5 C5 C6 -178.30(18) . . . . ?
C23 N5 C5 C4 0.6(3) . . . . ?
C23 N5 C26 C25 -0.3(2) . . . . ?
C23 N5 C26 C27 178.52(17) . . . . ?
C23 C22 C21 C20 179.6(3) . . . . ?
C23 C22 C21 C41 3.9(5) . . . . ?
C23 C24 C43 C44 74.3(3) . . . . ?
C18 N3 C3 C2 -176.63(18) . . . . ?
C18 N3 C3 C4 1.3(3) . . . . ?
C18 N3 C15 C16 -0.2(2) . . . . ?
C18 N3 C15 C14 178.19(17) . . . . ?
C18 C19 C20 C21 -175.4(3) . . . . ?
C18 C19 C20 C39 -4.1(5) . . . . ?
C18 C19 C20 C51 30.7(6) . . . . ?
C18 C17 C16 C15 0.7(2) . . . . ?
C18 C17 C16 C35 -175.6(2) . . . . ?
C18 C17 C37 C38 97.3(3) . . . . ?
C14 N2 C2 C1 179.87(18) . . . . ?
C14 N2 C2 C3 -0.2(3) . . . . ?
C14 N2 C11 C10 -179.80(17) . . . . ?
C14 N2 C11 C12 -0.1(2) . . . . ?
C14 C13 C33 C34 109.9(3) . . . . ?
C11 N2 C2 C1 1.8(3) . . . . ?
C11 N2 C2 C3 -178.26(18) . . . . ?
C11 N2 C14 C15 179.63(16) . . . . ?
C11 N2 C14 C13 0.3(2) . . . . ?
C11 C10 C9 C8 179.7(2) . . . . ?
C11 C12 C13 C14 0.2(2) . . . . ?
C11 C12 C13 C33 -178.97(19) . . . . ?
C11 C12 C31 C32 -76.4(3) . . . . ?
C25 C26 C27 N6 177.3(2) . . . . ?
C25 C26 C27 C28 -3.4(5) . . . . ?
C25 C24 C43 C44 -102.6(3) . . . . ?
C24 C25 C45 C46 75.5(3) . . . . ?
C27 N6 C6 C1 -178.89(18) . . . . ?
C27 N6 C6 C5 0.4(3) . . . . ?
C27 N6 C30 C7 179.62(17) . . . . ?
C27 N6 C30 C29 0.1(2) . . . . ?
C27 C26 C25 C24 -178.4(2) . . . . ?
C27 C26 C25 C45 1.1(4) . . . . ?
C27 C28 C47 C48 78.5(4) . . . . ?
C12 C13 C33 C34 -71.1(3) . . . . ?
C13 C12 C31 C32 105.5(3) . . . . ?
C29 C28 C47 C48 -98.0(3) . . . . ?
C9 C10 C11 N2 -178.9(2) . . . . ?
C9 C10 C11 C12 1.6(5) . . . . ?
C31 C12 C13 C14 178.62(19) . . . . ?
C31 C12 C13 C33 -0.6(3) . . . . ?
C37 C17 C16 C15 -179.7(2) . . . . ?
C37 C17 C16 C35 4.1(3) . . . . ?
C37 C17 C18 N3 179.6(2) . . . . ?
C37 C17 C18 C19 -1.8(4) . . . . ?
C8 C7 C30 N6 179.5(2) . . . . ?
C8 C7 C30 C29 -1.2(5) . . . . ?
C21 C22 C23 N5 -174.1(3) . . . . ?
C21 C22 C23 C24 6.2(5) . . . . ?
C21 C20 C39 C40 -97.5(4) . . . . ?
C21 C20 C51 C52 106.9(5) . . . . ?
C28 C29 C49 C50 86.3(3) . . . . ?
C35 C16 C15 N3 175.8(2) . . . . ?
C35 C16 C15 C14 -2.1(4) . . . . ?
C20 C19 C18 N3 176.0(3) . . . . ?
C20 C19 C18 C17 -2.5(5) . . . . ?
C20 C21 C41 C42 76.4(4) . . . . ?
C45 C25 C24 C23 -179.3(2) . . . . ?
C45 C25 C24 C43 -1.9(3) . . . . ?
C49 C29 C28 C27 -179.5(2) . . . . ?
C49 C29 C28 C47 -2.4(4) . . . . ?
C41 C21 C20 C19 175.7(3) . . . . ?
C41 C21 C20 C39 3.7(5) . . . . ?
C41 C21 C20 C51 -29.6(7) . . . . ?

_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 1.350
_oxdiff_exptl_absorpt_empirical_full_min 0.701
_exptl_crystal_recrystallization_method 
'Slow reaction in chlorobenzene solution'
####################################################################### 
# 
# 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_ethac2i3_autored_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 2394979'
loop_
_audit_author_name
_audit_author_address
'Toshio Naito'
;Ehime University
Japan
;
_audit_update_record             
;
2024-10-31 deposited with the CCDC.	2025-05-30 downloaded from the CCDC.
;
_audit_creation_date             2024-10-23
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        (EtHAC)2I3
_chemical_formula_moiety         'I3, 2(C50 H52 N6)'
_chemical_formula_sum            'C100 H104 I3 N12'
_chemical_formula_weight         1854.65
_chemical_melting_point          ?
_chemical_oxdiff_formula         C100H104N12I3
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'
I I -0.4742 1.8119 '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                   9.6685(2)
_cell_length_b                   14.7434(3)
_cell_length_c                   15.6366(3)
_cell_angle_alpha                105.909(2)
_cell_angle_beta                 99.158(2)
_cell_angle_gamma                104.078(2)
_cell_volume                     2017.34(8)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    26499
_cell_measurement_temperature    150
_cell_measurement_theta_max      31.3920
_cell_measurement_theta_min      2.2850
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.221
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             947
_exptl_crystal_size_max          0.389
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.038
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33948
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         2.238
_diffrn_ambient_temperature      150
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 7.111
_diffrn_detector_type            'Rigaku Saturn724+ area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50    6.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50    6.00    --  -20.00  45.00  90.00  360
  3  ω   -110.00  70.00   0.50    6.00    --  -20.00  45.00 180.00  360
  4  ω   -110.00  70.00   0.50    6.00    --  -20.00  45.00 270.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Rigaku Varimax with Saturn'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0289343000
_diffrn_orient_matrix_UB_12      0.0491369000
_diffrn_orient_matrix_UB_13      0.0309113000
_diffrn_orient_matrix_UB_21      0.0693163000
_diffrn_orient_matrix_UB_22      -0.0077129000
_diffrn_orient_matrix_UB_23      0.0111123000
_diffrn_orient_matrix_UB_31      0.0208492000
_diffrn_orient_matrix_UB_32      0.0167355000
_diffrn_orient_matrix_UB_33      -0.0358381000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'MicroMax 007'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8306
_reflns_number_total             9718
_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 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b46 (Rigaku, 2016)'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.268
_refine_diff_density_min         -1.867
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         9718
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0556
_refine_ls_restrained_S_all      1.081
_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)+(0.0593P)²+5.0761P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1400
_refine_ls_wR_factor_ref         0.1440
_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 Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C43(H43A,H43B), C35(H35A,H35B), C37(H37A,H37B), C45(H45A,
 H45B), C33(H33A,H33B), C49(H49A,H49B), C41(H41A,H41B), C47(H47A,H47B),
 C39(H39A,H39B)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C8(H8)
2.c Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C50(H50A,H50B,H50C), C32(H32A,H32B,H32C), C44(H44A,H44B,
 H44C), C38(H38A,H38B,H38C), C48(H48A,H48B,H48C), C40(H40A,H40B,H40C), C46(H46A,
 H46B,H46C), C34(H34A,H34B,H34C), C42(H42A,H42B,H42C)
;
_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
I1 I 0.000000 0.000000 0.000000 0.06578(16) Uani 1 2 d S . P . .
I2 I -0.03178(4) 0.16400(3) -0.06512(2) 0.07855(16) Uani 1 1 d . . . . .
N1 N 0.8446(2) 0.62750(15) 0.65431(14) 0.0175(4) Uani 1 1 d . . . . .
N2 N 0.9404(2) 0.46464(15) 0.61210(14) 0.0169(4) Uani 1 1 d . . . . .
N6 N 0.6407(2) 0.65163(16) 0.52765(15) 0.0183(4) Uani 1 1 d . . . . .
N4 N 0.6335(2) 0.35218(16) 0.31202(14) 0.0171(4) Uani 1 1 d . . . . .
N5 N 0.5303(2) 0.51265(16) 0.35729(15) 0.0179(4) Uani 1 1 d . . . . .
N3 N 0.8374(2) 0.32772(15) 0.44079(14) 0.0169(4) Uani 1 1 d . . . . .
C2 C 0.8406(3) 0.47740(18) 0.54768(16) 0.0156(4) Uani 1 1 d . . . . .
C1 C 0.7917(3) 0.55844(18) 0.56907(16) 0.0166(5) Uani 1 1 d . . . . .
C6 C 0.6884(3) 0.57029(18) 0.50557(17) 0.0171(5) Uani 1 1 d . . . . .
C10 C 0.9475(3) 0.61975(19) 0.72286(17) 0.0189(5) Uani 1 1 d . . . . .
C30 C 0.6912(3) 0.72459(19) 0.61317(18) 0.0201(5) Uani 1 1 d . . . . .
C5 C 0.6343(3) 0.50090(18) 0.41987(16) 0.0164(5) Uani 1 1 d . . . . .
C7 C 0.8007(3) 0.71146(18) 0.68140(18) 0.0196(5) Uani 1 1 d . . . . .
C3 C 0.7890(3) 0.40905(17) 0.46142(16) 0.0156(4) Uani 1 1 d . . . . .
C11 C 0.9991(3) 0.53320(19) 0.69980(17) 0.0176(5) Uani 1 1 d . . . . .
C22 C 0.5229(3) 0.35696(19) 0.24516(17) 0.0191(5) Uani 1 1 d . . . . .
C25 C 0.3831(3) 0.5803(2) 0.2907(2) 0.0227(5) Uani 1 1 d . . . . .
C24 C 0.3789(3) 0.4890(2) 0.22622(19) 0.0227(5) Uani 1 1 d . . . . .
C14 C 0.9969(3) 0.38450(18) 0.59654(17) 0.0170(5) Uani 1 1 d . . . . .
C15 C 0.9393(3) 0.30966(18) 0.50375(17) 0.0172(5) Uani 1 1 d . . . . .
C16 C 0.9512(3) 0.21782(19) 0.45491(19) 0.0201(5) Uani 1 1 d . . . . .
C26 C 0.4798(3) 0.5957(2) 0.37423(19) 0.0198(5) Uani 1 1 d . . . . .
C4 C 0.6865(3) 0.42093(18) 0.39734(16) 0.0159(5) Uani 1 1 d . . . . .
C23 C 0.4726(3) 0.44587(19) 0.26829(17) 0.0194(5) Uani 1 1 d . . . . .
C12 C 1.0990(3) 0.4955(2) 0.74315(17) 0.0196(5) Uani 1 1 d . . . . .
C29 C 0.6180(3) 0.7939(2) 0.6080(2) 0.0235(5) Uani 1 1 d . . . . .
C18 C 0.7845(3) 0.25288(18) 0.35586(17) 0.0183(5) Uani 1 1 d . . . . .
C19 C 0.6738(3) 0.26580(18) 0.28701(17) 0.0197(5) Uani 1 1 d . . . . .
C13 C 1.0983(3) 0.4042(2) 0.68027(18) 0.0193(5) Uani 1 1 d . . . . .
C17 C 0.8579(3) 0.18320(19) 0.36457(19) 0.0211(5) Uani 1 1 d . . . . .
C27 C 0.5376(3) 0.6706(2) 0.46664(19) 0.0199(5) Uani 1 1 d . . . . .
C9 C 0.9699(3) 0.7040(2) 0.79753(18) 0.0240(5) Uani 1 1 d . . . . .
H9 H 1.034583 0.721081 0.855850 0.029 Uiso 1 1 calc R U . . .
C8 C 0.8806(3) 0.7599(2) 0.77219(19) 0.0243(5) Uani 1 1 d . . . . .
H8 H 0.875726 0.820740 0.810744 0.029 Uiso 1 1 calc R U . . .
C31 C 1.1926(3) 0.5463(2) 0.83940(18) 0.0251(6) Uani 1 1 d . . . . .
H31A H 1.237757 0.616945 0.847366 0.030 Uiso 1 1 calc R U . . .
H31B H 1.273222 0.516696 0.847733 0.030 Uiso 1 1 calc R U . . .
C28 C 0.5237(3) 0.7617(2) 0.5185(2) 0.0234(5) Uani 1 1 d . . . . .
C21 C 0.4914(3) 0.2679(2) 0.17329(18) 0.0241(5) Uani 1 1 d . . . . .
C20 C 0.5831(3) 0.2123(2) 0.19867(19) 0.0246(6) Uani 1 1 d . . . . .
C43 C 0.2899(3) 0.4532(2) 0.1289(2) 0.0288(6) Uani 1 1 d . . . . .
H43A H 0.220387 0.491953 0.123643 0.035 Uiso 1 1 calc R U . . .
H43B H 0.231717 0.383004 0.112678 0.035 Uiso 1 1 calc R U . . .
C35 C 1.0380(3) 0.1590(2) 0.4905(2) 0.0266(6) Uani 1 1 d . . . . .
H35A H 1.139417 0.202148 0.522091 0.032 Uiso 1 1 calc R U . . .
H35B H 1.043622 0.104909 0.438399 0.032 Uiso 1 1 calc R U . . .
C37 C 0.8451(3) 0.0874(2) 0.2931(2) 0.0284(6) Uani 1 1 d . . . . .
H37A H 0.943928 0.078530 0.296944 0.034 Uiso 1 1 calc R U . . .
H37B H 0.810624 0.091862 0.231744 0.034 Uiso 1 1 calc R U . . .
C45 C 0.2970(3) 0.6461(2) 0.2673(2) 0.0320(7) Uani 1 1 d . . . . .
H45A H 0.296428 0.694997 0.325031 0.038 Uiso 1 1 calc R U . . .
H45B H 0.193942 0.605209 0.237260 0.038 Uiso 1 1 calc R U . . .
C33 C 1.1957(3) 0.3457(2) 0.7060(2) 0.0268(6) Uani 1 1 d . . . . .
H33A H 1.297770 0.390310 0.731449 0.032 Uiso 1 1 calc R U . . .
H33B H 1.194640 0.293905 0.649863 0.032 Uiso 1 1 calc R U . . .
C36 C 0.9683(4) 0.1149(2) 0.5572(2) 0.0352(7) Uani 1 1 d . . . . .
H36A H 0.874929 0.063733 0.523596 0.053 Uiso 1 1 calc R U . . .
H36B H 0.950562 0.167164 0.604286 0.053 Uiso 1 1 calc R U . . .
H36C H 1.034954 0.085469 0.586278 0.053 Uiso 1 1 calc R U . . .
C49 C 0.6383(4) 0.8876(2) 0.6846(2) 0.0292(6) Uani 1 1 d . . . . .
H49A H 0.670118 0.877600 0.743813 0.035 Uiso 1 1 calc R U . . .
H49B H 0.542293 0.900586 0.682943 0.035 Uiso 1 1 calc R U . . .
C41 C 0.3733(4) 0.2286(2) 0.0854(2) 0.0357(7) Uani 1 1 d . . . . .
H41A H 0.308174 0.271341 0.089926 0.043 Uiso 1 1 calc R U . . .
H41B H 0.313194 0.161643 0.080075 0.043 Uiso 1 1 calc R U . . .
C47 C 0.4338(4) 0.8223(2) 0.4888(2) 0.0323(7) Uani 1 1 d . . . . .
H47A H 0.422597 0.870148 0.543709 0.039 Uiso 1 1 calc R U . . .
H47B H 0.334601 0.778329 0.453260 0.039 Uiso 1 1 calc R U . . .
C39 C 0.5692(4) 0.1089(2) 0.1410(2) 0.0345(7) Uani 1 1 d . . . . .
H39A H 0.467471 0.077648 0.102672 0.041 Uiso 1 1 calc R U . . .
H39B H 0.586012 0.070120 0.182111 0.041 Uiso 1 1 calc R U . . .
C50 C 0.7500(4) 0.9783(2) 0.6804(2) 0.0332(7) Uani 1 1 d . . . . .
H50A H 0.722217 0.987080 0.620774 0.050 Uiso 1 1 calc R U . . .
H50B H 0.847701 0.969121 0.688380 0.050 Uiso 1 1 calc R U . . .
H50C H 0.751875 1.037109 0.729279 0.050 Uiso 1 1 calc R U . . .
C32 C 1.1094(3) 0.5400(3) 0.9144(2) 0.0340(7) Uani 1 1 d . . . . .
H32A H 1.059912 0.470446 0.905377 0.051 Uiso 1 1 calc R U . . .
H32B H 1.036180 0.575447 0.911049 0.051 Uiso 1 1 calc R U . . .
H32C H 1.178924 0.569983 0.974638 0.051 Uiso 1 1 calc R U . . .
C44 C 0.3862(4) 0.4629(3) 0.0616(2) 0.0385(8) Uani 1 1 d . . . . .
H44A H 0.324883 0.433399 -0.001251 0.058 Uiso 1 1 calc R U . . .
H44B H 0.459791 0.428504 0.069512 0.058 Uiso 1 1 calc R U . . .
H44C H 0.435886 0.533026 0.073120 0.058 Uiso 1 1 calc R U . . .
C38 C 0.7401(4) -0.0041(2) 0.3025(3) 0.0413(8) Uani 1 1 d . . . . .
H38A H 0.735088 -0.063129 0.252741 0.062 Uiso 1 1 calc R U . . .
H38B H 0.641954 0.003952 0.299028 0.062 Uiso 1 1 calc R U . . .
H38C H 0.776427 -0.011517 0.361588 0.062 Uiso 1 1 calc R U . . .
C48 C 0.5049(4) 0.8787(2) 0.4300(3) 0.0392(8) Uani 1 1 d . . . . .
H48A H 0.527414 0.832587 0.379821 0.059 Uiso 1 1 calc R U . . .
H48B H 0.595801 0.929937 0.467983 0.059 Uiso 1 1 calc R U . . .
H48C H 0.436840 0.909697 0.404708 0.059 Uiso 1 1 calc R U . . .
C40 C 0.6750(4) 0.1033(3) 0.0789(3) 0.0439(8) Uani 1 1 d . . . . .
H40A H 0.652086 0.134999 0.033268 0.066 Uiso 1 1 calc R U . . .
H40B H 0.665283 0.033815 0.047721 0.066 Uiso 1 1 calc R U . . .
H40C H 0.775982 0.137409 0.115722 0.066 Uiso 1 1 calc R U . . .
C46 C 0.3545(5) 0.7014(3) 0.2053(3) 0.0457(9) Uani 1 1 d . . . . .
H46A H 0.339096 0.654373 0.144040 0.069 Uiso 1 1 calc R U . . .
H46B H 0.459724 0.735955 0.230585 0.069 Uiso 1 1 calc R U . . .
H46C H 0.301822 0.749657 0.201109 0.069 Uiso 1 1 calc R U . . .
C34 C 1.1515(4) 0.2964(3) 0.7759(3) 0.0404(8) Uani 1 1 d . . . . .
H34A H 1.048543 0.255294 0.753165 0.061 Uiso 1 1 calc R U . . .
H34B H 1.163525 0.347391 0.834285 0.061 Uiso 1 1 calc R U . . .
H34C H 1.214090 0.254925 0.784903 0.061 Uiso 1 1 calc R U . . .
C42 C 0.4261(5) 0.2223(4) -0.0024(2) 0.0546(11) Uani 1 1 d . . . . .
H42A H 0.344955 0.217044 -0.051663 0.082 Uiso 1 1 calc R U . . .
H42B H 0.459967 0.163870 -0.019808 0.082 Uiso 1 1 calc R U . . .
H42C H 0.507253 0.281894 0.007934 0.082 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 I2 2.9307(5) 2 ?
I1 I2 2.9308(5) . ?
N1 C1 1.364(3) . ?
N1 C10 1.391(3) . ?
N1 C7 1.385(3) . ?
N2 C2 1.365(3) . ?
N2 C11 1.392(3) . ?
N2 C14 1.397(3) . ?
N6 C6 1.365(3) . ?
N6 C30 1.390(3) . ?
N6 C27 1.400(3) . ?
N4 C22 1.401(3) . ?
N4 C4 1.363(3) . ?
N4 C19 1.394(3) . ?
N5 C5 1.365(3) . ?
N5 C26 1.401(3) . ?
N5 C23 1.397(3) . ?
N3 C3 1.367(3) . ?
N3 C15 1.404(3) . ?
N3 C18 1.396(3) . ?
C2 C1 1.367(3) . ?
C2 C3 1.371(3) . ?
C1 C6 1.371(4) . ?
C6 C5 1.372(3) . ?
C10 C11 1.457(4) . ?
C10 C9 1.396(4) . ?
C30 C7 1.466(4) . ?
C30 C29 1.389(4) . ?
C5 C4 1.374(4) . ?
C7 C8 1.396(4) . ?
C3 C4 1.372(3) . ?
C11 C12 1.400(4) . ?
C22 C23 1.480(4) . ?
C22 C21 1.402(4) . ?
C25 C24 1.430(4) . ?
C25 C26 1.407(4) . ?
C25 C45 1.503(4) . ?
C24 C23 1.406(4) . ?
C24 C43 1.502(4) . ?
C14 C15 1.483(3) . ?
C14 C13 1.416(3) . ?
C15 C16 1.402(4) . ?
C16 C17 1.430(4) . ?
C16 C35 1.496(4) . ?
C26 C27 1.479(4) . ?
C12 C13 1.431(4) . ?
C12 C31 1.505(4) . ?
C29 C28 1.426(4) . ?
C29 C49 1.506(4) . ?
C18 C19 1.479(4) . ?
C18 C17 1.406(4) . ?
C19 C20 1.407(4) . ?
C13 C33 1.503(4) . ?
C17 C37 1.505(4) . ?
C27 C28 1.415(4) . ?
C9 H9 0.9500 . ?
C9 C8 1.413(4) . ?
C8 H8 0.9500 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.535(4) . ?
C28 C47 1.499(4) . ?
C21 C20 1.427(4) . ?
C21 C41 1.506(4) . ?
C20 C39 1.505(4) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.525(4) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.532(4) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.537(5) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.517(5) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.528(4) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C49 C50 1.526(4) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.527(5) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C47 C48 1.533(5) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.520(5) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?

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
I2 I1 I2 180.0 2 . ?
C1 N1 C10 123.0(2) . . ?
C1 N1 C7 123.6(2) . . ?
C7 N1 C10 113.4(2) . . ?
C2 N2 C11 122.4(2) . . ?
C2 N2 C14 124.1(2) . . ?
C11 N2 C14 113.5(2) . . ?
C6 N6 C30 123.0(2) . . ?
C6 N6 C27 123.7(2) . . ?
C30 N6 C27 113.3(2) . . ?
C4 N4 C22 122.9(2) . . ?
C4 N4 C19 122.7(2) . . ?
C19 N4 C22 114.0(2) . . ?
C5 N5 C26 123.2(2) . . ?
C5 N5 C23 122.6(2) . . ?
C23 N5 C26 114.1(2) . . ?
C3 N3 C15 123.4(2) . . ?
C3 N3 C18 122.6(2) . . ?
C18 N3 C15 114.0(2) . . ?
N2 C2 C1 120.0(2) . . ?
N2 C2 C3 120.2(2) . . ?
C1 C2 C3 119.8(2) . . ?
N1 C1 C2 120.0(2) . . ?
N1 C1 C6 119.6(2) . . ?
C2 C1 C6 120.4(2) . . ?
N6 C6 C1 119.8(2) . . ?
N6 C6 C5 120.2(2) . . ?
C1 C6 C5 119.9(2) . . ?
N1 C10 C11 116.8(2) . . ?
N1 C10 C9 104.3(2) . . ?
C9 C10 C11 138.9(2) . . ?
N6 C30 C7 117.1(2) . . ?
C29 C30 N6 105.5(2) . . ?
C29 C30 C7 137.4(3) . . ?
N5 C5 C6 119.6(2) . . ?
N5 C5 C4 120.6(2) . . ?
C6 C5 C4 119.8(2) . . ?
N1 C7 C30 116.8(2) . . ?
N1 C7 C8 104.3(2) . . ?
C8 C7 C30 138.9(2) . . ?
N3 C3 C2 119.5(2) . . ?
N3 C3 C4 120.4(2) . . ?
C2 C3 C4 120.1(2) . . ?
N2 C11 C10 117.8(2) . . ?
N2 C11 C12 105.0(2) . . ?
C12 C11 C10 137.2(2) . . ?
N4 C22 C23 116.7(2) . . ?
N4 C22 C21 104.0(2) . . ?
C21 C22 C23 139.2(2) . . ?
C24 C25 C45 123.0(3) . . ?
C26 C25 C24 108.8(2) . . ?
C26 C25 C45 128.2(3) . . ?
C25 C24 C43 121.9(2) . . ?
C23 C24 C25 109.3(2) . . ?
C23 C24 C43 128.8(3) . . ?
N2 C14 C15 115.7(2) . . ?
N2 C14 C13 104.2(2) . . ?
C13 C14 C15 140.1(2) . . ?
N3 C15 C14 117.1(2) . . ?
C16 C15 N3 103.7(2) . . ?
C16 C15 C14 139.2(2) . . ?
C15 C16 C17 109.5(2) . . ?
C15 C16 C35 127.1(2) . . ?
C17 C16 C35 123.3(2) . . ?
N5 C26 C25 104.0(2) . . ?
N5 C26 C27 117.3(2) . . ?
C25 C26 C27 138.7(2) . . ?
N4 C4 C5 119.9(2) . . ?
N4 C4 C3 120.1(2) . . ?
C3 C4 C5 120.0(2) . . ?
N5 C23 C22 117.0(2) . . ?
N5 C23 C24 103.9(2) . . ?
C24 C23 C22 139.1(2) . . ?
C11 C12 C13 108.7(2) . . ?
C11 C12 C31 124.2(2) . . ?
C13 C12 C31 127.0(2) . . ?
C30 C29 C28 108.5(2) . . ?
C30 C29 C49 124.9(3) . . ?
C28 C29 C49 126.5(3) . . ?
N3 C18 C19 116.9(2) . . ?
N3 C18 C17 104.2(2) . . ?
C17 C18 C19 138.9(2) . . ?
N4 C19 C18 117.2(2) . . ?
N4 C19 C20 103.9(2) . . ?
C20 C19 C18 138.8(2) . . ?
C14 C13 C12 108.6(2) . . ?
C14 C13 C33 129.6(3) . . ?
C12 C13 C33 121.7(2) . . ?
C16 C17 C37 123.7(2) . . ?
C18 C17 C16 108.7(2) . . ?
C18 C17 C37 127.6(3) . . ?
N6 C27 C26 115.9(2) . . ?
N6 C27 C28 103.6(2) . . ?
C28 C27 C26 140.4(2) . . ?
C10 C9 H9 125.6 . . ?
C10 C9 C8 108.8(2) . . ?
C8 C9 H9 125.6 . . ?
C7 C8 C9 109.1(2) . . ?
C7 C8 H8 125.5 . . ?
C9 C8 H8 125.5 . . ?
C12 C31 H31A 108.7 . . ?
C12 C31 H31B 108.7 . . ?
C12 C31 C32 114.4(2) . . ?
H31A C31 H31B 107.6 . . ?
C32 C31 H31A 108.7 . . ?
C32 C31 H31B 108.7 . . ?
C29 C28 C47 122.1(3) . . ?
C27 C28 C29 109.1(2) . . ?
C27 C28 C47 128.8(3) . . ?
C22 C21 C20 109.0(2) . . ?
C22 C21 C41 128.0(3) . . ?
C20 C21 C41 122.8(3) . . ?
C19 C20 C21 109.2(2) . . ?
C19 C20 C39 127.4(3) . . ?
C21 C20 C39 123.2(3) . . ?
C24 C43 H43A 109.2 . . ?
C24 C43 H43B 109.2 . . ?
C24 C43 C44 112.2(2) . . ?
H43A C43 H43B 107.9 . . ?
C44 C43 H43A 109.2 . . ?
C44 C43 H43B 109.2 . . ?
C16 C35 H35A 109.3 . . ?
C16 C35 H35B 109.3 . . ?
C16 C35 C36 111.4(2) . . ?
H35A C35 H35B 108.0 . . ?
C36 C35 H35A 109.3 . . ?
C36 C35 H35B 109.3 . . ?
C17 C37 H37A 108.7 . . ?
C17 C37 H37B 108.7 . . ?
C17 C37 C38 114.1(3) . . ?
H37A C37 H37B 107.6 . . ?
C38 C37 H37A 108.7 . . ?
C38 C37 H37B 108.7 . . ?
C25 C45 H45A 108.5 . . ?
C25 C45 H45B 108.5 . . ?
C25 C45 C46 114.9(3) . . ?
H45A C45 H45B 107.5 . . ?
C46 C45 H45A 108.5 . . ?
C46 C45 H45B 108.5 . . ?
C13 C33 H33A 108.7 . . ?
C13 C33 H33B 108.7 . . ?
C13 C33 C34 114.2(3) . . ?
H33A C33 H33B 107.6 . . ?
C34 C33 H33A 108.7 . . ?
C34 C33 H33B 108.7 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C29 C49 H49A 108.7 . . ?
C29 C49 H49B 108.7 . . ?
C29 C49 C50 114.0(2) . . ?
H49A C49 H49B 107.6 . . ?
C50 C49 H49A 108.7 . . ?
C50 C49 H49B 108.7 . . ?
C21 C41 H41A 108.3 . . ?
C21 C41 H41B 108.3 . . ?
C21 C41 C42 116.1(3) . . ?
H41A C41 H41B 107.4 . . ?
C42 C41 H41A 108.3 . . ?
C42 C41 H41B 108.3 . . ?
C28 C47 H47A 109.3 . . ?
C28 C47 H47B 109.3 . . ?
C28 C47 C48 111.8(3) . . ?
H47A C47 H47B 107.9 . . ?
C48 C47 H47A 109.3 . . ?
C48 C47 H47B 109.3 . . ?
C20 C39 H39A 108.7 . . ?
C20 C39 H39B 108.7 . . ?
C20 C39 C40 114.3(3) . . ?
H39A C39 H39B 107.6 . . ?
C40 C39 H39A 108.7 . . ?
C40 C39 H39B 108.7 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C6 N6 0.9(4) . . . . ?
N1 C1 C6 C5 -179.7(2) . . . . ?
N1 C10 C11 N2 -0.9(3) . . . . ?
N1 C10 C11 C12 178.7(3) . . . . ?
N1 C10 C9 C8 0.0(3) . . . . ?
N1 C7 C8 C9 -0.2(3) . . . . ?
N2 C2 C1 N1 1.2(4) . . . . ?
N2 C2 C1 C6 -178.1(2) . . . . ?
N2 C2 C3 N3 0.5(4) . . . . ?
N2 C2 C3 C4 178.7(2) . . . . ?
N2 C11 C12 C13 -0.1(3) . . . . ?
N2 C11 C12 C31 178.4(2) . . . . ?
N2 C14 C15 N3 1.4(3) . . . . ?
N2 C14 C15 C16 -176.1(3) . . . . ?
N2 C14 C13 C12 0.0(3) . . . . ?
N2 C14 C13 C33 -179.1(3) . . . . ?
N6 C6 C5 N5 -1.2(4) . . . . ?
N6 C6 C5 C4 177.9(2) . . . . ?
N6 C30 C7 N1 0.3(3) . . . . ?
N6 C30 C7 C8 -179.2(3) . . . . ?
N6 C30 C29 C28 -0.2(3) . . . . ?
N6 C30 C29 C49 -179.4(3) . . . . ?
N6 C27 C28 C29 0.0(3) . . . . ?
N6 C27 C28 C47 177.0(3) . . . . ?
N4 C22 C23 N5 -5.5(3) . . . . ?
N4 C22 C23 C24 173.8(3) . . . . ?
N4 C22 C21 C20 0.1(3) . . . . ?
N4 C22 C21 C41 175.2(3) . . . . ?
N4 C19 C20 C21 0.0(3) . . . . ?
N4 C19 C20 C39 -174.2(3) . . . . ?
N5 C5 C4 N4 -0.4(4) . . . . ?
N5 C5 C4 C3 -178.8(2) . . . . ?
N5 C26 C27 N6 1.5(3) . . . . ?
N5 C26 C27 C28 -178.6(3) . . . . ?
N3 C3 C4 N4 -0.9(4) . . . . ?
N3 C3 C4 C5 177.5(2) . . . . ?
N3 C15 C16 C17 0.3(3) . . . . ?
N3 C15 C16 C35 -175.8(3) . . . . ?
N3 C18 C19 N4 1.1(3) . . . . ?
N3 C18 C19 C20 -174.4(3) . . . . ?
N3 C18 C17 C16 0.7(3) . . . . ?
N3 C18 C17 C37 -179.0(3) . . . . ?
C2 N2 C11 C10 1.7(4) . . . . ?
C2 N2 C11 C12 -178.1(2) . . . . ?
C2 N2 C14 C15 -1.2(3) . . . . ?
C2 N2 C14 C13 178.0(2) . . . . ?
C2 C1 C6 N6 -179.9(2) . . . . ?
C2 C1 C6 C5 -0.4(4) . . . . ?
C2 C3 C4 N4 -179.0(2) . . . . ?
C2 C3 C4 C5 -0.6(4) . . . . ?
C1 N1 C10 C11 0.4(4) . . . . ?
C1 N1 C10 C9 -179.7(2) . . . . ?
C1 N1 C7 C30 0.1(4) . . . . ?
C1 N1 C7 C8 179.7(2) . . . . ?
C1 C2 C3 N3 -179.4(2) . . . . ?
C1 C2 C3 C4 -1.3(4) . . . . ?
C1 C6 C5 N5 179.3(2) . . . . ?
C1 C6 C5 C4 -1.5(4) . . . . ?
C6 N6 C30 C7 -0.1(4) . . . . ?
C6 N6 C30 C29 179.6(2) . . . . ?
C6 N6 C27 C26 0.5(4) . . . . ?
C6 N6 C27 C28 -179.5(2) . . . . ?
C6 C5 C4 N4 -179.6(2) . . . . ?
C6 C5 C4 C3 2.1(4) . . . . ?
C10 N1 C1 C2 -0.5(4) . . . . ?
C10 N1 C1 C6 178.8(2) . . . . ?
C10 N1 C7 C30 -179.4(2) . . . . ?
C10 N1 C7 C8 0.2(3) . . . . ?
C10 C11 C12 C13 -179.8(3) . . . . ?
C10 C11 C12 C31 -1.2(5) . . . . ?
C10 C9 C8 C7 0.1(3) . . . . ?
C30 N6 C6 C1 -0.5(4) . . . . ?
C30 N6 C6 C5 -179.9(2) . . . . ?
C30 N6 C27 C26 179.8(2) . . . . ?
C30 N6 C27 C28 -0.1(3) . . . . ?
C30 C7 C8 C9 179.3(3) . . . . ?
C30 C29 C28 C27 0.1(3) . . . . ?
C30 C29 C28 C47 -177.1(3) . . . . ?
C30 C29 C49 C50 94.7(3) . . . . ?
C5 N5 C26 C25 176.1(2) . . . . ?
C5 N5 C26 C27 -3.5(4) . . . . ?
C5 N5 C23 C22 3.4(4) . . . . ?
C5 N5 C23 C24 -176.1(2) . . . . ?
C7 N1 C1 C2 -179.9(2) . . . . ?
C7 N1 C1 C6 -0.6(4) . . . . ?
C7 N1 C10 C11 179.9(2) . . . . ?
C7 N1 C10 C9 -0.1(3) . . . . ?
C7 C30 C29 C28 179.3(3) . . . . ?
C7 C30 C29 C49 0.2(5) . . . . ?
C3 N3 C15 C14 -0.8(4) . . . . ?
C3 N3 C15 C16 177.6(2) . . . . ?
C3 N3 C18 C19 1.0(4) . . . . ?
C3 N3 C18 C17 -178.0(2) . . . . ?
C3 C2 C1 N1 -178.9(2) . . . . ?
C3 C2 C1 C6 1.8(4) . . . . ?
C11 N2 C2 C1 -1.8(4) . . . . ?
C11 N2 C2 C3 178.2(2) . . . . ?
C11 N2 C14 C15 -179.4(2) . . . . ?
C11 N2 C14 C13 -0.1(3) . . . . ?
C11 C10 C9 C8 180.0(3) . . . . ?
C11 C12 C13 C14 0.0(3) . . . . ?
C11 C12 C13 C33 179.3(2) . . . . ?
C11 C12 C31 C32 75.1(4) . . . . ?
C22 N4 C4 C5 -2.0(4) . . . . ?
C22 N4 C4 C3 176.3(2) . . . . ?
C22 N4 C19 C18 -176.9(2) . . . . ?
C22 N4 C19 C20 0.0(3) . . . . ?
C22 C21 C20 C19 -0.1(3) . . . . ?
C22 C21 C20 C39 174.5(3) . . . . ?
C22 C21 C41 C42 112.9(4) . . . . ?
C25 C24 C23 N5 0.2(3) . . . . ?
C25 C24 C23 C22 -179.1(3) . . . . ?
C25 C24 C43 C44 106.8(3) . . . . ?
C25 C26 C27 N6 -177.9(3) . . . . ?
C25 C26 C27 C28 2.1(6) . . . . ?
C24 C25 C26 N5 -0.2(3) . . . . ?
C24 C25 C26 C27 179.1(3) . . . . ?
C24 C25 C45 C46 -72.5(4) . . . . ?
C14 N2 C2 C1 -179.8(2) . . . . ?
C14 N2 C2 C3 0.2(4) . . . . ?
C14 N2 C11 C10 179.9(2) . . . . ?
C14 N2 C11 C12 0.1(3) . . . . ?
C14 C15 C16 C17 178.0(3) . . . . ?
C14 C15 C16 C35 2.0(5) . . . . ?
C14 C13 C33 C34 -110.3(3) . . . . ?
C15 N3 C3 C2 -0.2(4) . . . . ?
C15 N3 C3 C4 -178.3(2) . . . . ?
C15 N3 C18 C19 178.4(2) . . . . ?
C15 N3 C18 C17 -0.6(3) . . . . ?
C15 C14 C13 C12 179.0(3) . . . . ?
C15 C14 C13 C33 -0.2(5) . . . . ?
C15 C16 C17 C18 -0.7(3) . . . . ?
C15 C16 C17 C37 179.1(2) . . . . ?
C15 C16 C35 C36 71.0(4) . . . . ?
C16 C17 C37 C38 82.0(4) . . . . ?
C26 N5 C5 C6 3.4(4) . . . . ?
C26 N5 C5 C4 -175.8(2) . . . . ?
C26 N5 C23 C22 179.1(2) . . . . ?
C26 N5 C23 C24 -0.3(3) . . . . ?
C26 C25 C24 C23 0.0(3) . . . . ?
C26 C25 C24 C43 -177.5(2) . . . . ?
C26 C25 C45 C46 106.3(4) . . . . ?
C26 C27 C28 C29 -180.0(3) . . . . ?
C26 C27 C28 C47 -2.9(6) . . . . ?
C4 N4 C22 C23 5.0(4) . . . . ?
C4 N4 C22 C21 -173.7(2) . . . . ?
C4 N4 C19 C18 -3.2(4) . . . . ?
C4 N4 C19 C20 173.7(2) . . . . ?
C23 N5 C5 C6 178.7(2) . . . . ?
C23 N5 C5 C4 -0.4(4) . . . . ?
C23 N5 C26 C25 0.4(3) . . . . ?
C23 N5 C26 C27 -179.2(2) . . . . ?
C23 C22 C21 C20 -178.2(3) . . . . ?
C23 C22 C21 C41 -3.1(6) . . . . ?
C23 C24 C43 C44 -70.2(4) . . . . ?
C12 C13 C33 C34 70.6(3) . . . . ?
C29 C30 C7 N1 -179.2(3) . . . . ?
C29 C30 C7 C8 1.3(6) . . . . ?
C29 C28 C47 C48 100.6(3) . . . . ?
C18 N3 C3 C2 176.9(2) . . . . ?
C18 N3 C3 C4 -1.2(4) . . . . ?
C18 N3 C15 C14 -178.2(2) . . . . ?
C18 N3 C15 C16 0.2(3) . . . . ?
C18 C19 C20 C21 175.9(3) . . . . ?
C18 C19 C20 C39 1.7(6) . . . . ?
C18 C17 C37 C38 -98.2(4) . . . . ?
C19 N4 C22 C23 178.6(2) . . . . ?
C19 N4 C22 C21 -0.1(3) . . . . ?
C19 N4 C4 C5 -175.2(2) . . . . ?
C19 N4 C4 C3 3.2(4) . . . . ?
C19 C18 C17 C16 -177.9(3) . . . . ?
C19 C18 C17 C37 2.3(5) . . . . ?
C19 C20 C39 C40 -90.0(4) . . . . ?
C13 C14 C15 N3 -177.4(3) . . . . ?
C13 C14 C15 C16 5.0(6) . . . . ?
C13 C12 C31 C32 -106.6(3) . . . . ?
C17 C16 C35 C36 -104.6(3) . . . . ?
C17 C18 C19 N4 179.7(3) . . . . ?
C17 C18 C19 C20 4.2(6) . . . . ?
C27 N6 C6 C1 178.8(2) . . . . ?
C27 N6 C6 C5 -0.7(4) . . . . ?
C27 N6 C30 C7 -179.4(2) . . . . ?
C27 N6 C30 C29 0.2(3) . . . . ?
C27 C28 C47 C48 -76.1(4) . . . . ?
C9 C10 C11 N2 179.1(3) . . . . ?
C9 C10 C11 C12 -1.3(6) . . . . ?
C31 C12 C13 C14 -178.4(2) . . . . ?
C31 C12 C13 C33 0.8(4) . . . . ?
C28 C29 C49 C50 -84.3(4) . . . . ?
C21 C22 C23 N5 172.6(3) . . . . ?
C21 C22 C23 C24 -8.1(6) . . . . ?
C21 C20 C39 C40 96.5(4) . . . . ?
C20 C21 C41 C42 -72.7(4) . . . . ?
C43 C24 C23 N5 177.5(3) . . . . ?
C43 C24 C23 C22 -1.8(5) . . . . ?
C35 C16 C17 C18 175.6(2) . . . . ?
C35 C16 C17 C37 -4.6(4) . . . . ?
C45 C25 C24 C23 179.1(3) . . . . ?
C45 C25 C24 C43 1.5(4) . . . . ?
C45 C25 C26 N5 -179.2(3) . . . . ?
C45 C25 C26 C27 0.2(5) . . . . ?
C49 C29 C28 C27 179.3(3) . . . . ?
C49 C29 C28 C47 2.0(4) . . . . ?
C41 C21 C20 C19 -175.4(3) . . . . ?
C41 C21 C20 C39 -0.9(5) . . . . ?

_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 1.368
_oxdiff_exptl_absorpt_empirical_full_min 0.732
_exptl_crystal_recrystallization_method 
'Slow reaction in chlorobenzene solution'
_exptl_crystal_preparation       'Magnetic properties,Conducting properties'
