# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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. 
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#######################################################################

data_kato_200909_1
_database_code_depnum_ccdc_archive 'CCDC 2305237'
loop_
_audit_author_name
_audit_author_address
'Koji Hirano'
;Osaka University
Japan
;
_audit_update_record             
;
2023-11-02 deposited with the CCDC.	2024-01-02 downloaded from the CCDC.
;
_audit_creation_date             2020-09-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C29 H18 F3 N'
_chemical_formula_sum            'C29 H18 F3 N'
_chemical_formula_weight         437.44
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C29 H18 F3 N'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y, x+1/2, z+1/2'
'y+1/2, -x, z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y, -x-1/2, -z-1/2'
'-y-1/2, x, -z-1/2'

_cell_length_a                   22.8051(3)
_cell_length_b                   22.8051(3)
_cell_length_c                   8.2792(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4305.78(15)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    7818
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.0870
_cell_measurement_theta_min      3.8290
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.796
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.43a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1808
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 14 1 0.1234
-13 7 -1 0.0575
1 -14 -1 0.1211
10 -11 0 0.1166
14 2 2 0.0975
7 13 0 0.1249
1 0 -5 0.1166
-7 -13 0 0.1214
-1 1 5 0.1087
14 -2 -1 0.1132
14 5 0 0.0957
0 -15 0 0.1001

_exptl_crystal_size_max          0.254
_exptl_crystal_size_mid          0.247
_exptl_crystal_size_min          0.182
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.1410 14.2615 1.4381 0.0108 0.4432 0.8964
-12.8610 6.7032 -1.0643 0.0257 0.9970 -0.0734
0.7136 -14.3231 -1.3292 -0.0122 -0.4973 -0.8675
9.5376 -11.2989 0.1596 -0.0239 -0.9398 -0.3409
13.6113 1.8108 2.0126 -0.0203 -0.7730 0.6340
7.2003 12.9367 0.1080 0.3633 0.0295 0.9312
1.1632 -0.1967 -5.3576 0.9309 0.0735 -0.3579
-7.2120 -12.9328 -0.0498 -0.3734 -0.0302 -0.9272
-0.8331 0.7881 5.3586 -0.9136 -0.0721 0.4002
14.4239 -1.5309 -1.0755 0.4622 -0.8499 0.2529
14.0651 4.6211 0.1533 0.3547 -0.6514 0.6708
0.4016 -14.7352 0.4708 -0.3317 -0.5429 -0.7715

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            18566
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.249
_diffrn_reflns_theta_min         3.877
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     82.00 131.00   0.50    0.40    --   76.50  89.00 168.00   98
  2  ω   -176.00 -85.00   0.50    0.40    -- -106.00 -93.00 -46.00  182
  3  ω    -71.00 -46.00   0.50    0.40    -- -106.00  46.00 -42.00   50
  4  ω   -127.00-101.00   0.50    0.40    -- -106.00  46.00 -42.00   52
  5  ω    -62.00  33.00   0.50    0.12    --  -42.80  46.00 -42.00  190
  6  ω   -116.00 -87.00   0.50    0.12    --  -42.80-125.00 -30.00   58
  7  ω   -107.00 -70.00   0.50    0.12    --  -42.80-125.00  90.00   74
  8  ω     30.00  75.00   0.50    0.12    --   42.80-125.00-180.00   90
  9  ω    -65.00 -35.00   0.50    0.40    -- -106.00 125.00  30.00   60
 10  ω   -117.00 -75.00   0.50    0.40    -- -106.00 125.00  30.00   84
 11  ω    -91.00 -65.00   0.50    0.40    -- -106.00 125.00 120.00   52
 12  ω   -156.00-130.00   0.50    0.40    -- -106.00 -37.00 120.00   52
 13  ω   -177.00 -83.00   0.50    0.40    -- -106.00 -99.00   0.00  188
 14  ω   -163.00 -83.00   0.50    0.40    -- -106.00 -37.00   0.00  160
 15  ω    -97.00 -64.00   0.50    0.40    -- -106.00  57.00-180.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0212630000
_diffrn_orient_matrix_UB_12      0.0176673000
_diffrn_orient_matrix_UB_13      -0.1697788000
_diffrn_orient_matrix_UB_21      -0.0573166000
_diffrn_orient_matrix_UB_22      0.0344070000
_diffrn_orient_matrix_UB_23      -0.0274186000
_diffrn_orient_matrix_UB_31      0.0287116000
_diffrn_orient_matrix_UB_32      0.0554080000
_diffrn_orient_matrix_UB_33      0.0710069000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3654
_reflns_number_total             4300
_reflns_odcompleteness_completeness 99.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         4300
_refine_ls_number_restraints     158
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0918
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1706P)²+3.1964P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2877
_refine_ls_wR_factor_ref         0.2963
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C20, C15, C16, C17, C18, C19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C15A, C16A, C17A, C18A, C19A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C21A, C22A, C23A, C24A, C14A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C14, C13, C21, C22, C23, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C20 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C15A \\sim C16A \\sim C17A \\sim C18A \\sim C19A: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
C21A \\sim C22A \\sim C23A \\sim C24A \\sim C14A: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
C13 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C14: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=
 Sof(H24A)=Sof(C14A)=Sof(C15A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=
 Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=1-FVAR(1)
 Sof(C15)=Sof(C14)=Sof(C19)=Sof(H19)=Sof(C21)=Sof(H21)=Sof(C24)=Sof(H24)=
 Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=Sof(C16)=Sof(H16)=Sof(C23)=Sof(H23)=
 Sof(C22)=Sof(H22)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C27(H27), C28(H28), C4(H4), C19(H19), C21(H21), C25(H25),
 C24(H24), C26(H26), C17(H17), C18(H18), C16(H16), C23(H23), C22(H22),
 C21A(H21A), C22A(H22A), C23A(H23A), C24A(H24A), C16A(H16A), C17A(H17A),
 C18A(H18A), C19A(H19A)
5.b Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C)
;
_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
N12 N 0.02459(12) 0.53574(11) 0.3348(4) 0.0527(7) Uani 1 1 d . . . . .
F30 F 0.32495(13) 0.61470(14) 0.6557(4) 0.0970(9) Uani 1 1 d . . . . .
F31 F 0.27882(14) 0.69233(14) 0.7166(4) 0.1065(11) Uani 1 1 d . . . . .
C9 C 0.11046(12) 0.48800(12) 0.2901(3) 0.0405(6) Uani 1 1 d . . . . .
C8 C 0.17639(12) 0.48987(12) 0.3126(3) 0.0398(6) Uani 1 1 d . . . . .
C7 C 0.18264(13) 0.54704(12) 0.4084(3) 0.0435(7) Uani 1 1 d . . . . .
C1 C 0.08401(13) 0.53578(12) 0.3614(4) 0.0438(7) Uani 1 1 d . . . . .
C2 C 0.12759(13) 0.57300(13) 0.4379(4) 0.0458(7) Uani 1 1 d . . . . .
C10 C 0.06751(13) 0.45483(13) 0.2101(3) 0.0454(7) Uani 1 1 d . . . . .
C20 C 0.20224(14) 0.43569(12) 0.3945(4) 0.0499(8) Uani 1 1 d . U . . .
C13 C 0.20868(13) 0.48911(15) 0.1513(4) 0.0495(7) Uani 1 1 d . U . . .
C3 C 0.12545(16) 0.62499(14) 0.5252(4) 0.0529(8) Uani 1 1 d . . . . .
H3 H 0.089605 0.642473 0.548760 0.063 Uiso 1 1 calc R . . . .
F32 F 0.31508(17) 0.68129(19) 0.4823(4) 0.1275(15) Uani 1 1 d . . . . .
C11 C 0.01248(15) 0.48647(14) 0.2397(4) 0.0539(8) Uani 1 1 d . . . . .
C6 C 0.23342(16) 0.57406(15) 0.4610(4) 0.0542(8) Uani 1 1 d . . . . .
H6 H 0.269701 0.557140 0.439581 0.065 Uiso 1 1 calc R . . . .
C15 C 0.2440(5) 0.4102(5) 0.2760(14) 0.0391(18) Uani 0.63(2) 1 d . U P A 1
C14 C 0.2458(5) 0.4455(5) 0.1294(11) 0.040(2) Uani 0.63(2) 1 d . U P A 1
C27 C 0.01125(17) 0.38550(18) 0.0491(6) 0.0681(10) Uani 1 1 d . . . . .
H27 H 0.010176 0.352568 -0.017102 0.082 Uiso 1 1 calc R . . . .
C28 C 0.06518(16) 0.40496(15) 0.1157(4) 0.0561(8) Uani 1 1 d . . . . .
H28 H 0.099333 0.383911 0.095491 0.067 Uiso 1 1 calc R . . . .
C5 C 0.23024(18) 0.62606(16) 0.5451(4) 0.0616(9) Uani 1 1 d . . . . .
C4 C 0.17744(19) 0.65056(18) 0.5769(5) 0.0658(9) Uani 1 1 d . . . . .
H4 H 0.175936 0.685440 0.635014 0.079 Uiso 1 1 calc R . . . .
C19 C 0.1954(5) 0.4112(5) 0.5318(15) 0.052(2) Uani 0.63(2) 1 d . U P A 1
H19 H 0.169577 0.428002 0.605474 0.063 Uiso 0.63(2) 1 calc R . P A 1
C21 C 0.2012(5) 0.5338(5) 0.0287(15) 0.049(2) Uani 0.63(2) 1 d . U P A 1
H21 H 0.177559 0.566362 0.046434 0.058 Uiso 0.63(2) 1 calc R . P A 1
C25 C -0.04006(16) 0.46728(18) 0.1781(5) 0.0658(10) Uani 1 1 d . . . . .
H25 H -0.074529 0.487750 0.198761 0.079 Uiso 1 1 calc R . . . .
C24 C 0.2759(4) 0.4370(6) -0.0188(13) 0.055(2) Uani 0.63(2) 1 d . U P A 1
H24 H 0.300305 0.404833 -0.034863 0.066 Uiso 0.63(2) 1 calc R . P A 1
C26 C -0.0408(2) 0.41656(19) 0.0841(6) 0.0749(11) Uani 1 1 d . . . . .
H26 H -0.076257 0.402896 0.043627 0.090 Uiso 1 1 calc R . . . .
C29 C 0.2865(2) 0.6539(2) 0.5996(5) 0.0748(11) Uani 1 1 d . . . . .
C33 C -0.01741(17) 0.57935(17) 0.3819(5) 0.0668(10) Uani 1 1 d . . . . .
H33A H 0.002108 0.610097 0.440137 0.100 Uiso 1 1 calc GR . . . .
H33B H -0.046652 0.561769 0.449838 0.100 Uiso 1 1 calc GR . . . .
H33C H -0.035769 0.595381 0.287410 0.100 Uiso 1 1 calc GR . . . .
C17 C 0.2634(5) 0.3338(4) 0.4682(18) 0.059(2) Uani 0.63(2) 1 d . U P A 1
H17 H 0.283133 0.299729 0.497538 0.070 Uiso 0.63(2) 1 calc R . P A 1
C18 C 0.2253(5) 0.3601(5) 0.5757(15) 0.059(2) Uani 0.63(2) 1 d . U P A 1
H18 H 0.219470 0.343835 0.677393 0.070 Uiso 0.63(2) 1 calc R . P A 1
C16 C 0.2724(3) 0.3582(3) 0.3165(15) 0.0506(19) Uani 0.63(2) 1 d . U P A 1
H16 H 0.297216 0.339992 0.242658 0.061 Uiso 0.63(2) 1 calc R . P A 1
C23 C 0.2673(4) 0.4783(7) -0.1380(11) 0.065(3) Uani 0.63(2) 1 d . U P A 1
H23 H 0.286618 0.473863 -0.236076 0.078 Uiso 0.63(2) 1 calc R . P A 1
C22 C 0.2309(4) 0.5261(6) -0.1167(11) 0.063(2) Uani 0.63(2) 1 d . U P A 1
H22 H 0.226269 0.553205 -0.199591 0.075 Uiso 0.63(2) 1 calc R . P A 1
C21A C 0.2099(11) 0.5137(11) 0.021(3) 0.064(5) Uani 0.37(2) 1 d . U P A 2
H21A H 0.186432 0.546786 0.009432 0.077 Uiso 0.37(2) 1 calc R . P A 2
C22A C 0.2429(10) 0.4970(13) -0.111(2) 0.074(5) Uani 0.37(2) 1 d . U P A 2
H22A H 0.242894 0.519724 -0.203922 0.088 Uiso 0.37(2) 1 calc R . P A 2
C23A C 0.2762(8) 0.4462(15) -0.103(4) 0.082(6) Uani 0.37(2) 1 d . U P A 2
H23A H 0.297166 0.433783 -0.193357 0.099 Uiso 0.37(2) 1 calc R . P A 2
C24A C 0.2780(7) 0.4134(11) 0.041(3) 0.075(5) Uani 0.37(2) 1 d . U P A 2
H24A H 0.302567 0.380920 0.047911 0.090 Uiso 0.37(2) 1 calc R . P A 2
C14A C 0.2441(8) 0.4287(8) 0.171(3) 0.051(5) Uani 0.37(2) 1 d . U P A 2
C15A C 0.2349(9) 0.4017(9) 0.328(3) 0.053(5) Uani 0.37(2) 1 d . U P A 2
C16A C 0.2603(10) 0.3507(7) 0.405(4) 0.072(6) Uani 0.37(2) 1 d . U P A 2
H16A H 0.288138 0.327773 0.352266 0.086 Uiso 0.37(2) 1 calc R . P A 2
C17A C 0.2422(12) 0.3377(7) 0.555(4) 0.077(6) Uani 0.37(2) 1 d . U P A 2
H17A H 0.257593 0.304610 0.605367 0.093 Uiso 0.37(2) 1 calc R . P A 2
C18A C 0.2041(11) 0.3690(7) 0.633(3) 0.071(5) Uani 0.37(2) 1 d . U P A 2
H18A H 0.191746 0.356573 0.734736 0.086 Uiso 0.37(2) 1 calc R . P A 2
C19A C 0.1816(11) 0.4197(8) 0.572(2) 0.052(4) Uani 0.37(2) 1 d . U P A 2
H19A H 0.155893 0.443345 0.629607 0.062 Uiso 0.37(2) 1 calc R . 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
N12 C1 1.373(4) . ?
N12 C11 1.400(5) . ?
N12 C33 1.435(4) . ?
F30 C29 1.335(5) . ?
F31 C29 1.319(5) . ?
C9 C8 1.516(4) . ?
C9 C1 1.378(4) . ?
C9 C10 1.403(4) . ?
C8 C7 1.533(4) . ?
C8 C20 1.528(4) . ?
C8 C13 1.525(4) . ?
C7 C2 1.409(4) . ?
C7 C6 1.382(5) . ?
C1 C2 1.453(4) . ?
C2 C3 1.390(4) . ?
C10 C11 1.468(5) . ?
C10 C28 1.381(5) . ?
C20 C15 1.486(11) . ?
C20 C19 1.276(12) . ?
C20 C15A 1.21(2) . ?
C20 C19A 1.58(2) . ?
C13 C14 1.317(12) . ?
C13 C21 1.448(11) . ?
C13 C21A 1.21(3) . ?
C13 C14A 1.60(2) . ?
C3 H3 0.9300 . ?
C3 C4 1.389(6) . ?
F32 C29 1.327(6) . ?
C11 C25 1.374(5) . ?
C6 H6 0.9300 . ?
C6 C5 1.377(5) . ?
C15 C14 1.458(10) . ?
C15 C16 1.392(11) . ?
C14 C24 1.420(12) . ?
C27 H27 0.9300 . ?
C27 C28 1.419(5) . ?
C27 C26 1.412(6) . ?
C28 H28 0.9300 . ?
C5 C4 1.353(6) . ?
C5 C29 1.500(6) . ?
C4 H4 0.9300 . ?
C19 H19 0.9300 . ?
C19 C18 1.397(14) . ?
C21 H21 0.9300 . ?
C21 C22 1.392(12) . ?
C25 H25 0.9300 . ?
C25 C26 1.394(6) . ?
C24 H24 0.9300 . ?
C24 C23 1.379(14) . ?
C26 H26 0.9300 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C17 H17 0.9300 . ?
C17 C18 1.382(14) . ?
C17 C16 1.389(13) . ?
C18 H18 0.9300 . ?
C16 H16 0.9300 . ?
C23 H23 0.9300 . ?
C23 C22 1.380(13) . ?
C22 H22 0.9300 . ?
C21A H21A 0.9300 . ?
C21A C22A 1.38(2) . ?
C22A H22A 0.9300 . ?
C22A C23A 1.39(3) . ?
C23A H23A 0.9300 . ?
C23A C24A 1.41(3) . ?
C24A H24A 0.9300 . ?
C24A C14A 1.37(2) . ?
C14A C15A 1.46(2) . ?
C15A C16A 1.45(2) . ?
C16A H16A 0.9300 . ?
C16A C17A 1.34(3) . ?
C17A H17A 0.9300 . ?
C17A C18A 1.30(3) . ?
C18A H18A 0.9300 . ?
C18A C19A 1.36(2) . ?
C19A H19A 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N12 C11 106.6(2) . . ?
C1 N12 C33 127.9(3) . . ?
C11 N12 C33 125.3(3) . . ?
C1 C9 C8 111.1(3) . . ?
C1 C9 C10 108.8(3) . . ?
C10 C9 C8 139.9(3) . . ?
C9 C8 C7 100.4(2) . . ?
C9 C8 C20 114.5(2) . . ?
C9 C8 C13 111.8(2) . . ?
C20 C8 C7 115.0(2) . . ?
C13 C8 C7 114.7(2) . . ?
C13 C8 C20 101.1(2) . . ?
C2 C7 C8 111.4(3) . . ?
C6 C7 C8 128.3(3) . . ?
C6 C7 C2 120.3(3) . . ?
N12 C1 C9 111.3(3) . . ?
N12 C1 C2 138.2(3) . . ?
C9 C1 C2 110.4(3) . . ?
C7 C2 C1 106.8(2) . . ?
C3 C2 C7 118.7(3) . . ?
C3 C2 C1 134.5(3) . . ?
C9 C10 C11 104.7(3) . . ?
C28 C10 C9 137.5(3) . . ?
C28 C10 C11 117.8(3) . . ?
C8 C20 C19A 118.9(7) . . ?
C15 C20 C8 105.7(5) . . ?
C19 C20 C8 134.6(6) . . ?
C19 C20 C15 119.7(6) . . ?
C15A C20 C8 123.7(12) . . ?
C15A C20 C19A 117.2(12) . . ?
C8 C13 C14A 99.5(10) . . ?
C14 C13 C8 116.1(5) . . ?
C14 C13 C21 120.6(6) . . ?
C21 C13 C8 123.3(5) . . ?
C21A C13 C8 141.5(12) . . ?
C21A C13 C14A 118.3(12) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 C2 119.2(3) . . ?
C4 C3 H3 120.4 . . ?
N12 C11 C10 108.6(3) . . ?
C25 C11 N12 129.5(3) . . ?
C25 C11 C10 121.8(3) . . ?
C7 C6 H6 120.0 . . ?
C5 C6 C7 119.9(3) . . ?
C5 C6 H6 120.0 . . ?
C14 C15 C20 110.5(8) . . ?
C16 C15 C20 118.3(7) . . ?
C16 C15 C14 131.2(10) . . ?
C13 C14 C15 106.6(8) . . ?
C13 C14 C24 122.2(8) . . ?
C24 C14 C15 131.0(10) . . ?
C28 C27 H27 120.3 . . ?
C26 C27 H27 120.3 . . ?
C26 C27 C28 119.4(4) . . ?
C10 C28 C27 120.7(3) . . ?
C10 C28 H28 119.6 . . ?
C27 C28 H28 119.6 . . ?
C6 C5 C29 118.1(4) . . ?
C4 C5 C6 120.1(4) . . ?
C4 C5 C29 121.8(4) . . ?
C3 C4 H4 119.1 . . ?
C5 C4 C3 121.7(4) . . ?
C5 C4 H4 119.1 . . ?
C20 C19 H19 118.8 . . ?
C20 C19 C18 122.4(8) . . ?
C18 C19 H19 118.8 . . ?
C13 C21 H21 121.3 . . ?
C22 C21 C13 117.4(7) . . ?
C22 C21 H21 121.3 . . ?
C11 C25 H25 120.6 . . ?
C11 C25 C26 118.8(4) . . ?
C26 C25 H25 120.6 . . ?
C14 C24 H24 121.5 . . ?
C23 C24 C14 117.1(9) . . ?
C23 C24 H24 121.5 . . ?
C27 C26 H26 119.3 . . ?
C25 C26 C27 121.4(4) . . ?
C25 C26 H26 119.3 . . ?
F30 C29 C5 112.6(4) . . ?
F31 C29 F30 106.0(4) . . ?
F31 C29 F32 106.8(4) . . ?
F31 C29 C5 112.9(4) . . ?
F32 C29 F30 104.3(4) . . ?
F32 C29 C5 113.5(4) . . ?
N12 C33 H33A 109.5 . . ?
N12 C33 H33B 109.5 . . ?
N12 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C18 C17 H17 119.9 . . ?
C18 C17 C16 120.1(8) . . ?
C16 C17 H17 119.9 . . ?
C19 C18 H18 119.9 . . ?
C17 C18 C19 120.1(9) . . ?
C17 C18 H18 119.9 . . ?
C15 C16 H16 120.3 . . ?
C17 C16 C15 119.3(8) . . ?
C17 C16 H16 120.3 . . ?
C24 C23 H23 118.9 . . ?
C24 C23 C22 122.3(8) . . ?
C22 C23 H23 118.9 . . ?
C21 C22 H22 119.9 . . ?
C23 C22 C21 120.1(7) . . ?
C23 C22 H22 119.9 . . ?
C13 C21A H21A 117.0 . . ?
C13 C21A C22A 125.9(19) . . ?
C22A C21A H21A 117.0 . . ?
C21A C22A H22A 120.2 . . ?
C21A C22A C23A 119.7(18) . . ?
C23A C22A H22A 120.2 . . ?
C22A C23A H23A 120.1 . . ?
C22A C23A C24A 119.8(16) . . ?
C24A C23A H23A 120.1 . . ?
C23A C24A H24A 119.6 . . ?
C14A C24A C23A 120.8(17) . . ?
C14A C24A H24A 119.6 . . ?
C24A C14A C13 115.1(18) . . ?
C24A C14A C15A 132.5(17) . . ?
C15A C14A C13 112.3(14) . . ?
C20 C15A C14A 103.0(14) . . ?
C20 C15A C16A 124(2) . . ?
C16A C15A C14A 132.4(19) . . ?
C15A C16A H16A 121.3 . . ?
C17A C16A C15A 117.4(17) . . ?
C17A C16A H16A 121.3 . . ?
C16A C17A H17A 118.5 . . ?
C18A C17A C16A 123.1(15) . . ?
C18A C17A H17A 118.5 . . ?
C17A C18A H18A 119.0 . . ?
C17A C18A C19A 122.1(17) . . ?
C19A C18A H18A 119.0 . . ?
C20 C19A H19A 122.2 . . ?
C18A C19A C20 115.5(14) . . ?
C18A C19A H19A 122.2 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.728
_oxdiff_exptl_absorpt_empirical_full_min 0.590
####################################################################### 
# 
# 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_210114_1
_database_code_depnum_ccdc_archive 'CCDC 2305241'
loop_
_audit_author_name
_audit_author_address
'Koji Hirano'
;Osaka University
Japan
;
_audit_update_record             
;
2023-11-02 deposited with the CCDC.	2024-01-02 downloaded from the CCDC.
;
_audit_creation_date             2021-01-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C38 H39 N'
_chemical_formula_sum            'C38 H39 N'
_chemical_formula_weight         509.70
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C56 H34 N2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           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                   10.9754(2)
_cell_length_b                   12.1150(4)
_cell_length_c                   12.3347(3)
_cell_angle_alpha                116.431(3)
_cell_angle_beta                 95.048(2)
_cell_angle_gamma                94.470(2)
_cell_volume                     1450.31(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8423
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      74.0890
_cell_measurement_theta_min      4.0260
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.498
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63235
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.43a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             548
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 -3 8 0.0469
2 3 -8 0.0369
0 6 2 0.0283
0 -7 0 0.0019
0 4 -8 0.0148
0 -4 8 0.0371
5 -1 4 0.1233
-3 3 -7 0.0516

_exptl_crystal_size_max          0.371
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.033
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.5980 -3.3338 8.0042 -0.1482 -0.0114 -0.9889
1.6257 3.0457 -7.9190 0.2912 0.0227 0.9564
0.1819 6.1254 1.5499 -0.0254 -0.9785 -0.2048
-0.0940 -6.9692 0.0022 0.0260 0.9996 0.0089
-0.3998 3.5631 -7.9234 0.0080 -0.0026 1.0000
0.0601 -3.6427 7.9689 -0.0550 0.0193 -0.9983
5.3633 -1.0909 4.4007 0.7024 -0.2487 -0.6669
-2.8115 2.7217 -6.9966 -0.3310 0.1173 0.9363

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20471
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.274
_diffrn_reflns_theta_min         4.041
_diffrn_ambient_temperature      223(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     43.00 121.00   0.50    0.73    --   42.80  35.00 -20.00  156
  2  ω    101.00 127.00   0.50    2.92    --   76.50  35.00 -20.00   52
  3  ω     70.00  96.00   0.50    2.92    --   76.50  35.00 -20.00   52
  4  ω     98.00 124.00   0.50    2.92    --   76.50 125.00-150.00   52
  5  ω     85.00 117.00   0.50    0.73    --   42.80 125.00-180.00   64
  6  ω     25.00  50.00   0.50    2.92    --   76.50 -35.00-177.00   50
  7  ω    -32.00  59.00   0.50    0.73    --   42.80 -35.00-177.00  182
  8  ω    -15.00  21.00   0.50    0.73    --  -42.80  35.00 -20.00   72
  9  ω    -62.00 -28.00   0.50    2.92    -- -106.00  35.00 -20.00   68
 10  ω    -77.00 -51.00   0.50    2.92    -- -106.00  57.00 -90.00   52
 11  ω    -98.00 -69.00   0.50    2.92    -- -106.00  37.00-180.00   58
 12  ω    -74.00 -33.00   0.50    2.92    -- -106.00  57.00-180.00   82
 13  ω    -67.00 -41.00   0.50    2.92    -- -106.00 125.00 -90.00   52
 14  ω    -69.00 -34.00   0.50    2.92    -- -106.00 125.00 -30.00   70
 15  ω    -59.00 -32.00   0.50    2.92    -- -106.00 125.00  60.00   54
 16  ω    -96.00 -59.00   0.50    0.73    --  -42.80 125.00 150.00   74
 17  ω   -127.00 -68.00   0.50    2.92    -- -106.00  57.00  90.00  118
 18  ω    -84.00 -29.00   0.50    2.92    -- -106.00  19.00 120.00  110
 19  ω   -111.00 -32.00   0.50    2.92    -- -106.00 125.00 150.00  158
 20  ω   -114.00 -35.00   0.50    2.92    -- -106.00 125.00  30.00  158
 21  ω   -117.00 -75.00   0.50    2.92    -- -106.00 125.00 -90.00   84
 22  ω   -115.00 -63.00   0.50    2.92    -- -106.00 125.00-120.00  104
 23  ω   -105.00 -50.00   0.50    2.92    -- -106.00  77.00 -90.00  110
 24  ω   -119.00 -93.00   0.50    2.92    -- -106.00  35.00 -20.00   52
 25  ω   -113.00 -32.00   0.50    2.92    -- -106.00  77.00  30.00  162
 26  ω   -108.00 -83.00   0.50    2.92    -- -106.00 125.00  90.00   50
 27  ω   -108.00 -65.00   0.50    2.92    -- -106.00 125.00  60.00   86
 28  ω   -117.00 -61.00   0.50    2.92    -- -106.00 125.00   0.00  112
 29  ω   -118.00 -81.00   0.50    2.92    -- -106.00  57.00 -90.00   74
 30  ω   -114.00 -35.00   0.50    2.92    -- -106.00 125.00-180.00  158
 31  ω   -113.00 -88.00   0.50    2.92    -- -106.00  57.00-180.00   50
 32  ω   -120.00 -63.00   0.50    0.73    --  -42.80 -35.00-177.00  114
 33  ω      2.00 102.00   0.50    2.92    --   76.50 -77.00  30.00  200
 34  ω    -44.00 -19.00   0.50    0.73    --  -42.80 -35.00-177.00   50
 35  ω   -115.00 -71.00   0.50    0.73    --  -42.80-125.00-180.00   88
 36  ω   -152.00 -95.00   0.50    2.92    -- -106.00 -35.00-177.00  114
 37  ω   -155.00-130.00   0.50    2.92    -- -106.00 -37.00-120.00   50
 38  ω   -177.00 -75.00   0.50    2.92    -- -106.00 -19.00-120.00  204
 39  ω   -136.00 -83.00   0.50    2.92    -- -106.00-125.00  30.00  106
 40  ω   -101.00 -75.00   0.50    0.73    --  -42.80-125.00 120.00   52
 41  ω   -171.00-144.00   0.50    2.92    -- -106.00-125.00  30.00   54
 42  ω   -174.00 -85.00   0.50    2.92    -- -106.00 -99.00   0.00  178
 43  ω   -172.00-112.00   0.50    2.92    -- -106.00 -37.00 120.00  120
 44  ω   -134.00-109.00   0.50    2.92    -- -106.00  19.00 120.00   50
 45  ω   -176.00-149.00   0.50    2.92    -- -106.00 -99.00 150.00   54
 46  ω   -177.00-111.00   0.50    2.92    -- -106.00 -57.00-150.00  132
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1384506000
_diffrn_orient_matrix_UB_12      -0.0055991000
_diffrn_orient_matrix_UB_13      -0.0105080000
_diffrn_orient_matrix_UB_21      -0.0239376000
_diffrn_orient_matrix_UB_22      -0.1431321000
_diffrn_orient_matrix_UB_23      -0.0628264000
_diffrn_orient_matrix_UB_31      -0.0215111000
_diffrn_orient_matrix_UB_32      -0.0010266000
_diffrn_orient_matrix_UB_33      -0.1255808000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4776
_reflns_number_total             5815
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         5815
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0723
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1129P)²+0.4895P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2040
_refine_ls_wR_factor_ref         0.2161
_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. Others
 Fixed Sof: C21(0.5) H21A(0.5) H21B(0.5) C29(0.5) H29A(0.5) H29B(0.5)
 C9AA(0.5) H9AA(0.5) H9AB(0.5) C5AA(0.5) H5AA(0.5) H5AB(0.5) C2AA(0.5)
 H2AA(0.5) H2AB(0.5) C4AA(0.5) H4AA(0.5) H4AB(0.5) C1AA(0.5) H1AA(0.5)
 H1AB(0.5) C7AA(0.5) H7AA(0.5) H7AB(0.5) C6AA(0.5) H6AA(0.5) H6AB(0.5)
 C8AA(0.5) H8AA(0.5) H8AB(0.5) C0BA(0.5) H0BA(0.5) H0BB(0.5) C2BA(0.5)
 H2BA(0.5) H2BB(0.5) H2BC(0.5) C4BA(0.5) H4BA(0.5) H4BB(0.5) C7BA(0.5)
 H7BA(0.5) H7BB(0.5) C6BA(0.5) H6BA(0.5) H6BB(0.5) C8BA(0.5) H8BA(0.5)
 H8BB(0.5) H8BC(0.5) C5BA(0.5) H5BA(0.5) H5BB(0.5) C1CA(0.5) H1CA(0.5)
 H1CB(0.5) C0CA(0.5) H0CA(0.5) H0CB(0.5) C9BA(0.5) H9BA(0.5) H9BB(0.5)
 C2CA(0.5) H2CA(0.5) H2CB(0.5) C3CA(0.5) H3CA(0.5) H3CB(0.5) C4CA(0.5)
 H4CA(0.5) H4CB(0.5) C5CA(0.5) H5CA(0.5) H5CB(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C29(H29A,H29B), C9AA(H9AA,H9AB), C5AA(H5AA,H5AB), C2AA(H2AA,
 H2AB), C4AA(H4AA,H4AB), C1AA(H1AA,H1AB), C7AA(H7AA,H7AB), C6AA(H6AA,H6AB),
 C8AA(H8AA,H8AB), C0BA(H0BA,H0BB), C4BA(H4BA,H4BB), C7BA(H7BA,H7BB), C6BA(H6BA,
 H6BB), C5BA(H5BA,H5BB), C1CA(H1CA,H1CB), C0CA(H0CA,H0CB), C9BA(H9BA,H9BB),
 C2CA(H2CA,H2CB), C3CA(H3CA,H3CB), C4CA(H4CA,H4CB), C5CA(H5CA,H5CB)
3.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C24(H24), C25(H25), C5(H5), C28(H28), C8(H8), C26(H26), C27(H27),
 C7(H7), C6(H6), C0AA(H0AA), C3AA(H3AA), C3BA(H3BA), C1BA(H1BA)
3.c Idealised Me refined as rotating group:
 C2BA(H2BA,H2BB,H2BC), C8BA(H8BA,H8BB,H8BC)
;
_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
N18 N 1.00008(15) 0.3709(2) 0.34635(16) 0.0660(6) Uani 1 1 d . . . . .
C13 C 1.08402(14) 0.47941(17) 0.12652(15) 0.0409(4) Uani 1 1 d . . . . .
C23 C 0.84054(14) 0.44911(19) 0.01942(16) 0.0446(4) Uani 1 1 d . . . . .
H23 H 0.759448 0.438979 -0.016013 0.054 Uiso 1 1 calc R . . . .
C2 C 1.30387(15) 0.41277(18) 0.12793(15) 0.0420(4) Uani 1 1 d . . . . .
C1 C 1.20882(14) 0.48933(18) 0.20105(15) 0.0423(4) Uani 1 1 d . . . . .
C22 C 1.06283(14) 0.50792(17) 0.02771(14) 0.0393(4) Uani 1 1 d . . . . .
C4 C 1.40188(15) 0.61640(19) 0.23385(16) 0.0455(4) Uani 1 1 d . . . . .
C9 C 1.28140(16) 0.61934(19) 0.26400(15) 0.0453(4) Uani 1 1 d . . . . .
C3 C 1.41604(15) 0.48826(19) 0.15159(16) 0.0440(4) Uani 1 1 d . . . . .
C12 C 0.98636(15) 0.43721(19) 0.16929(16) 0.0455(4) Uani 1 1 d . . . . .
C24 C 0.86333(15) 0.4224(2) 0.11469(16) 0.0481(5) Uani 1 1 d . . . . .
H24 H 0.798473 0.394657 0.143858 0.058 Uiso 1 1 calc R . . . .
C10 C 1.16510(16) 0.4437(2) 0.28904(16) 0.0500(5) Uani 1 1 d . . . . .
C11 C 1.04017(16) 0.4154(2) 0.26890(17) 0.0520(5) Uani 1 1 d . . . . .
C25 C 1.51782(17) 0.4370(2) 0.09915(19) 0.0556(5) Uani 1 1 d . . . . .
H25 H 1.592537 0.486859 0.115104 0.067 Uiso 1 1 calc R . . . .
C5 C 1.4841(2) 0.7261(2) 0.2807(2) 0.0611(6) Uani 1 1 d . . . . .
H5 H 1.563809 0.724932 0.260528 0.073 Uiso 1 1 calc R . . . .
C28 C 1.29270(19) 0.2874(2) 0.05284(19) 0.0566(5) Uani 1 1 d . . . . .
H28 H 1.218403 0.237094 0.037409 0.068 Uiso 1 1 calc R . . . .
C8 C 1.2437(2) 0.7301(2) 0.34145(19) 0.0649(6) Uani 1 1 d . . . . .
H8 H 1.164217 0.732257 0.362406 0.078 Uiso 1 1 calc R . . . .
C26 C 1.5064(2) 0.3117(3) 0.0235(2) 0.0661(6) Uani 1 1 d . . . . .
H26 H 1.573797 0.276444 -0.012422 0.079 Uiso 1 1 calc R . . . .
C14 C 1.21124(18) 0.4174(3) 0.38488(19) 0.0620(6) Uani 1 1 d . . . . .
C27 C 1.3954(2) 0.2369(2) 0.0000(2) 0.0692(6) Uani 1 1 d . . . . .
H27 H 1.389206 0.152120 -0.051625 0.083 Uiso 1 1 calc R . . . .
C7 C 1.3269(3) 0.8390(3) 0.3879(2) 0.0822(8) Uani 1 1 d . . . . .
H7 H 1.302427 0.914336 0.439962 0.099 Uiso 1 1 calc R . . . .
C6 C 1.4447(3) 0.8361(2) 0.3576(2) 0.0773(7) Uani 1 1 d . . . . .
H6 H 1.498607 0.909697 0.389459 0.093 Uiso 1 1 calc R . . . .
C19 C 1.10483(19) 0.3712(3) 0.4189(2) 0.0742(8) Uani 1 1 d . . . . .
C21 C 0.8750(6) 0.3127(6) 0.3434(6) 0.0481(14) Uani 0.5 1 d . . P A 1
H21A H 0.817442 0.369753 0.344082 0.058 Uiso 0.5 1 calc R . P A 1
H21B H 0.873886 0.306481 0.419052 0.058 Uiso 0.5 1 calc R . P A 1
C29 C 0.4056(9) 0.0665(10) 0.2053(8) 0.088(2) Uani 0.5 1 d . . P A 1
H29A H 0.447316 -0.006905 0.172629 0.105 Uiso 0.5 1 calc R . P A 1
H29B H 0.408053 0.101003 0.147960 0.105 Uiso 0.5 1 calc R . P A 1
C9AA C 0.2412(9) 0.0090(9) 0.1941(9) 0.091(2) Uani 0.5 1 d . . P A 1
H9AA H 0.229059 0.027767 0.277225 0.110 Uiso 0.5 1 calc R . P A 1
H9AB H 0.195473 0.064294 0.174120 0.110 Uiso 0.5 1 calc R . P A 1
C5AA C 0.8249(6) 0.1863(6) 0.2397(7) 0.0778(18) Uani 0.5 1 d . . P A 1
H5AA H 0.853530 0.121728 0.257763 0.093 Uiso 0.5 1 calc R . P A 1
H5AB H 0.854349 0.177923 0.164898 0.093 Uiso 0.5 1 calc R . P A 1
C2AA C 0.5884(5) 0.1274(6) 0.2326(5) 0.0803(15) Uani 0.5 1 d . . P A 2
H2AA H 0.619013 0.064034 0.251449 0.096 Uiso 0.5 1 calc R . P A 2
H2AB H 0.596199 0.104395 0.147747 0.096 Uiso 0.5 1 calc R . P A 2
C4AA C 0.6635(5) 0.2453(5) 0.3093(5) 0.0705(12) Uani 0.5 1 d . . P A 2
H4AA H 0.657002 0.267448 0.394282 0.085 Uiso 0.5 1 calc R . P A 2
H4AB H 0.631717 0.309003 0.291748 0.085 Uiso 0.5 1 calc R . P A 2
C1AA C 0.4534(7) 0.1307(11) 0.2493(7) 0.100(3) Uani 0.5 1 d . . P A 2
H1AA H 0.424037 0.196692 0.234163 0.120 Uiso 0.5 1 calc R . P A 2
H1AB H 0.445533 0.150358 0.333506 0.120 Uiso 0.5 1 calc R . P A 2
C7AA C 0.0132(7) -0.0820(8) 0.2653(7) 0.100(2) Uani 0.5 1 d . . P A 1
H7AA H 0.066475 -0.118755 0.303525 0.119 Uiso 0.5 1 calc R . P A 1
H7AB H 0.033074 0.007572 0.311251 0.119 Uiso 0.5 1 calc R . P A 1
C6AA C 0.0425(8) -0.1232(9) 0.1313(7) 0.106(2) Uani 0.5 1 d . . P A 1
H6AA H 0.006035 -0.208864 0.080916 0.127 Uiso 0.5 1 calc R . P A 1
H6AB H 0.003137 -0.072678 0.099459 0.127 Uiso 0.5 1 calc R . P A 1
C8AA C -0.1195(9) -0.1178(8) 0.2746(11) 0.125(4) Uani 0.5 1 d . . P A 1
H8AA H -0.173129 -0.085184 0.232214 0.151 Uiso 0.5 1 calc R . P A 1
H8AB H -0.137978 -0.207692 0.232809 0.151 Uiso 0.5 1 calc R . P A 1
C0BA C 0.1737(8) -0.1132(7) 0.1197(7) 0.106(2) Uani 0.5 1 d . . P A 1
H0BA H 0.210940 -0.171961 0.141338 0.127 Uiso 0.5 1 calc R . P A 1
H0BB H 0.182084 -0.137062 0.034762 0.127 Uiso 0.5 1 calc R . P A 1
C2BA C -0.1464(8) -0.0759(7) 0.3919(9) 0.122(3) Uani 0.5 1 d . . P A 1
H2BA H -0.087222 -0.098653 0.437911 0.183 Uiso 0.5 1 calc GR . P A 1
H2BB H -0.227602 -0.112648 0.390438 0.183 Uiso 0.5 1 calc GR . P A 1
H2BC H -0.143056 0.012975 0.429531 0.183 Uiso 0.5 1 calc GR . P A 1
C0AA C 1.3277(2) 0.4293(3) 0.4490(2) 0.0752(8) Uani 1 1 d . . . . .
H0AA H 1.398402 0.458776 0.428514 0.090 Uiso 1 1 calc R . . . .
C3AA C 1.3356(2) 0.3967(4) 0.5426(3) 0.1021(12) Uani 1 1 d . . . . .
H3AA H 1.412479 0.404701 0.585596 0.123 Uiso 1 1 calc R . . . .
C3BA C 1.1142(2) 0.3374(4) 0.5129(3) 0.1030(12) Uani 1 1 d . . . . .
H3BA H 1.044830 0.306161 0.533698 0.124 Uiso 1 1 calc R . . . .
C1BA C 1.2305(3) 0.3518(4) 0.5743(3) 0.1159(14) Uani 1 1 d . . . . .
H1BA H 1.238991 0.330995 0.638436 0.139 Uiso 1 1 calc R . . . .
C4BA C 0.1870(8) -0.0137(10) 0.1059(8) 0.120(3) Uani 0.5 1 d . . P A 2
H4BA H 0.203627 -0.097124 0.087944 0.144 Uiso 0.5 1 calc R . P A 2
H4BB H 0.211518 0.001926 0.039785 0.144 Uiso 0.5 1 calc R . P A 2
C7BA C -0.0017(8) -0.1547(9) 0.1864(10) 0.106(2) Uani 0.5 1 d . . P A 2
H7BA H 0.082510 -0.157385 0.215587 0.127 Uiso 0.5 1 calc R . P A 2
H7BB H -0.020195 -0.217565 0.101871 0.127 Uiso 0.5 1 calc R . P A 2
C6BA C -0.0100(8) -0.0357(8) 0.1916(9) 0.115(2) Uani 0.5 1 d . . P A 2
H6BA H 0.025281 0.027856 0.272580 0.138 Uiso 0.5 1 calc R . P A 2
H6BB H -0.096468 -0.026309 0.179827 0.138 Uiso 0.5 1 calc R . P A 2
C8BA C -0.0862(8) -0.1860(10) 0.2597(9) 0.116(3) Uani 0.5 1 d . . P A 2
H8BA H -0.074399 -0.266026 0.253845 0.173 Uiso 0.5 1 calc GR . P A 2
H8BB H -0.170152 -0.187710 0.228910 0.173 Uiso 0.5 1 calc GR . P A 2
H8BC H -0.068613 -0.124283 0.343707 0.173 Uiso 0.5 1 calc GR . P A 2
C5BA C 0.0526(9) -0.0142(12) 0.1005(10) 0.152(4) Uani 0.5 1 d . . P A 2
H5BA H 0.015283 -0.077530 0.020137 0.183 Uiso 0.5 1 calc R . P A 2
H5BB H 0.034473 0.065225 0.106387 0.183 Uiso 0.5 1 calc R . P A 2
C1CA C 0.6760(6) 0.1708(6) 0.2220(6) 0.0949(19) Uani 0.5 1 d . . P A 1
H1CA H 0.647283 0.244554 0.222161 0.114 Uiso 0.5 1 calc R . P A 1
H1CB H 0.643117 0.099914 0.144542 0.114 Uiso 0.5 1 calc R . P A 1
C0CA C 0.6358(9) 0.1531(8) 0.3186(7) 0.116(3) Uani 0.5 1 d . . P A 1
H0CA H 0.678793 0.217688 0.395669 0.139 Uiso 0.5 1 calc R . P A 1
H0CB H 0.655097 0.073482 0.311337 0.139 Uiso 0.5 1 calc R . P A 1
C9BA C 0.4855(7) 0.1568(9) 0.3172(9) 0.098(2) Uani 0.5 1 d . . P A 1
H9BA H 0.461491 0.143990 0.385040 0.117 Uiso 0.5 1 calc R . P A 1
H9BB H 0.469184 0.239576 0.332150 0.117 Uiso 0.5 1 calc R . P A 1
C2CA C 0.8020(5) 0.2432(7) 0.2905(6) 0.0659(12) Uani 0.5 1 d . . P A 2
H2CA H 0.835778 0.181497 0.309936 0.079 Uiso 0.5 1 calc R . P A 2
H2CB H 0.810071 0.221656 0.205927 0.079 Uiso 0.5 1 calc R . P A 2
C3CA C 0.8701(7) 0.3693(6) 0.3727(7) 0.0519(15) Uani 0.5 1 d . . P A 2
H3CA H 0.831481 0.431873 0.358329 0.062 Uiso 0.5 1 calc R . P A 2
H3CB H 0.868361 0.387665 0.457452 0.062 Uiso 0.5 1 calc R . P A 2
C4CA C 0.2674(9) 0.0708(9) 0.2152(10) 0.094(3) Uani 0.5 1 d . . P A 2
H4CA H 0.248259 0.064352 0.287648 0.113 Uiso 0.5 1 calc R . P A 2
H4CB H 0.273923 0.156524 0.229152 0.113 Uiso 0.5 1 calc R . P A 2
C5CA C 0.3720(11) 0.0090(10) 0.1654(10) 0.101(3) Uani 0.5 1 d . . P A 2
H5CA H 0.371902 -0.015682 0.079035 0.122 Uiso 0.5 1 calc R . P A 2
H5CB H 0.386202 -0.059117 0.184083 0.122 Uiso 0.5 1 calc R . 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
N18 C11 1.376(2) . ?
N18 C19 1.392(3) . ?
N18 C21 1.484(7) . ?
N18 C3CA 1.491(7) . ?
C13 C1 1.546(2) . ?
C13 C22 1.413(2) . ?
C13 C12 1.394(2) . ?
C23 H23 0.9300 . ?
C23 C22 1.423(2) 2_765 ?
C23 C24 1.359(2) . ?
C2 C1 1.528(2) . ?
C2 C3 1.400(2) . ?
C2 C28 1.370(3) . ?
C1 C9 1.525(3) . ?
C1 C10 1.516(2) . ?
C22 C22 1.443(3) 2_765 ?
C4 C9 1.404(2) . ?
C4 C3 1.458(3) . ?
C4 C5 1.397(3) . ?
C9 C8 1.378(3) . ?
C3 C25 1.389(3) . ?
C12 C24 1.416(2) . ?
C12 C11 1.454(2) . ?
C24 H24 0.9300 . ?
C10 C11 1.360(2) . ?
C10 C14 1.418(3) . ?
C25 H25 0.9300 . ?
C25 C26 1.371(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.378(4) . ?
C28 H28 0.9300 . ?
C28 C27 1.397(3) . ?
C8 H8 0.9300 . ?
C8 C7 1.397(4) . ?
C26 H26 0.9300 . ?
C26 C27 1.385(4) . ?
C14 C19 1.430(3) . ?
C14 C0AA 1.405(3) . ?
C27 H27 0.9300 . ?
C7 H7 0.9300 . ?
C7 C6 1.375(4) . ?
C6 H6 0.9300 . ?
C19 C3BA 1.390(3) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C5AA 1.512(8) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C9AA 1.853(13) . ?
C29 C9BA 1.471(10) . ?
C9AA H9AA 0.9700 . ?
C9AA H9AB 0.9700 . ?
C9AA C0BA 1.443(12) . ?
C5AA H5AA 0.9700 . ?
C5AA H5AB 0.9700 . ?
C5AA C1CA 1.614(9) . ?
C2AA H2AA 0.9700 . ?
C2AA H2AB 0.9700 . ?
C2AA C4AA 1.446(8) . ?
C2AA C1AA 1.515(9) . ?
C4AA H4AA 0.9700 . ?
C4AA H4AB 0.9700 . ?
C4AA C2CA 1.558(7) . ?
C1AA H1AA 0.9700 . ?
C1AA H1AB 0.9700 . ?
C1AA C5CA 1.522(12) . ?
C7AA H7AA 0.9700 . ?
C7AA H7AB 0.9700 . ?
C7AA C6AA 1.571(11) . ?
C7AA C8AA 1.515(13) . ?
C6AA H6AA 0.9700 . ?
C6AA H6AB 0.9700 . ?
C6AA C0BA 1.461(11) . ?
C8AA H8AA 0.9700 . ?
C8AA H8AB 0.9700 . ?
C8AA C2BA 1.373(14) . ?
C0BA H0BA 0.9700 . ?
C0BA H0BB 0.9700 . ?
C2BA H2BA 0.9600 . ?
C2BA H2BB 0.9600 . ?
C2BA H2BC 0.9600 . ?
C0AA H0AA 0.9300 . ?
C0AA C3AA 1.374(3) . ?
C3AA H3AA 0.9300 . ?
C3AA C1BA 1.397(4) . ?
C3BA H3BA 0.9300 . ?
C3BA C1BA 1.382(4) . ?
C1BA H1BA 0.9300 . ?
C4BA H4BA 0.9700 . ?
C4BA H4BB 0.9700 . ?
C4BA C5BA 1.470(12) . ?
C4BA C4CA 1.438(13) . ?
C7BA H7BA 0.9700 . ?
C7BA H7BB 0.9700 . ?
C7BA C6BA 1.425(12) . ?
C7BA C8BA 1.490(12) . ?
C6BA H6BA 0.9700 . ?
C6BA H6BB 0.9700 . ?
C6BA C5BA 1.474(12) . ?
C8BA H8BA 0.9600 . ?
C8BA H8BB 0.9600 . ?
C8BA H8BC 0.9600 . ?
C5BA H5BA 0.9700 . ?
C5BA H5BB 0.9700 . ?
C1CA H1CA 0.9700 . ?
C1CA H1CB 0.9700 . ?
C1CA C0CA 1.402(10) . ?
C0CA H0CA 0.9700 . ?
C0CA H0CB 0.9700 . ?
C0CA C9BA 1.652(11) . ?
C9BA H9BA 0.9700 . ?
C9BA H9BB 0.9700 . ?
C2CA H2CA 0.9700 . ?
C2CA H2CB 0.9700 . ?
C2CA C3CA 1.494(8) . ?
C3CA H3CA 0.9700 . ?
C3CA H3CB 0.9700 . ?
C4CA H4CA 0.9700 . ?
C4CA H4CB 0.9700 . ?
C4CA C5CA 1.451(15) . ?
C5CA H5CA 0.9700 . ?
C5CA H5CB 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
C11 N18 C19 106.57(16) . . ?
C11 N18 C21 128.6(3) . . ?
C11 N18 C3CA 122.6(3) . . ?
C19 N18 C21 124.1(3) . . ?
C19 N18 C3CA 127.4(3) . . ?
C22 C13 C1 127.93(14) . . ?
C12 C13 C1 111.11(14) . . ?
C12 C13 C22 120.96(15) . . ?
C22 C23 H23 119.0 2_765 . ?
C24 C23 H23 119.0 . . ?
C24 C23 C22 121.91(15) . 2_765 ?
C3 C2 C1 110.41(16) . . ?
C28 C2 C1 128.88(17) . . ?
C28 C2 C3 120.64(17) . . ?
C2 C1 C13 115.85(14) . . ?
C9 C1 C13 114.42(15) . . ?
C9 C1 C2 101.29(13) . . ?
C10 C1 C13 100.17(13) . . ?
C10 C1 C2 112.00(15) . . ?
C10 C1 C9 113.73(15) . . ?
C13 C22 C23 123.03(14) . 2_765 ?
C13 C22 C22 118.11(18) . 2_765 ?
C23 C22 C22 118.86(18) 2_765 2_765 ?
C9 C4 C3 108.48(16) . . ?
C5 C4 C9 120.2(2) . . ?
C5 C4 C3 131.28(18) . . ?
C4 C9 C1 110.71(16) . . ?
C8 C9 C1 128.92(18) . . ?
C8 C9 C4 120.4(2) . . ?
C2 C3 C4 109.04(15) . . ?
C25 C3 C2 120.38(19) . . ?
C25 C3 C4 130.59(18) . . ?
C13 C12 C24 120.54(16) . . ?
C13 C12 C11 106.68(14) . . ?
C24 C12 C11 132.77(16) . . ?
C23 C24 C12 119.62(15) . . ?
C23 C24 H24 120.2 . . ?
C12 C24 H24 120.2 . . ?
C11 C10 C1 110.75(15) . . ?
C11 C10 C14 108.15(16) . . ?
C14 C10 C1 141.08(16) . . ?
N18 C11 C12 137.61(16) . . ?
C10 C11 N18 111.08(16) . . ?
C10 C11 C12 111.28(16) . . ?
C3 C25 H25 120.5 . . ?
C26 C25 C3 118.9(2) . . ?
C26 C25 H25 120.5 . . ?
C4 C5 H5 120.7 . . ?
C6 C5 C4 118.6(2) . . ?
C6 C5 H5 120.7 . . ?
C2 C28 H28 120.7 . . ?
C2 C28 C27 118.5(2) . . ?
C27 C28 H28 120.7 . . ?
C9 C8 H8 120.6 . . ?
C9 C8 C7 118.8(2) . . ?
C7 C8 H8 120.6 . . ?
C25 C26 H26 119.6 . . ?
C25 C26 C27 120.7(2) . . ?
C27 C26 H26 119.6 . . ?
C10 C14 C19 105.21(16) . . ?
C0AA C14 C10 135.93(19) . . ?
C0AA C14 C19 118.83(18) . . ?
C28 C27 H27 119.6 . . ?
C26 C27 C28 120.8(2) . . ?
C26 C27 H27 119.6 . . ?
C8 C7 H7 119.6 . . ?
C6 C7 C8 120.8(2) . . ?
C6 C7 H7 119.6 . . ?
C5 C6 H6 119.4 . . ?
C7 C6 C5 121.2(2) . . ?
C7 C6 H6 119.4 . . ?
N18 C19 C14 108.98(17) . . ?
C3BA C19 N18 129.4(2) . . ?
C3BA C19 C14 121.6(2) . . ?
N18 C21 H21A 107.4 . . ?
N18 C21 H21B 107.4 . . ?
N18 C21 C5AA 119.5(5) . . ?
H21A C21 H21B 107.0 . . ?
C5AA C21 H21A 107.4 . . ?
C5AA C21 H21B 107.4 . . ?
H29A C29 H29B 106.2 . . ?
C9AA C29 H29A 105.8 . . ?
C9AA C29 H29B 105.8 . . ?
C9BA C29 H29A 105.8 . . ?
C9BA C29 H29B 105.8 . . ?
C9BA C29 C9AA 126.2(7) . . ?
C29 C9AA H9AA 104.8 . . ?
C29 C9AA H9AB 104.8 . . ?
H9AA C9AA H9AB 105.8 . . ?
C0BA C9AA C29 130.0(8) . . ?
C0BA C9AA H9AA 104.8 . . ?
C0BA C9AA H9AB 104.8 . . ?
C21 C5AA H5AA 109.8 . . ?
C21 C5AA H5AB 109.8 . . ?
C21 C5AA C1CA 109.4(5) . . ?
H5AA C5AA H5AB 108.2 . . ?
C1CA C5AA H5AA 109.8 . . ?
C1CA C5AA H5AB 109.8 . . ?
H2AA C2AA H2AB 107.8 . . ?
C4AA C2AA H2AA 109.1 . . ?
C4AA C2AA H2AB 109.1 . . ?
C4AA C2AA C1AA 112.7(6) . . ?
C1AA C2AA H2AA 109.1 . . ?
C1AA C2AA H2AB 109.1 . . ?
C2AA C4AA H4AA 109.0 . . ?
C2AA C4AA H4AB 109.0 . . ?
C2AA C4AA C2CA 112.9(5) . . ?
H4AA C4AA H4AB 107.8 . . ?
C2CA C4AA H4AA 109.0 . . ?
C2CA C4AA H4AB 109.0 . . ?
C2AA C1AA H1AA 108.9 . . ?
C2AA C1AA H1AB 108.9 . . ?
C2AA C1AA C5CA 113.5(9) . . ?
H1AA C1AA H1AB 107.7 . . ?
C5CA C1AA H1AA 108.9 . . ?
C5CA C1AA H1AB 108.9 . . ?
H7AA C7AA H7AB 107.6 . . ?
C6AA C7AA H7AA 108.6 . . ?
C6AA C7AA H7AB 108.6 . . ?
C8AA C7AA H7AA 108.6 . . ?
C8AA C7AA H7AB 108.6 . . ?
C8AA C7AA C6AA 114.7(8) . . ?
C7AA C6AA H6AA 108.6 . . ?
C7AA C6AA H6AB 108.6 . . ?
H6AA C6AA H6AB 107.5 . . ?
C0BA C6AA C7AA 114.8(6) . . ?
C0BA C6AA H6AA 108.6 . . ?
C0BA C6AA H6AB 108.6 . . ?
C7AA C8AA H8AA 108.6 . . ?
C7AA C8AA H8AB 108.6 . . ?
H8AA C8AA H8AB 107.6 . . ?
C2BA C8AA C7AA 114.5(9) . . ?
C2BA C8AA H8AA 108.6 . . ?
C2BA C8AA H8AB 108.6 . . ?
C9AA C0BA C6AA 114.7(7) . . ?
C9AA C0BA H0BA 108.6 . . ?
C9AA C0BA H0BB 108.6 . . ?
C6AA C0BA H0BA 108.6 . . ?
C6AA C0BA H0BB 108.6 . . ?
H0BA C0BA H0BB 107.6 . . ?
C8AA C2BA H2BA 109.5 . . ?
C8AA C2BA H2BB 109.5 . . ?
C8AA C2BA H2BC 109.5 . . ?
H2BA C2BA H2BB 109.5 . . ?
H2BA C2BA H2BC 109.5 . . ?
H2BB C2BA H2BC 109.5 . . ?
C14 C0AA H0AA 120.5 . . ?
C3AA C0AA C14 119.0(2) . . ?
C3AA C0AA H0AA 120.5 . . ?
C0AA C3AA H3AA 119.3 . . ?
C0AA C3AA C1BA 121.3(2) . . ?
C1BA C3AA H3AA 119.3 . . ?
C19 C3BA H3BA 121.2 . . ?
C1BA C3BA C19 117.6(2) . . ?
C1BA C3BA H3BA 121.2 . . ?
C3AA C1BA H1BA 119.2 . . ?
C3BA C1BA C3AA 121.7(2) . . ?
C3BA C1BA H1BA 119.2 . . ?
H4BA C4BA H4BB 106.9 . . ?
C5BA C4BA H4BA 107.2 . . ?
C5BA C4BA H4BB 107.2 . . ?
C4CA C4BA H4BA 107.2 . . ?
C4CA C4BA H4BB 107.2 . . ?
C4CA C4BA C5BA 120.3(9) . . ?
H7BA C7BA H7BB 107.7 . . ?
C6BA C7BA H7BA 108.8 . . ?
C6BA C7BA H7BB 108.8 . . ?
C6BA C7BA C8BA 113.9(9) . . ?
C8BA C7BA H7BA 108.8 . . ?
C8BA C7BA H7BB 108.8 . . ?
C7BA C6BA H6BA 108.7 . . ?
C7BA C6BA H6BB 108.7 . . ?
C7BA C6BA C5BA 114.3(10) . . ?
H6BA C6BA H6BB 107.6 . . ?
C5BA C6BA H6BA 108.7 . . ?
C5BA C6BA H6BB 108.7 . . ?
C7BA C8BA H8BA 109.5 . . ?
C7BA C8BA H8BB 109.5 . . ?
C7BA C8BA H8BC 109.5 . . ?
H8BA C8BA H8BB 109.5 . . ?
H8BA C8BA H8BC 109.5 . . ?
H8BB C8BA H8BC 109.5 . . ?
C4BA C5BA C6BA 118.9(9) . . ?
C4BA C5BA H5BA 107.6 . . ?
C4BA C5BA H5BB 107.6 . . ?
C6BA C5BA H5BA 107.6 . . ?
C6BA C5BA H5BB 107.6 . . ?
H5BA C5BA H5BB 107.0 . . ?
C5AA C1CA H1CA 110.0 . . ?
C5AA C1CA H1CB 110.0 . . ?
H1CA C1CA H1CB 108.4 . . ?
C0CA C1CA C5AA 108.3(7) . . ?
C0CA C1CA H1CA 110.0 . . ?
C0CA C1CA H1CB 110.0 . . ?
C1CA C0CA H0CA 109.5 . . ?
C1CA C0CA H0CB 109.5 . . ?
C1CA C0CA C9BA 110.7(7) . . ?
H0CA C0CA H0CB 108.1 . . ?
C9BA C0CA H0CA 109.5 . . ?
C9BA C0CA H0CB 109.5 . . ?
C29 C9BA C0CA 116.9(7) . . ?
C29 C9BA H9BA 108.1 . . ?
C29 C9BA H9BB 108.1 . . ?
C0CA C9BA H9BA 108.1 . . ?
C0CA C9BA H9BB 108.1 . . ?
H9BA C9BA H9BB 107.3 . . ?
C4AA C2CA H2CA 110.0 . . ?
C4AA C2CA H2CB 110.0 . . ?
H2CA C2CA H2CB 108.4 . . ?
C3CA C2CA C4AA 108.3(5) . . ?
C3CA C2CA H2CA 110.0 . . ?
C3CA C2CA H2CB 110.0 . . ?
N18 C3CA C2CA 108.4(5) . . ?
N18 C3CA H3CA 110.0 . . ?
N18 C3CA H3CB 110.0 . . ?
C2CA C3CA H3CA 110.0 . . ?
C2CA C3CA H3CB 110.0 . . ?
H3CA C3CA H3CB 108.4 . . ?
C4BA C4CA H4CA 113.5 . . ?
C4BA C4CA H4CB 113.5 . . ?
C4BA C4CA C5CA 90.5(9) . . ?
H4CA C4CA H4CB 110.8 . . ?
C5CA C4CA H4CA 113.5 . . ?
C5CA C4CA H4CB 113.5 . . ?
C1AA C5CA H5CA 114.1 . . ?
C1AA C5CA H5CB 114.1 . . ?
C4CA C5CA C1AA 87.3(8) . . ?
C4CA C5CA H5CA 114.1 . . ?
C4CA C5CA H5CB 114.1 . . ?
H5CA C5CA H5CB 111.3 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.735
_oxdiff_exptl_absorpt_empirical_full_min 0.538
####################################################################### 
# 
# 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_kato_210306
_database_code_depnum_ccdc_archive 'CCDC 2305239'
loop_
_audit_author_name
_audit_author_address
'Koji Hirano'
;Osaka University
Japan
;
_audit_update_record             
;
2023-11-02 deposited with the CCDC.	2024-01-02 downloaded from the CCDC.
;
_audit_creation_date             2021-03-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C47 H45 N)'
_chemical_formula_sum            'C94 H90 N2'
_chemical_formula_weight         1247.67
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C47 H45 N'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   27.4355(3)
_cell_length_b                   7.95430(10)
_cell_length_c                   31.2422(3)
_cell_angle_alpha                90
_cell_angle_beta                 91.9370(10)
_cell_angle_gamma                90
_cell_volume                     6814.10(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    31506
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      74.1780
_cell_measurement_theta_min      4.2040
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.520
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89198
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.43a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2672
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 -19 0.1965
-11 4 -1 0.1127
-1 -1 20 0.1045
12 -3 -9 0.1213
-7 2 -16 0.1693
-10 -4 1 0.1107
1 -4 13 0.1535
13 2 11 0.1002
12 3 5 0.1039
-17 0 4 0.1388
-3 -1 -20 0.1615

_exptl_crystal_size_max          0.352
_exptl_crystal_size_mid          0.285
_exptl_crystal_size_min          0.272
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.2116 1.4882 -19.3912 0.1323 0.3743 0.9178
-11.3492 3.9510 -1.3965 -0.2487 -0.7025 0.6668
-0.9990 -1.1074 19.7981 -0.1628 -0.4603 -0.8727
11.6083 -3.2956 -8.7770 0.3266 0.9227 -0.2048
-7.0565 2.1152 -16.3668 -0.1666 0.0788 0.9829
-9.9328 -4.2843 0.6311 -0.8581 0.4093 -0.3101
0.6806 -3.8466 13.4514 -0.2968 0.1421 -0.9443
12.9728 1.9143 11.1748 0.8046 -0.3833 -0.4536
12.2576 3.4572 5.1856 0.9018 -0.4299 -0.0441
-17.4672 0.2738 4.4997 -0.8687 -0.4719 0.1508
-3.1204 -0.5610 -19.7129 -0.1840 0.6203 0.7625

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            58837
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.165
_diffrn_reflns_theta_min         4.219
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -13.00  22.00   0.50    0.09    --   42.80 -77.00  57.00   70
  2  ω     30.00  55.00   0.50    0.35    --   76.50 -77.00  57.00   50
  3  ω    -13.00  31.00   0.50    0.09    --  -42.80  77.00-176.00   88
  4  ω    -65.00   3.00   0.50    0.09    --  -42.80  57.00  90.00  136
  5  ω    -56.00 -28.00   0.50    0.35    -- -106.00  37.00  60.00   56
  6  ω    -84.00 -58.00   0.50    0.35    -- -106.00  77.00 150.00   52
  7  ω    -83.00 -33.00   0.50    0.35    -- -106.00 125.00 150.00  100
  8  ω    -95.00 -68.00   0.50    0.35    -- -106.00  37.00  60.00   54
  9  ω   -115.00 -33.00   0.50    0.35    -- -106.00  57.00 150.00  164
 10  ω    -92.00 -66.00   0.50    0.35    -- -106.00  77.00 -30.00   52
 11  ω   -105.00 -36.00   0.50    0.35    -- -106.00 125.00 -60.00  138
 12  ω    -96.00 -11.00   0.50    0.09    --  -42.80 125.00-180.00  170
 13  ω    -67.00 -36.00   0.50    0.35    -- -106.00 125.00-180.00   62
 14  ω   -113.00 -32.00   0.50    0.35    -- -106.00 125.00 -90.00  162
 15  ω   -110.00 -60.00   0.50    0.35    -- -106.00  37.00-180.00  100
 16  ω   -121.00 -35.00   0.50    0.35    -- -106.00  77.00-176.00  172
 17  ω   -107.00 -77.00   0.50    0.35    -- -106.00 125.00-180.00   60
 18  ω   -133.00 -27.00   0.50    0.35    -- -106.00  19.00-180.00  212
 19  ω   -111.00 -72.00   0.50    0.09    --  -42.80-125.00 -30.00   78
 20  ω   -138.00-113.00   0.50    0.35    -- -106.00 -77.00  57.00   50
 21  ω   -165.00 -83.00   0.50    0.35    -- -106.00 -57.00  60.00  164
 22  ω   -106.00 -70.00   0.50    0.09    --  -42.80-125.00 120.00   72
 23  ω   -155.00 -80.00   0.50    0.35    -- -106.00 -19.00 -60.00  150
 24  ω   -173.00 -84.00   0.50    0.35    -- -106.00 -99.00  30.00  178
 25  ω   -124.00 -99.00   0.50    0.35    -- -106.00  77.00 150.00   50
 26  ω     67.00  92.00   0.50    0.09    --   42.80  77.00-176.00   50
 27  ω     75.00 100.00   0.50    0.35    --   76.50  77.00-176.00   50
 28  ω     71.00 117.00   0.50    0.09    --   42.80 125.00  30.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0507544000
_diffrn_orient_matrix_UB_12      0.0824650000
_diffrn_orient_matrix_UB_13      -0.0010476000
_diffrn_orient_matrix_UB_21      0.0170498000
_diffrn_orient_matrix_UB_22      -0.1395103000
_diffrn_orient_matrix_UB_23      -0.0301937000
_diffrn_orient_matrix_UB_31      -0.0170195000
_diffrn_orient_matrix_UB_32      0.1060835000
_diffrn_orient_matrix_UB_33      -0.0390054000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12364
_reflns_number_total             13645
_reflns_odcompleteness_completeness 99.34
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.153
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     914
_refine_ls_number_reflns         13645
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0548
_refine_ls_restrained_S_all      1.032
_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)+(0.0653P)²+4.1452P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1401
_refine_ls_wR_factor_ref         0.1435
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Others
 Sof(H90C)=Sof(H90D)=Sof(H88C)=Sof(H88D)=Sof(H92C)=Sof(H92D)=Sof(H86C)=
 Sof(H86D)=Sof(C87A)=Sof(H87C)=Sof(H87D)=Sof(C89A)=Sof(H89C)=Sof(H89D)=
 Sof(C91A)=Sof(H91C)=Sof(H91D)=1-FVAR(1)
 Sof(H90A)=Sof(H90B)=Sof(H88A)=Sof(H88B)=Sof(H92A)=Sof(H92B)=Sof(H86A)=
 Sof(H86B)=Sof(C87)=Sof(H87A)=Sof(H87B)=Sof(C89)=Sof(H89A)=Sof(H89B)=Sof(C91)=
 Sof(H91A)=Sof(H91B)=FVAR(1)
 Sof(H94C)=Sof(H94D)=Sof(H96D)=Sof(H96E)=Sof(H96F)=Sof(C95A)=Sof(H95C)=
 Sof(H95D)=Sof(C93A)=Sof(H93C)=Sof(H93D)=1-FVAR(2)
 Sof(H94A)=Sof(H94B)=Sof(H96A)=Sof(H96B)=Sof(H96C)=Sof(C93)=Sof(H93A)=
 Sof(H93B)=Sof(C95)=Sof(H95A)=Sof(H95B)=FVAR(2)
3.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B), C43(H43A,H43B), C40(H40A,H40B), C44(H44A,
 H44B), C42(H42A,H42B), C46(H46A,H46B), C85(H85A,H85B), C39(H39A,H39B),
 C41(H41A,H41B), C90(H90A,H90B), C90(H90C,H90D), C45(H45A,H45B), C47(H47A,H47B),
  C88(H88A,H88B), C88(H88C,H88D), C92(H92A,H92B), C92(H92C,H92D), C94(H94A,
 H94B), C94(H94C,H94D), C86(H86A,H86B), C86(H86C,H86D), C87(H87A,H87B),
 C89(H89A,H89B), C91(H91A,H91B), C93(H93A,H93B), C95(H95A,H95B), C87A(H87C,
 H87D), C89A(H89C,H89D), C91A(H91C,H91D), C95A(H95C,H95D), C93A(H93C,H93D)
3.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C14(H14), C22(H22), C21(H21), C51(H51), C68(H68), C33(H33), C7(H7),
 C16(H16), C23(H23), C5(H5), C62(H62), C72(H72), C65(H65), C66(H66), C81(H81),
 C64(H64), C26(H26), C74(H74), C63(H63), C6(H6), C67(H67), C19(H19), C71(H71),
 C69(H69), C17(H17), C36(H36), C70(H70), C77(H77), C29(H29), C27(H27), C18(H18),
  C84(H84), C35(H35), C82(H82), C34(H34), C76(H76), C28(H28), C83(H83), C75(H75)
3.c Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C96(H96A,H96B,H96C), C96(H96D,H96E,H96F)
;
_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
N13 N 0.34710(4) 0.40048(15) 0.74541(4) 0.0201(2) Uani 1 1 d . . . . .
N61 N 0.65014(4) 0.53750(17) 0.75036(4) 0.0248(3) Uani 1 1 d . . . . .
C1 C 0.37194(5) 0.30552(17) 0.71530(4) 0.0190(3) Uani 1 1 d . . . . .
C11 C 0.29419(5) 0.34499(18) 0.68971(4) 0.0200(3) Uani 1 1 d . . . . .
C10 C 0.34031(5) 0.27126(18) 0.68128(4) 0.0201(3) Uani 1 1 d . . . . .
C24 C 0.24872(5) 0.35172(19) 0.66744(4) 0.0232(3) Uani 1 1 d . . . . .
H24 H 0.244309 0.300014 0.640889 0.028 Uiso 1 1 calc R . . . .
C2 C 0.42263(5) 0.24940(17) 0.71711(4) 0.0201(3) Uani 1 1 d . . . . .
C49 C 0.62466(5) 0.63268(19) 0.77999(4) 0.0223(3) Uani 1 1 d . . . . .
C12 C 0.29977(5) 0.42365(18) 0.73006(4) 0.0206(3) Uani 1 1 d . . . . .
C58 C 0.65565(5) 0.66921(19) 0.81428(4) 0.0224(3) Uani 1 1 d . . . . .
C3 C 0.43863(5) 0.14969(18) 0.68091(4) 0.0206(3) Uani 1 1 d . . . . .
C50 C 0.57352(5) 0.68565(18) 0.77776(4) 0.0223(3) Uani 1 1 d . . . . .
C30 C 0.29875(5) 0.1099(2) 0.58313(4) 0.0248(3) Uani 1 1 d . . . . .
C9 C 0.35540(5) 0.18820(18) 0.64067(4) 0.0203(3) Uani 1 1 d . . . . .
C8 C 0.40636(5) 0.11016(18) 0.64581(4) 0.0217(3) Uani 1 1 d . . . . .
C14 C 0.45534(5) 0.27950(18) 0.75038(5) 0.0231(3) Uani 1 1 d . . . . .
H14 H 0.444791 0.339576 0.773871 0.028 Uiso 1 1 calc R . . . .
C73 C 0.64244(5) 0.62853(19) 0.89170(4) 0.0234(3) Uani 1 1 d . . . . .
C59 C 0.70201(5) 0.59608(19) 0.80662(4) 0.0239(3) Uani 1 1 d . . . . .
C25 C 0.31769(5) 0.06065(18) 0.62340(4) 0.0218(3) Uani 1 1 d . . . . .
C32 C 0.35425(5) 0.31811(18) 0.60422(4) 0.0220(3) Uani 1 1 d . . . . .
C37 C 0.36333(5) 0.46613(18) 0.78719(4) 0.0221(3) Uani 1 1 d . . . . .
H37A H 0.344091 0.564607 0.793706 0.026 Uiso 1 1 calc R . . . .
H37B H 0.397099 0.501155 0.785773 0.026 Uiso 1 1 calc R . . . .
C56 C 0.58868(5) 0.82805(19) 0.84888(4) 0.0232(3) Uani 1 1 d . . . . .
C60 C 0.69727(5) 0.5153(2) 0.76646(5) 0.0250(3) Uani 1 1 d . . . . .
C15 C 0.50477(5) 0.22328(18) 0.75079(4) 0.0232(3) Uani 1 1 d . . . . .
C79 C 0.69480(5) 0.8474(2) 0.91209(5) 0.0260(3) Uani 1 1 d . . . . .
C55 C 0.55699(5) 0.78605(18) 0.81359(4) 0.0221(3) Uani 1 1 d . . . . .
C57 C 0.64020(5) 0.75453(19) 0.85433(4) 0.0219(3) Uani 1 1 d . . . . .
C4 C 0.48724(5) 0.08463(18) 0.68119(4) 0.0221(3) Uani 1 1 d . . . . .
C20 C 0.52141(5) 0.12612(18) 0.71648(5) 0.0233(3) Uani 1 1 d . . . . .
C54 C 0.50813(5) 0.84827(19) 0.81293(5) 0.0234(3) Uani 1 1 d . . . . .
C52 C 0.49157(5) 0.70657(19) 0.74363(5) 0.0239(3) Uani 1 1 d . . . . .
C53 C 0.47442(5) 0.80605(18) 0.77720(5) 0.0234(3) Uani 1 1 d . . . . .
C80 C 0.67684(5) 0.88730(19) 0.87071(5) 0.0235(3) Uani 1 1 d . . . . .
C22 C 0.21727(5) 0.51550(19) 0.72599(5) 0.0261(3) Uani 1 1 d . . . . .
H22 H 0.191223 0.572751 0.737510 0.031 Uiso 1 1 calc R . . . .
C21 C 0.26131(5) 0.50983(19) 0.74866(5) 0.0238(3) Uani 1 1 d . . . . .
H21 H 0.265300 0.561299 0.775273 0.029 Uiso 1 1 calc R . . . .
C51 C 0.54109(5) 0.65079(19) 0.74466(5) 0.0245(3) Uani 1 1 d . . . . .
H51 H 0.551829 0.587747 0.721748 0.029 Uiso 1 1 calc R . . . .
C68 C 0.57245(5) 0.9342(2) 0.88075(5) 0.0262(3) Uani 1 1 d . . . . .
H68 H 0.593653 0.963797 0.903349 0.031 Uiso 1 1 calc R . . . .
C31 C 0.32087(5) 0.2708(2) 0.57152(4) 0.0249(3) Uani 1 1 d . . . . .
C33 C 0.38030(6) 0.4667(2) 0.60151(5) 0.0274(3) Uani 1 1 d . . . . .
H33 H 0.402481 0.497869 0.623235 0.033 Uiso 1 1 calc R . . . .
C7 C 0.42165(5) 0.00242(19) 0.61401(5) 0.0248(3) Uani 1 1 d . . . . .
H7 H 0.400158 -0.025358 0.591459 0.030 Uiso 1 1 calc R . . . .
C16 C 0.53702(5) 0.2640(2) 0.78552(5) 0.0267(3) Uani 1 1 d . . . . .
H16 H 0.525814 0.328234 0.808042 0.032 Uiso 1 1 calc R . . . .
C78 C 0.67414(5) 0.6852(2) 0.92466(5) 0.0261(3) Uani 1 1 d . . . . .
C23 C 0.21086(5) 0.43654(19) 0.68579(5) 0.0256(3) Uani 1 1 d . . . . .
H23 H 0.180645 0.441710 0.671433 0.031 Uiso 1 1 calc R . . . .
C5 C 0.50088(5) -0.0224(2) 0.64798(5) 0.0269(3) Uani 1 1 d . . . . .
H5 H 0.532394 -0.065469 0.648091 0.032 Uiso 1 1 calc R . . . .
C62 C 0.45977(5) 0.6643(2) 0.70863(5) 0.0272(3) Uani 1 1 d . . . . .
H62 H 0.471153 0.597965 0.686574 0.033 Uiso 1 1 calc R . . . .
C72 C 0.74681(5) 0.5913(2) 0.82962(5) 0.0270(3) Uani 1 1 d . . . . .
H72 H 0.750508 0.644687 0.856012 0.032 Uiso 1 1 calc R . . . .
C65 C 0.42558(5) 0.8617(2) 0.77441(5) 0.0268(3) Uani 1 1 d . . . . .
H65 H 0.413537 0.927617 0.796246 0.032 Uiso 1 1 calc R . . . .
C66 C 0.49328(5) 0.9526(2) 0.84634(5) 0.0277(3) Uani 1 1 d . . . . .
H66 H 0.461423 0.992599 0.846117 0.033 Uiso 1 1 calc R . . . .
C81 C 0.69223(5) 1.0310(2) 0.85023(5) 0.0286(3) Uani 1 1 d . . . . .
H81 H 0.680686 1.056392 0.822648 0.034 Uiso 1 1 calc R . . . .
C64 C 0.39538(5) 0.8199(2) 0.73981(5) 0.0289(3) Uani 1 1 d . . . . .
H64 H 0.363392 0.858745 0.738477 0.035 Uiso 1 1 calc R . . . .
C26 C 0.30213(5) -0.0865(2) 0.64228(5) 0.0270(3) Uani 1 1 d . . . . .
H26 H 0.314332 -0.118448 0.669205 0.032 Uiso 1 1 calc R . . . .
C38 C 0.35892(6) 0.3387(2) 0.82326(5) 0.0284(3) Uani 1 1 d . . . . .
H38A H 0.379948 0.243428 0.817974 0.034 Uiso 1 1 calc R . . . .
H38B H 0.325603 0.298123 0.823744 0.034 Uiso 1 1 calc R . . . .
C74 C 0.61864(6) 0.4754(2) 0.89479(5) 0.0287(3) Uani 1 1 d . . . . .
H74 H 0.597535 0.438277 0.872865 0.034 Uiso 1 1 calc R . . . .
C63 C 0.41240(6) 0.7198(2) 0.70681(5) 0.0284(3) Uani 1 1 d . . . . .
H63 H 0.391778 0.690943 0.683742 0.034 Uiso 1 1 calc R . . . .
C6 C 0.46833(6) -0.0647(2) 0.61519(5) 0.0282(3) Uani 1 1 d . . . . .
H6 H 0.477671 -0.138278 0.593832 0.034 Uiso 1 1 calc R . . . .
C67 C 0.52525(6) 0.9966(2) 0.87948(5) 0.0297(3) Uani 1 1 d . . . . .
H67 H 0.515138 1.068211 0.900979 0.036 Uiso 1 1 calc R . . . .
C19 C 0.57046(5) 0.0729(2) 0.71835(5) 0.0292(3) Uani 1 1 d . . . . .
H19 H 0.582315 0.008966 0.696061 0.035 Uiso 1 1 calc R . . . .
C71 C 0.78530(5) 0.5059(2) 0.81238(5) 0.0305(3) Uani 1 1 d . . . . .
H71 H 0.815190 0.502017 0.827295 0.037 Uiso 1 1 calc R . . . .
C43 C 0.49995(6) 0.6951(2) 0.96359(5) 0.0304(3) Uani 1 1 d . . . . .
H43A H 0.480975 0.660158 0.987667 0.037 Uiso 1 1 calc R . . . .
H43B H 0.487871 0.804261 0.954294 0.037 Uiso 1 1 calc R . . . .
C69 C 0.73623(5) 0.4287(2) 0.74902(5) 0.0303(3) Uani 1 1 d . . . . .
H69 H 0.732935 0.375665 0.722550 0.036 Uiso 1 1 calc R . . . .
C40 C 0.42747(6) 0.4453(2) 0.87463(5) 0.0313(3) Uani 1 1 d . . . . .
H40A H 0.443705 0.337723 0.878331 0.038 Uiso 1 1 calc R . . . .
H40B H 0.440711 0.499815 0.849789 0.038 Uiso 1 1 calc R . . . .
C17 C 0.58444(6) 0.2105(2) 0.78652(5) 0.0306(3) Uani 1 1 d . . . . .
H17 H 0.605325 0.237897 0.809532 0.037 Uiso 1 1 calc R . . . .
C36 C 0.31337(6) 0.3735(2) 0.53571(5) 0.0331(4) Uani 1 1 d . . . . .
H36 H 0.291263 0.342686 0.513894 0.040 Uiso 1 1 calc R . . . .
C70 C 0.77987(6) 0.4245(2) 0.77253(5) 0.0325(3) Uani 1 1 d . . . . .
H70 H 0.806216 0.366673 0.761724 0.039 Uiso 1 1 calc R . . . .
C44 C 0.55299(5) 0.7138(2) 0.97873(5) 0.0298(3) Uani 1 1 d . . . . .
H44A H 0.563507 0.610119 0.992550 0.036 Uiso 1 1 calc R . . . .
H44B H 0.572857 0.730364 0.953980 0.036 Uiso 1 1 calc R . . . .
C77 C 0.68209(6) 0.5876(2) 0.96137(5) 0.0337(4) Uani 1 1 d . . . . .
H77 H 0.702892 0.624795 0.983504 0.040 Uiso 1 1 calc R . . . .
C42 C 0.49150(6) 0.5703(2) 0.92726(5) 0.0311(3) Uani 1 1 d . . . . .
H42A H 0.509647 0.606304 0.902777 0.037 Uiso 1 1 calc R . . . .
H42B H 0.503953 0.461202 0.936193 0.037 Uiso 1 1 calc R . . . .
C29 C 0.26424(6) 0.0112(2) 0.56132(5) 0.0333(4) Uani 1 1 d . . . . .
H29 H 0.251437 0.044010 0.534678 0.040 Uiso 1 1 calc R . . . .
C46 C 0.61492(6) 0.8903(2) 1.02219(5) 0.0326(3) Uani 1 1 d . . . . .
H46A H 0.628102 0.791405 1.036561 0.039 Uiso 1 1 calc R . . . .
H46B H 0.633037 0.907377 0.996414 0.039 Uiso 1 1 calc R . . . .
C85 C 0.63493(6) 0.4741(2) 0.70819(5) 0.0329(4) Uani 1 1 d . . . . .
H85A H 0.601677 0.433380 0.709323 0.039 Uiso 1 1 calc R . . . .
H85B H 0.655493 0.379644 0.701100 0.039 Uiso 1 1 calc R . . . .
C27 C 0.26786(6) -0.1859(2) 0.62021(6) 0.0342(4) Uani 1 1 d . . . . .
H27 H 0.257285 -0.285610 0.632371 0.041 Uiso 1 1 calc R . . . .
C39 C 0.37304(6) 0.4160(2) 0.86660(5) 0.0346(4) Uani 1 1 d . . . . .
H39A H 0.356307 0.522848 0.869066 0.042 Uiso 1 1 calc R . . . .
H39B H 0.361446 0.342910 0.888926 0.042 Uiso 1 1 calc R . . . .
C41 C 0.43802(6) 0.5531(2) 0.91388(5) 0.0321(3) Uani 1 1 d . . . . .
H41A H 0.420772 0.505841 0.937657 0.039 Uiso 1 1 calc R . . . .
H41B H 0.424879 0.664568 0.908447 0.039 Uiso 1 1 calc R . . . .
C18 C 0.60117(6) 0.1140(2) 0.75261(5) 0.0341(4) Uani 1 1 d . . . . .
H18 H 0.633360 0.077232 0.753155 0.041 Uiso 1 1 calc R . . . .
C84 C 0.72785(6) 0.9540(2) 0.93335(5) 0.0336(4) Uani 1 1 d . . . . .
H84 H 0.739783 0.928296 0.960790 0.040 Uiso 1 1 calc R . . . .
C90 C 0.50890(6) 0.3533(2) 0.56959(5) 0.0338(4) Uani 1 1 d . . . . .
H90A H 0.496306 0.465206 0.563761 0.041 Uiso 0.570(6) 1 calc R . P A 1
H90B H 0.492018 0.309080 0.593942 0.041 Uiso 0.570(6) 1 calc R . P A 1
H90C H 0.519372 0.242250 0.578866 0.041 Uiso 0.430(6) 1 calc R . P A 2
H90D H 0.482551 0.387227 0.587633 0.041 Uiso 0.430(6) 1 calc R . P A 2
C35 C 0.33936(7) 0.5221(2) 0.53318(5) 0.0377(4) Uani 1 1 d . . . . .
H35 H 0.334510 0.591733 0.509500 0.045 Uiso 1 1 calc R . . . .
C45 C 0.56177(6) 0.8582(2) 1.00960(5) 0.0346(4) Uani 1 1 d . . . . .
H45A H 0.544126 0.836001 1.035387 0.042 Uiso 1 1 calc R . . . .
H45B H 0.548254 0.959742 0.996747 0.042 Uiso 1 1 calc R . . . .
C82 C 0.72529(6) 1.1371(2) 0.87157(6) 0.0353(4) Uani 1 1 d . . . . .
H82 H 0.735889 1.234215 0.858168 0.042 Uiso 1 1 calc R . . . .
C34 C 0.37265(7) 0.5686(2) 0.56562(5) 0.0346(4) Uani 1 1 d . . . . .
H34 H 0.389957 0.668527 0.563333 0.042 Uiso 1 1 calc R . . . .
C76 C 0.65849(7) 0.4345(2) 0.96427(5) 0.0387(4) Uani 1 1 d . . . . .
H76 H 0.663720 0.368124 0.988498 0.046 Uiso 1 1 calc R . . . .
C28 C 0.24934(6) -0.1371(2) 0.58012(6) 0.0378(4) Uani 1 1 d . . . . .
H28 H 0.226599 -0.205059 0.565710 0.045 Uiso 1 1 calc R . . . .
C83 C 0.74262(6) 1.0988(2) 0.91287(6) 0.0383(4) Uani 1 1 d . . . . .
H83 H 0.764389 1.171500 0.926871 0.046 Uiso 1 1 calc R . . . .
C75 C 0.62704(6) 0.3783(2) 0.93143(5) 0.0359(4) Uani 1 1 d . . . . .
H75 H 0.611476 0.275124 0.933967 0.043 Uiso 1 1 calc R . . . .
C47 C 0.62253(6) 1.0413(2) 1.05129(6) 0.0405(4) Uani 1 1 d . . . . .
H47A H 0.605329 1.021960 1.077461 0.049 Uiso 1 1 calc R . . . .
H47B H 0.608025 1.139004 1.037339 0.049 Uiso 1 1 calc R . . . .
C88 C 0.57185(6) 0.4790(3) 0.62238(5) 0.0386(4) Uani 1 1 d . . . . .
H88A H 0.557829 0.589931 0.618170 0.046 Uiso 0.570(6) 1 calc R . P A 1
H88B H 0.557359 0.428200 0.647156 0.046 Uiso 0.570(6) 1 calc R . P A 1
H88C H 0.578325 0.364269 0.631456 0.046 Uiso 0.430(6) 1 calc R . P A 2
H88D H 0.547262 0.524732 0.640695 0.046 Uiso 0.430(6) 1 calc R . P A 2
C92 C 0.44718(7) 0.2191(3) 0.51801(6) 0.0435(4) Uani 1 1 d . . . . .
H92A H 0.430477 0.316724 0.528978 0.052 Uiso 0.570(6) 1 calc R . P A 1
H92B H 0.436155 0.124129 0.534580 0.052 Uiso 0.570(6) 1 calc R . P A 1
H92C H 0.446227 0.158775 0.544952 0.052 Uiso 0.430(6) 1 calc R . P A 2
H92D H 0.418866 0.292182 0.517652 0.052 Uiso 0.430(6) 1 calc R . P A 2
C48 C 0.67547(7) 1.0802(3) 1.06294(7) 0.0482(5) Uani 1 1 d . . . . .
H48A H 0.693440 1.091605 1.037267 0.072 Uiso 1 1 calc GR . . . .
H48B H 0.689101 0.990392 1.080025 0.072 Uiso 1 1 calc GR . . . .
H48C H 0.677355 1.183250 1.078910 0.072 Uiso 1 1 calc GR . . . .
C94 C 0.38268(8) 0.0589(3) 0.47467(6) 0.0511(5) Uani 1 1 d . . . . .
H94A H 0.396252 -0.050348 0.482054 0.061 Uiso 0.530(5) 1 calc R . P A 1
H94B H 0.360584 0.089805 0.496948 0.061 Uiso 0.530(5) 1 calc R . P A 1
H94C H 0.368791 0.163739 0.464129 0.061 Uiso 0.470(5) 1 calc R . P A 2
H94D H 0.366280 0.030768 0.500747 0.061 Uiso 0.470(5) 1 calc R . P A 2
C86 C 0.63755(8) 0.6047(4) 0.67304(6) 0.0615(7) Uani 1 1 d . . . . .
H86A H 0.669419 0.657507 0.672997 0.074 Uiso 0.570(6) 1 calc R . P A 1
H86B H 0.612816 0.690629 0.676026 0.074 Uiso 0.570(6) 1 calc R . P A 1
H86C H 0.621251 0.703602 0.683740 0.074 Uiso 0.430(6) 1 calc R . P A 2
H86D H 0.671749 0.634231 0.671473 0.074 Uiso 0.430(6) 1 calc R . P A 2
C96 C 0.31646(9) -0.0975(4) 0.43593(11) 0.0798(9) Uani 1 1 d . . . . .
H96A H 0.330285 -0.196606 0.449005 0.120 Uiso 0.530(5) 1 calc GR . P A 1
H96B H 0.305805 -0.122500 0.407045 0.120 Uiso 0.530(5) 1 calc GR . P A 1
H96C H 0.289134 -0.060745 0.451899 0.120 Uiso 0.530(5) 1 calc GR . P A 1
H96D H 0.303310 -0.005502 0.419346 0.120 Uiso 0.470(5) 1 calc GR . P A 2
H96E H 0.301744 -0.099563 0.463373 0.120 Uiso 0.470(5) 1 calc GR . P A 2
H96F H 0.309689 -0.201248 0.421195 0.120 Uiso 0.470(5) 1 calc GR . P A 2
C87 C 0.62737(14) 0.4925(7) 0.62961(11) 0.0371(9) Uani 0.570(6) 1 d . . P A 1
H87A H 0.641834 0.546391 0.605251 0.044 Uiso 0.570(6) 1 calc R . P A 1
H87B H 0.641578 0.381454 0.633105 0.044 Uiso 0.570(6) 1 calc R . P A 1
C89 C 0.56123(11) 0.3658(5) 0.58104(9) 0.0333(9) Uani 0.570(6) 1 d . . P A 1
H89A H 0.578115 0.413345 0.557084 0.040 Uiso 0.570(6) 1 calc R . P A 1
H89B H 0.574144 0.253904 0.586254 0.040 Uiso 0.570(6) 1 calc R . P A 1
C91 C 0.49745(13) 0.2416(7) 0.53071(13) 0.0451(11) Uani 0.570(6) 1 d . . P A 1
H91A H 0.514158 0.288047 0.506526 0.054 Uiso 0.570(6) 1 calc R . P A 1
H91B H 0.511357 0.131478 0.536493 0.054 Uiso 0.570(6) 1 calc R . P A 1
C93 C 0.35559(18) 0.0440(7) 0.43568(16) 0.0665(15) Uani 0.530(5) 1 d . . P A 1
H93A H 0.377845 0.021714 0.412886 0.080 Uiso 0.530(5) 1 calc R . P A 1
H93B H 0.339546 0.150289 0.429432 0.080 Uiso 0.530(5) 1 calc R . P A 1
C95 C 0.42626(15) 0.1931(5) 0.47455(14) 0.0507(12) Uani 0.530(5) 1 d . . P A 1
H95A H 0.451489 0.153565 0.456014 0.061 Uiso 0.530(5) 1 calc R . P A 1
H95B H 0.414065 0.299257 0.463259 0.061 Uiso 0.530(5) 1 calc R . P A 1
C87A C 0.61961(18) 0.5843(8) 0.62847(14) 0.0339(11) Uani 0.430(6) 1 d . . P A 2
H87C H 0.644978 0.531001 0.612366 0.041 Uiso 0.430(6) 1 calc R . P A 2
H87D H 0.613948 0.694948 0.616256 0.041 Uiso 0.430(6) 1 calc R . P A 2
C89A C 0.55224(15) 0.4773(7) 0.57733(11) 0.0322(12) Uani 0.430(6) 1 d . . P A 2
H89C H 0.578298 0.446901 0.558587 0.039 Uiso 0.430(6) 1 calc R . P A 2
H89D H 0.541524 0.589849 0.569639 0.039 Uiso 0.430(6) 1 calc R . P A 2
C91A C 0.48951(16) 0.3407(7) 0.52527(13) 0.0323(11) Uani 0.430(6) 1 d . . P A 2
H91C H 0.515821 0.306624 0.507193 0.039 Uiso 0.430(6) 1 calc R . P A 2
H91D H 0.478973 0.451588 0.515970 0.039 Uiso 0.430(6) 1 calc R . P A 2
C95A C 0.43353(14) 0.0884(7) 0.48580(13) 0.0431(13) Uani 0.470(5) 1 d . . P A 2
H95C H 0.449679 0.116479 0.459597 0.052 Uiso 0.470(5) 1 calc R . P A 2
H95D H 0.447273 -0.017245 0.495939 0.052 Uiso 0.470(5) 1 calc R . P A 2
C93A C 0.37063(17) -0.0759(7) 0.44201(16) 0.0529(14) Uani 0.470(5) 1 d . . P A
2
H93C H 0.384464 -0.045911 0.414883 0.063 Uiso 0.470(5) 1 calc R . P A 2
H93D H 0.385100 -0.181512 0.451401 0.063 Uiso 0.470(5) 1 calc R . 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
N13 C1 1.4013(17) . ?
N13 C12 1.3813(17) . ?
N13 C37 1.4611(17) . ?
N61 C49 1.4010(18) . ?
N61 C60 1.3830(19) . ?
N61 C85 1.4582(18) . ?
C1 C10 1.3765(18) . ?
C1 C2 1.4600(18) . ?
C11 C10 1.4270(19) . ?
C11 C24 1.4090(19) . ?
C11 C12 1.4111(19) . ?
C10 C9 1.5010(18) . ?
C24 H24 0.9300 . ?
C24 C23 1.380(2) . ?
C2 C3 1.4611(19) . ?
C2 C14 1.3711(19) . ?
C49 C58 1.3760(19) . ?
C49 C50 1.4642(19) . ?
C12 C21 1.401(2) . ?
C58 C59 1.426(2) . ?
C58 C57 1.4971(19) . ?
C3 C8 1.4211(19) . ?
C3 C4 1.4301(19) . ?
C50 C55 1.460(2) . ?
C50 C51 1.369(2) . ?
C30 C25 1.401(2) . ?
C30 C31 1.467(2) . ?
C30 C29 1.390(2) . ?
C9 C8 1.5334(19) . ?
C9 C25 1.5338(19) . ?
C9 C32 1.5373(19) . ?
C8 C7 1.388(2) . ?
C14 H14 0.9300 . ?
C14 C15 1.4277(19) . ?
C73 C57 1.539(2) . ?
C73 C78 1.400(2) . ?
C73 C74 1.387(2) . ?
C59 C60 1.412(2) . ?
C59 C72 1.403(2) . ?
C25 C26 1.385(2) . ?
C32 C31 1.400(2) . ?
C32 C33 1.385(2) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 C38 1.523(2) . ?
C56 C55 1.4205(19) . ?
C56 C57 1.5339(19) . ?
C56 C68 1.390(2) . ?
C60 C69 1.398(2) . ?
C15 C20 1.410(2) . ?
C15 C16 1.414(2) . ?
C79 C80 1.404(2) . ?
C79 C78 1.468(2) . ?
C79 C84 1.393(2) . ?
C55 C54 1.4285(19) . ?
C57 C80 1.534(2) . ?
C4 C20 1.461(2) . ?
C4 C5 1.403(2) . ?
C20 C19 1.410(2) . ?
C54 C53 1.464(2) . ?
C54 C66 1.405(2) . ?
C52 C53 1.407(2) . ?
C52 C51 1.429(2) . ?
C52 C62 1.416(2) . ?
C53 C65 1.411(2) . ?
C80 C81 1.383(2) . ?
C22 H22 0.9300 . ?
C22 C21 1.380(2) . ?
C22 C23 1.410(2) . ?
C21 H21 0.9300 . ?
C51 H51 0.9300 . ?
C68 H68 0.9300 . ?
C68 C67 1.386(2) . ?
C31 C36 1.395(2) . ?
C33 H33 0.9300 . ?
C33 C34 1.394(2) . ?
C7 H7 0.9300 . ?
C7 C6 1.387(2) . ?
C16 H16 0.9300 . ?
C16 C17 1.368(2) . ?
C78 C77 1.396(2) . ?
C23 H23 0.9300 . ?
C5 H5 0.9300 . ?
C5 C6 1.378(2) . ?
C62 H62 0.9300 . ?
C62 C63 1.372(2) . ?
C72 H72 0.9300 . ?
C72 C71 1.380(2) . ?
C65 H65 0.9300 . ?
C65 C64 1.380(2) . ?
C66 H66 0.9300 . ?
C66 C67 1.379(2) . ?
C81 H81 0.9300 . ?
C81 C82 1.392(2) . ?
C64 H64 0.9300 . ?
C64 C63 1.395(2) . ?
C26 H26 0.9300 . ?
C26 C27 1.393(2) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 C39 1.525(2) . ?
C74 H74 0.9300 . ?
C74 C75 1.394(2) . ?
C63 H63 0.9300 . ?
C6 H6 0.9300 . ?
C67 H67 0.9300 . ?
C19 H19 0.9300 . ?
C19 C18 1.379(2) . ?
C71 H71 0.9300 . ?
C71 C70 1.406(2) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C43 C44 1.522(2) . ?
C43 C42 1.520(2) . ?
C69 H69 0.9300 . ?
C69 C70 1.384(2) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C40 C39 1.524(2) . ?
C40 C41 1.516(2) . ?
C17 H17 0.9300 . ?
C17 C18 1.398(2) . ?
C36 H36 0.9300 . ?
C36 C35 1.384(3) . ?
C70 H70 0.9300 . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C44 C45 1.514(2) . ?
C77 H77 0.9300 . ?
C77 C76 1.384(3) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C42 C41 1.518(2) . ?
C29 H29 0.9300 . ?
C29 C28 1.386(3) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C46 C45 1.519(2) . ?
C46 C47 1.516(2) . ?
C85 H85A 0.9700 . ?
C85 H85B 0.9700 . ?
C85 C86 1.515(3) . ?
C27 H27 0.9300 . ?
C27 C28 1.391(3) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C18 H18 0.9300 . ?
C84 H84 0.9300 . ?
C84 C83 1.385(3) . ?
C90 H90A 0.9700 . ?
C90 H90B 0.9700 . ?
C90 H90C 0.9700 . ?
C90 H90D 0.9700 . ?
C90 C89 1.471(3) . ?
C90 C91 1.529(4) . ?
C90 C89A 1.558(4) . ?
C90 C91A 1.470(4) . ?
C35 H35 0.9300 . ?
C35 C34 1.391(3) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C82 H82 0.9300 . ?
C82 C83 1.394(3) . ?
C34 H34 0.9300 . ?
C76 H76 0.9300 . ?
C76 C75 1.391(3) . ?
C28 H28 0.9300 . ?
C83 H83 0.9300 . ?
C75 H75 0.9300 . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C47 C48 1.517(2) . ?
C88 H88A 0.9700 . ?
C88 H88B 0.9700 . ?
C88 H88C 0.9700 . ?
C88 H88D 0.9700 . ?
C88 C87 1.536(4) . ?
C88 C89 1.593(3) . ?
C88 C87A 1.561(5) . ?
C88 C89A 1.490(4) . ?
C92 H92A 0.9700 . ?
C92 H92B 0.9700 . ?
C92 H92C 0.9700 . ?
C92 H92D 0.9700 . ?
C92 C91 1.433(4) . ?
C92 C95 1.471(4) . ?
C92 C91A 1.522(5) . ?
C92 C95A 1.486(4) . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C94 H94A 0.9700 . ?
C94 H94B 0.9700 . ?
C94 H94C 0.9700 . ?
C94 H94D 0.9700 . ?
C94 C93 1.410(5) . ?
C94 C95 1.603(5) . ?
C94 C95A 1.446(4) . ?
C94 C93A 1.509(5) . ?
C86 H86A 0.9700 . ?
C86 H86B 0.9700 . ?
C86 H86C 0.9700 . ?
C86 H86D 0.9700 . ?
C86 C87 1.640(4) . ?
C86 C87A 1.470(5) . ?
C96 H96A 0.9600 . ?
C96 H96B 0.9600 . ?
C96 H96C 0.9600 . ?
C96 H96D 0.9600 . ?
C96 H96E 0.9600 . ?
C96 H96F 0.9600 . ?
C96 C93 1.556(6) . ?
C96 C93A 1.502(5) . ?
C87 H87A 0.9700 . ?
C87 H87B 0.9700 . ?
C89 H89A 0.9700 . ?
C89 H89B 0.9700 . ?
C91 H91A 0.9700 . ?
C91 H91B 0.9700 . ?
C93 H93A 0.9700 . ?
C93 H93B 0.9700 . ?
C95 H95A 0.9700 . ?
C95 H95B 0.9700 . ?
C87A H87C 0.9700 . ?
C87A H87D 0.9700 . ?
C89A H89C 0.9700 . ?
C89A H89D 0.9700 . ?
C91A H91C 0.9700 . ?
C91A H91D 0.9700 . ?
C95A H95C 0.9700 . ?
C95A H95D 0.9700 . ?
C93A H93C 0.9700 . ?
C93A H93D 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
C1 N13 C37 130.69(11) . . ?
C12 N13 C1 108.16(11) . . ?
C12 N13 C37 121.12(11) . . ?
C49 N61 C85 130.53(12) . . ?
C60 N61 C49 108.06(12) . . ?
C60 N61 C85 121.33(12) . . ?
N13 C1 C2 128.53(12) . . ?
C10 C1 N13 108.48(11) . . ?
C10 C1 C2 122.99(12) . . ?
C24 C11 C10 134.44(13) . . ?
C24 C11 C12 119.46(13) . . ?
C12 C11 C10 106.10(12) . . ?
C1 C10 C11 108.41(12) . . ?
C1 C10 C9 123.72(12) . . ?
C11 C10 C9 127.49(12) . . ?
C11 C24 H24 120.7 . . ?
C23 C24 C11 118.67(13) . . ?
C23 C24 H24 120.7 . . ?
C1 C2 C3 116.53(12) . . ?
C14 C2 C1 125.05(13) . . ?
C14 C2 C3 118.40(12) . . ?
N61 C49 C50 128.51(13) . . ?
C58 C49 N61 108.64(12) . . ?
C58 C49 C50 122.83(13) . . ?
N13 C12 C11 108.86(12) . . ?
N13 C12 C21 129.33(13) . . ?
C21 C12 C11 121.81(13) . . ?
C49 C58 C59 108.32(12) . . ?
C49 C58 C57 124.16(12) . . ?
C59 C58 C57 127.18(13) . . ?
C8 C3 C2 121.46(12) . . ?
C8 C3 C4 118.76(13) . . ?
C4 C3 C2 119.75(12) . . ?
C55 C50 C49 116.29(12) . . ?
C51 C50 C49 125.08(13) . . ?
C51 C50 C55 118.62(13) . . ?
C25 C30 C31 108.78(13) . . ?
C29 C30 C25 120.53(15) . . ?
C29 C30 C31 130.69(14) . . ?
C10 C9 C8 111.48(11) . . ?
C10 C9 C25 112.73(11) . . ?
C10 C9 C32 109.32(11) . . ?
C8 C9 C25 111.77(12) . . ?
C8 C9 C32 110.21(11) . . ?
C25 C9 C32 100.80(11) . . ?
C3 C8 C9 122.24(12) . . ?
C7 C8 C3 119.58(13) . . ?
C7 C8 C9 118.14(12) . . ?
C2 C14 H14 118.3 . . ?
C2 C14 C15 123.31(13) . . ?
C15 C14 H14 118.3 . . ?
C78 C73 C57 110.87(13) . . ?
C74 C73 C57 128.17(13) . . ?
C74 C73 C78 120.94(14) . . ?
C60 C59 C58 106.20(12) . . ?
C72 C59 C58 134.10(14) . . ?
C72 C59 C60 119.70(13) . . ?
C30 C25 C9 110.87(13) . . ?
C26 C25 C30 120.56(14) . . ?
C26 C25 C9 128.56(13) . . ?
C31 C32 C9 110.88(12) . . ?
C33 C32 C9 128.40(13) . . ?
C33 C32 C31 120.71(14) . . ?
N13 C37 H37A 108.9 . . ?
N13 C37 H37B 108.9 . . ?
N13 C37 C38 113.18(12) . . ?
H37A C37 H37B 107.8 . . ?
C38 C37 H37A 108.9 . . ?
C38 C37 H37B 108.9 . . ?
C55 C56 C57 122.28(13) . . ?
C68 C56 C55 119.76(13) . . ?
C68 C56 C57 117.92(13) . . ?
N61 C60 C59 108.78(12) . . ?
N61 C60 C69 129.73(14) . . ?
C69 C60 C59 121.48(14) . . ?
C20 C15 C14 119.79(13) . . ?
C20 C15 C16 119.92(13) . . ?
C16 C15 C14 120.29(14) . . ?
C80 C79 C78 108.57(13) . . ?
C84 C79 C80 120.25(15) . . ?
C84 C79 C78 131.15(15) . . ?
C56 C55 C50 121.73(13) . . ?
C56 C55 C54 118.63(13) . . ?
C54 C55 C50 119.62(13) . . ?
C58 C57 C73 109.50(12) . . ?
C58 C57 C56 111.46(11) . . ?
C58 C57 C80 112.96(11) . . ?
C56 C57 C73 110.23(11) . . ?
C80 C57 C73 100.74(11) . . ?
C80 C57 C56 111.44(12) . . ?
C3 C4 C20 119.83(13) . . ?
C5 C4 C3 119.15(13) . . ?
C5 C4 C20 121.00(13) . . ?
C15 C20 C4 118.79(13) . . ?
C15 C20 C19 117.78(13) . . ?
C19 C20 C4 123.43(14) . . ?
C55 C54 C53 119.98(13) . . ?
C66 C54 C55 119.30(13) . . ?
C66 C54 C53 120.70(13) . . ?
C53 C52 C51 119.97(13) . . ?
C53 C52 C62 119.75(13) . . ?
C62 C52 C51 120.27(14) . . ?
C52 C53 C54 118.59(13) . . ?
C52 C53 C65 118.10(13) . . ?
C65 C53 C54 123.30(14) . . ?
C79 C80 C57 110.92(13) . . ?
C81 C80 C79 120.65(14) . . ?
C81 C80 C57 128.43(13) . . ?
C21 C22 H22 119.2 . . ?
C21 C22 C23 121.54(13) . . ?
C23 C22 H22 119.2 . . ?
C12 C21 H21 121.2 . . ?
C22 C21 C12 117.50(13) . . ?
C22 C21 H21 121.2 . . ?
C50 C51 C52 123.18(14) . . ?
C50 C51 H51 118.4 . . ?
C52 C51 H51 118.4 . . ?
C56 C68 H68 119.4 . . ?
C67 C68 C56 121.25(14) . . ?
C67 C68 H68 119.4 . . ?
C32 C31 C30 108.65(12) . . ?
C36 C31 C30 131.16(14) . . ?
C36 C31 C32 120.18(15) . . ?
C32 C33 H33 120.6 . . ?
C32 C33 C34 118.78(15) . . ?
C34 C33 H33 120.6 . . ?
C8 C7 H7 119.3 . . ?
C6 C7 C8 121.33(14) . . ?
C6 C7 H7 119.3 . . ?
C15 C16 H16 119.5 . . ?
C17 C16 C15 121.05(15) . . ?
C17 C16 H16 119.5 . . ?
C73 C78 C79 108.80(13) . . ?
C77 C78 C73 120.05(15) . . ?
C77 C78 C79 131.13(15) . . ?
C24 C23 C22 121.01(13) . . ?
C24 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?
C4 C5 H5 119.5 . . ?
C6 C5 C4 121.06(14) . . ?
C6 C5 H5 119.5 . . ?
C52 C62 H62 119.6 . . ?
C63 C62 C52 120.89(15) . . ?
C63 C62 H62 119.6 . . ?
C59 C72 H72 120.6 . . ?
C71 C72 C59 118.81(14) . . ?
C71 C72 H72 120.6 . . ?
C53 C65 H65 119.5 . . ?
C64 C65 C53 121.10(15) . . ?
C64 C65 H65 119.5 . . ?
C54 C66 H66 119.5 . . ?
C67 C66 C54 120.99(14) . . ?
C67 C66 H66 119.5 . . ?
C80 C81 H81 120.5 . . ?
C80 C81 C82 118.91(15) . . ?
C82 C81 H81 120.5 . . ?
C65 C64 H64 119.7 . . ?
C65 C64 C63 120.59(14) . . ?
C63 C64 H64 119.7 . . ?
C25 C26 H26 120.6 . . ?
C25 C26 C27 118.78(14) . . ?
C27 C26 H26 120.6 . . ?
C37 C38 H38A 109.4 . . ?
C37 C38 H38B 109.4 . . ?
C37 C38 C39 111.37(13) . . ?
H38A C38 H38B 108.0 . . ?
C39 C38 H38A 109.4 . . ?
C39 C38 H38B 109.4 . . ?
C73 C74 H74 120.7 . . ?
C73 C74 C75 118.59(15) . . ?
C75 C74 H74 120.7 . . ?
C62 C63 C64 119.57(14) . . ?
C62 C63 H63 120.2 . . ?
C64 C63 H63 120.2 . . ?
C7 C6 H6 120.0 . . ?
C5 C6 C7 120.02(14) . . ?
C5 C6 H6 120.0 . . ?
C68 C67 H67 120.0 . . ?
C66 C67 C68 120.00(14) . . ?
C66 C67 H67 120.0 . . ?
C20 C19 H19 119.4 . . ?
C18 C19 C20 121.22(15) . . ?
C18 C19 H19 119.4 . . ?
C72 C71 H71 119.6 . . ?
C72 C71 C70 120.82(14) . . ?
C70 C71 H71 119.6 . . ?
H43A C43 H43B 107.6 . . ?
C44 C43 H43A 108.6 . . ?
C44 C43 H43B 108.6 . . ?
C42 C43 H43A 108.6 . . ?
C42 C43 H43B 108.6 . . ?
C42 C43 C44 114.56(13) . . ?
C60 C69 H69 121.2 . . ?
C70 C69 C60 117.66(14) . . ?
C70 C69 H69 121.2 . . ?
H40A C40 H40B 107.9 . . ?
C39 C40 H40A 109.2 . . ?
C39 C40 H40B 109.2 . . ?
C41 C40 H40A 109.2 . . ?
C41 C40 H40B 109.2 . . ?
C41 C40 C39 112.25(13) . . ?
C16 C17 H17 120.3 . . ?
C16 C17 C18 119.33(14) . . ?
C18 C17 H17 120.3 . . ?
C31 C36 H36 120.5 . . ?
C35 C36 C31 118.94(15) . . ?
C35 C36 H36 120.5 . . ?
C71 C70 H70 119.2 . . ?
C69 C70 C71 121.52(14) . . ?
C69 C70 H70 119.2 . . ?
C43 C44 H44A 108.8 . . ?
C43 C44 H44B 108.8 . . ?
H44A C44 H44B 107.7 . . ?
C45 C44 C43 113.68(14) . . ?
C45 C44 H44A 108.8 . . ?
C45 C44 H44B 108.8 . . ?
C78 C77 H77 120.6 . . ?
C76 C77 C78 118.88(15) . . ?
C76 C77 H77 120.6 . . ?
C43 C42 H42A 109.0 . . ?
C43 C42 H42B 109.0 . . ?
H42A C42 H42B 107.8 . . ?
C41 C42 C43 112.71(13) . . ?
C41 C42 H42A 109.0 . . ?
C41 C42 H42B 109.0 . . ?
C30 C29 H29 120.7 . . ?
C28 C29 C30 118.62(15) . . ?
C28 C29 H29 120.7 . . ?
H46A C46 H46B 107.7 . . ?
C45 C46 H46A 108.9 . . ?
C45 C46 H46B 108.9 . . ?
C47 C46 H46A 108.9 . . ?
C47 C46 H46B 108.9 . . ?
C47 C46 C45 113.57(14) . . ?
N61 C85 H85A 108.9 . . ?
N61 C85 H85B 108.9 . . ?
N61 C85 C86 113.51(15) . . ?
H85A C85 H85B 107.7 . . ?
C86 C85 H85A 108.9 . . ?
C86 C85 H85B 108.9 . . ?
C26 C27 H27 119.8 . . ?
C28 C27 C26 120.49(16) . . ?
C28 C27 H27 119.8 . . ?
C38 C39 H39A 108.5 . . ?
C38 C39 H39B 108.5 . . ?
C40 C39 C38 115.20(13) . . ?
C40 C39 H39A 108.5 . . ?
C40 C39 H39B 108.5 . . ?
H39A C39 H39B 107.5 . . ?
C40 C41 C42 115.47(14) . . ?
C40 C41 H41A 108.4 . . ?
C40 C41 H41B 108.4 . . ?
C42 C41 H41A 108.4 . . ?
C42 C41 H41B 108.4 . . ?
H41A C41 H41B 107.5 . . ?
C19 C18 C17 120.71(14) . . ?
C19 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C79 C84 H84 120.6 . . ?
C83 C84 C79 118.80(15) . . ?
C83 C84 H84 120.6 . . ?
H90A C90 H90B 107.7 . . ?
H90C C90 H90D 107.4 . . ?
C89 C90 H90A 108.8 . . ?
C89 C90 H90B 108.8 . . ?
C89 C90 C91 113.9(2) . . ?
C91 C90 H90A 108.8 . . ?
C91 C90 H90B 108.8 . . ?
C89A C90 H90C 108.3 . . ?
C89A C90 H90D 108.3 . . ?
C91A C90 H90C 108.3 . . ?
C91A C90 H90D 108.3 . . ?
C91A C90 C89A 116.1(3) . . ?
C36 C35 H35 119.6 . . ?
C36 C35 C34 120.80(15) . . ?
C34 C35 H35 119.6 . . ?
C44 C45 C46 115.04(14) . . ?
C44 C45 H45A 108.5 . . ?
C44 C45 H45B 108.5 . . ?
C46 C45 H45A 108.5 . . ?
C46 C45 H45B 108.5 . . ?
H45A C45 H45B 107.5 . . ?
C81 C82 H82 119.8 . . ?
C81 C82 C83 120.49(16) . . ?
C83 C82 H82 119.8 . . ?
C33 C34 H34 119.7 . . ?
C35 C34 C33 120.59(16) . . ?
C35 C34 H34 119.7 . . ?
C77 C76 H76 119.5 . . ?
C77 C76 C75 120.94(15) . . ?
C75 C76 H76 119.5 . . ?
C29 C28 C27 121.00(15) . . ?
C29 C28 H28 119.5 . . ?
C27 C28 H28 119.5 . . ?
C84 C83 C82 120.90(16) . . ?
C84 C83 H83 119.5 . . ?
C82 C83 H83 119.6 . . ?
C74 C75 H75 119.7 . . ?
C76 C75 C74 120.60(16) . . ?
C76 C75 H75 119.7 . . ?
C46 C47 H47A 108.6 . . ?
C46 C47 H47B 108.6 . . ?
C46 C47 C48 114.64(15) . . ?
H47A C47 H47B 107.6 . . ?
C48 C47 H47A 108.6 . . ?
C48 C47 H47B 108.6 . . ?
H88A C88 H88B 108.4 . . ?
H88C C88 H88D 107.7 . . ?
C87 C88 H88A 110.1 . . ?
C87 C88 H88B 110.1 . . ?
C87 C88 C89 108.2(2) . . ?
C89 C88 H88A 110.1 . . ?
C89 C88 H88B 110.1 . . ?
C87A C88 H88C 108.9 . . ?
C87A C88 H88D 108.9 . . ?
C89A C88 H88C 108.9 . . ?
C89A C88 H88D 108.9 . . ?
C89A C88 C87A 113.2(3) . . ?
H92A C92 H92B 106.0 . . ?
H92C C92 H92D 105.2 . . ?
C91 C92 H92A 105.3 . . ?
C91 C92 H92B 105.3 . . ?
C91 C92 C95 127.9(3) . . ?
C95 C92 H92A 105.3 . . ?
C95 C92 H92B 105.3 . . ?
C91A C92 H92C 103.2 . . ?
C91A C92 H92D 103.2 . . ?
C95A C92 H92C 103.2 . . ?
C95A C92 H92D 103.2 . . ?
C95A C92 C91A 136.0(3) . . ?
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 . . ?
H94A C94 H94B 107.5 . . ?
H94C C94 H94D 107.2 . . ?
C93 C94 H94A 108.5 . . ?
C93 C94 H94B 108.5 . . ?
C93 C94 C95 115.2(3) . . ?
C95 C94 H94A 108.5 . . ?
C95 C94 H94B 108.5 . . ?
C95A C94 H94C 107.9 . . ?
C95A C94 H94D 107.9 . . ?
C95A C94 C93A 117.8(3) . . ?
C93A C94 H94C 107.9 . . ?
C93A C94 H94D 107.9 . . ?
C85 C86 H86A 111.3 . . ?
C85 C86 H86B 111.3 . . ?
C85 C86 H86C 105.8 . . ?
C85 C86 H86D 105.8 . . ?
C85 C86 C87 102.5(2) . . ?
H86A C86 H86B 109.2 . . ?
H86C C86 H86D 106.2 . . ?
C87 C86 H86A 111.3 . . ?
C87 C86 H86B 111.3 . . ?
C87A C86 C85 126.0(3) . . ?
C87A C86 H86C 105.8 . . ?
C87A C86 H86D 105.8 . . ?
H96A C96 H96B 109.5 . . ?
H96A C96 H96C 109.5 . . ?
H96B C96 H96C 109.5 . . ?
H96D C96 H96E 109.5 . . ?
H96D C96 H96F 109.5 . . ?
H96E C96 H96F 109.5 . . ?
C93 C96 H96A 109.5 . . ?
C93 C96 H96B 109.5 . . ?
C93 C96 H96C 109.5 . . ?
C93A C96 H96D 109.5 . . ?
C93A C96 H96E 109.5 . . ?
C93A C96 H96F 109.5 . . ?
C88 C87 C86 107.5(3) . . ?
C88 C87 H87A 110.2 . . ?
C88 C87 H87B 110.2 . . ?
C86 C87 H87A 110.2 . . ?
C86 C87 H87B 110.2 . . ?
H87A C87 H87B 108.5 . . ?
C90 C89 C88 112.7(2) . . ?
C90 C89 H89A 109.1 . . ?
C90 C89 H89B 109.1 . . ?
C88 C89 H89A 109.1 . . ?
C88 C89 H89B 109.1 . . ?
H89A C89 H89B 107.8 . . ?
C90 C91 H91A 107.9 . . ?
C90 C91 H91B 107.9 . . ?
C92 C91 C90 117.5(3) . . ?
C92 C91 H91A 107.9 . . ?
C92 C91 H91B 107.9 . . ?
H91A C91 H91B 107.2 . . ?
C94 C93 C96 113.6(4) . . ?
C94 C93 H93A 108.8 . . ?
C94 C93 H93B 108.8 . . ?
C96 C93 H93A 108.8 . . ?
C96 C93 H93B 108.8 . . ?
H93A C93 H93B 107.7 . . ?
C92 C95 C94 111.1(3) . . ?
C92 C95 H95A 109.4 . . ?
C92 C95 H95B 109.4 . . ?
C94 C95 H95A 109.4 . . ?
C94 C95 H95B 109.4 . . ?
H95A C95 H95B 108.0 . . ?
C88 C87A H87C 108.4 . . ?
C88 C87A H87D 108.4 . . ?
C86 C87A C88 115.3(3) . . ?
C86 C87A H87C 108.4 . . ?
C86 C87A H87D 108.4 . . ?
H87C C87A H87D 107.5 . . ?
C90 C89A H89C 108.8 . . ?
C90 C89A H89D 108.8 . . ?
C88 C89A C90 113.7(3) . . ?
C88 C89A H89C 108.8 . . ?
C88 C89A H89D 108.8 . . ?
H89C C89A H89D 107.7 . . ?
C90 C91A C92 115.7(3) . . ?
C90 C91A H91C 108.4 . . ?
C90 C91A H91D 108.4 . . ?
C92 C91A H91C 108.4 . . ?
C92 C91A H91D 108.4 . . ?
H91C C91A H91D 107.4 . . ?
C92 C95A H95C 107.4 . . ?
C92 C95A H95D 107.4 . . ?
C94 C95A C92 119.7(3) . . ?
C94 C95A H95C 107.4 . . ?
C94 C95A H95D 107.4 . . ?
H95C C95A H95D 106.9 . . ?
C94 C93A H93C 109.4 . . ?
C94 C93A H93D 109.4 . . ?
C96 C93A C94 111.1(4) . . ?
C96 C93A H93C 109.4 . . ?
C96 C93A H93D 109.4 . . ?
H93C C93A H93D 108.0 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.234
_oxdiff_exptl_absorpt_empirical_full_min 0.863
####################################################################### 
# 
# 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_kato_200917
_database_code_depnum_ccdc_archive 'CCDC 2305238'
loop_
_audit_author_name
_audit_author_address
'Koji Hirano'
;Osaka University
Japan
;
_audit_update_record             
;
2023-11-02 deposited with the CCDC.	2024-01-02 downloaded from the CCDC.
;
_audit_creation_date             2020-09-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C32 H21 N)'
_chemical_formula_sum            'C64 H42 N2'
_chemical_formula_weight         838.99
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C32 N H21'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   15.7190(3)
_cell_length_b                   8.36430(10)
_cell_length_c                   33.8437(5)
_cell_angle_alpha                90
_cell_angle_beta                 101.487(2)
_cell_angle_gamma                90
_cell_volume                     4360.59(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    17855
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      74.1340
_cell_measurement_theta_min      4.3840
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45276
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.43a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1760
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-10 0 1 0.0469
-10 0 4 0.0563
10 0 1 0.0451
3 5 -11 0.1382
10 1 -4 0.0391
3 -2 -21 0.0485
-8 -1 -9 0.0597
1 2 19 0.0967
2 0 -22 0.0205
0 0 22 0.0561
4 -5 -5 0.1622
-6 -4 -2 0.1493
-1 5 4 0.1638

_exptl_crystal_size_max          0.364
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.088
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-10.0485 0.0938 0.6567 -0.0504 -0.1403 -0.9888
-10.1975 -0.0493 4.1888 0.1131 -0.1313 -0.9849
9.9383 -0.1170 0.5418 0.1049 0.1380 0.9849
2.7961 4.5932 -11.0360 -0.5772 -0.7526 0.3168
10.1450 0.5118 -3.5565 -0.0940 0.0440 0.9946
2.7848 -1.6790 -20.8202 -0.8978 0.4276 0.1057
-7.8958 -1.4702 -8.9229 -0.4406 0.2106 -0.8727
1.3073 1.8904 19.4402 0.8623 -0.4110 0.2960
2.2231 -0.0465 -21.9729 -0.9882 0.1295 0.0816
0.0169 0.2014 21.5144 0.9816 -0.1288 0.1411
3.9835 -4.9498 -4.5455 -0.0763 0.9656 0.2486
-5.7751 -4.3152 -2.1946 -0.0578 0.7234 -0.6880
-0.6053 5.3300 4.1903 0.0787 -0.9926 0.0927

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            38978
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.612
_diffrn_reflns_theta_min         3.396
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -65.00  31.00   0.50    0.46    --  -42.80  57.00   0.00  192
  2  ω     66.00  92.00   0.50    0.46    --   42.80 157.00 -78.00   52
  3  ω     76.00 101.00   0.50    1.96    --   76.50 157.00 -78.00   50
  4  ω     72.00 112.00   0.50    0.46    --   42.80 125.00  60.00   80
  5  ω     88.00 113.00   0.50    1.96    --   76.50 119.00 126.00   50
  6  ω     77.00 117.00   0.50    0.46    --   42.80 125.00  90.00   80
  7  ω     26.00  51.00   0.50    0.46    --   42.80-119.00  41.00   50
  8  ω     46.00 113.00   0.50    0.46    --   42.80-157.00-114.00  134
  9  ω     58.00  83.00   0.50    1.96    --   76.50-157.00-114.00   50
 10  ω    -85.00 -32.00   0.50    1.96    -- -106.00  77.00 150.00  106
 11  ω    -86.00 -60.00   0.50    1.96    -- -106.00  77.00  90.00   52
 12  ω   -110.00 -84.00   0.50    1.96    -- -106.00 119.00 126.00   52
 13  ω   -130.00 -94.00   0.50    1.96    -- -106.00  77.00 150.00   72
 14  ω   -134.00-109.00   0.50    1.96    -- -106.00  77.00  90.00   50
 15  ω    -68.00 -35.00   0.50    1.96    -- -106.00 125.00   0.00   66
 16  ω    -95.00 -70.00   0.50    0.46    --  -42.80 157.00 -78.00   50
 17  ω   -138.00 -33.00   0.50    1.96    -- -106.00 157.00 -78.00  210
 18  ω    -74.00 -32.00   0.50    1.96    -- -106.00 125.00-150.00   84
 19  ω    -68.00 -32.00   0.50    1.96    -- -106.00  77.00-180.00   72
 20  ω   -104.00 -78.00   0.50    1.96    -- -106.00 125.00-150.00   52
 21  ω   -131.00 -73.00   0.50    1.96    -- -106.00  77.00-180.00  116
 22  ω   -111.00 -73.00   0.50    1.96    -- -106.00 125.00   0.00   76
 23  ω   -177.00 -83.00   0.50    1.96    -- -106.00 -37.00  60.00  188
 24  ω   -135.00 -83.00   0.50    1.96    -- -106.00 -57.00  30.00  104
 25  ω   -105.00 -77.00   0.50    1.96    -- -106.00 -77.00 -30.00   56
 26  ω   -119.00 -84.00   0.50    1.96    -- -106.00 -99.00-120.00   70
 27  ω   -106.00 -81.00   0.50    0.46    --  -42.80-157.00-114.00   50
 28  ω   -116.00 -73.00   0.50    0.46    --  -42.80-125.00   0.00   86
 29  ω   -112.00 -85.00   0.50    0.46    --  -42.80-125.00 -30.00   54
 30  ω   -141.00-116.00   0.50    1.96    -- -106.00-119.00  41.00   50
 31  ω   -139.00 -70.00   0.50    1.96    -- -106.00-125.00  30.00  138
 32  ω   -110.00 -85.00   0.50    0.46    --  -42.80-125.00 120.00   50
 33  ω   -154.00-110.00   0.50    1.96    -- -106.00 -37.00  90.00   88
 34  ω   -132.00 -83.00   0.50    1.96    -- -106.00 -99.00 150.00   98
 35  ω   -159.00-125.00   0.50    1.96    -- -106.00 -77.00 -30.00   68
 36  ω   -174.00-149.00   0.50    1.96    -- -106.00-125.00  30.00   50
 37  ω   -176.00-150.00   0.50    1.96    -- -106.00 -99.00 150.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0078230000
_diffrn_orient_matrix_UB_12      -0.0203626000
_diffrn_orient_matrix_UB_13      0.0458088000
_diffrn_orient_matrix_UB_21      0.0119845000
_diffrn_orient_matrix_UB_22      -0.1814850000
_diffrn_orient_matrix_UB_23      -0.0042992000
_diffrn_orient_matrix_UB_31      0.0990354000
_diffrn_orient_matrix_UB_32      0.0237241000
_diffrn_orient_matrix_UB_33      0.0062571000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7828
_reflns_number_total             8727
_reflns_odcompleteness_completeness 99.40
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.215
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         8727
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0691
_refine_ls_restrained_S_all      1.129
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0380P)²+4.1008P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1621
_refine_ls_wR_factor_ref         0.1659
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C21, N20, C2, C3, C4, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C5A, C4A, C3A, N20A, C21A, C2A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C21 \\sim N20 \\sim C2 \\sim C3 \\sim C5 \\sim C4: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
C5A \\sim C4A \\sim C3A \\sim C2A \\sim N20A \\sim C21A: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(N20A)=Sof(C2A)=Sof(C3A)=Sof(C4A)=
 Sof(H4A)=Sof(C5A)=Sof(H5A)=1-FVAR(1)
 Sof(N20)=Sof(C3)=Sof(C2)=Sof(C5)=Sof(H5)=Sof(C4)=Sof(H4)=Sof(C21)=Sof(H21A)=
 Sof(H21B)=Sof(H21C)=FVAR(1)
 Sof(C67A)=Sof(H67D)=Sof(H67E)=Sof(H67F)=Sof(C1BB)=Sof(N66A)=Sof(C45A)=
 Sof(C46A)=Sof(H46A)=Sof(C4AB)=Sof(H4AB)=1-FVAR(2)
 Sof(N66)=Sof(C45)=Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(H67C)=Sof(C46)=Sof(H46)=
 Sof(C4AA)=Sof(H4AA)=Sof(C1BA)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C28(H28), C27(H27), C33(H33), C25(H25), C26(H26), C49(H49), C32(H32),
 C30(H30), C52(H52), C36(H36), C31(H31), C7(H7), C50(H50), C64(H64), C56(H56),
 C59(H59), C51(H51), C18(H18), C57(H57), C58(H58), C63(H63), C39(H39), C15(H15),
  C62(H62), C61(H61), C10(H10), C8(H8), C17(H17), C37(H37), C9(H9), C16(H16),
 C38(H38), C5(H5), C4(H4), C46(H46), C4AA(H4AA), C4A(H4A), C5A(H5A), C46A(H46A),
  C4AB(H4AB)
5.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C67(H67A,H67B,H67C), C21A(H21D,H21E,H21F), C67A(H67D,
 H67E,H67F)
;
_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
C24 C 0.95171(13) 0.9584(2) 0.42697(6) 0.0284(4) Uani 1 1 d . . . . .
C29 C 0.88079(13) 0.8587(2) 0.41281(6) 0.0275(4) Uani 1 1 d . . . . .
C22 C 0.86293(13) 1.0986(2) 0.37510(6) 0.0292(4) Uani 1 1 d . . . . .
C42 C 0.31297(13) 0.3974(2) 0.37172(6) 0.0281(4) Uani 1 1 d . . . . .
C23 C 0.94054(13) 1.1076(2) 0.40374(6) 0.0296(4) Uani 1 1 d . . . . .
C13 C 0.81578(13) 0.9417(2) 0.37932(6) 0.0279(4) Uani 1 1 d . . . . .
C28 C 0.87547(14) 0.7082(3) 0.42902(6) 0.0322(4) Uani 1 1 d . . . . .
H28 H 0.828702 0.641543 0.419185 0.039 Uiso 1 1 calc R . . . .
C48 C 0.28659(13) 0.3187(3) 0.40802(6) 0.0290(4) Uani 1 1 d . . . . .
C55 C 0.26861(14) 0.5602(2) 0.37115(6) 0.0316(4) Uani 1 1 d . . . . .
C53 C 0.23401(14) 0.4212(3) 0.42546(6) 0.0329(5) Uani 1 1 d . . . . .
C27 C 0.94166(15) 0.6583(3) 0.46045(6) 0.0355(5) Uani 1 1 d . . . . .
H27 H 0.939005 0.557399 0.471664 0.043 Uiso 1 1 calc R . . . .
C33 C 0.83619(15) 1.2254(3) 0.34947(6) 0.0339(5) Uani 1 1 d . . . . .
H33 H 0.784769 1.219314 0.330389 0.041 Uiso 1 1 calc R . . . .
C54 C 0.22197(14) 0.5704(3) 0.40226(6) 0.0344(5) Uani 1 1 d . . . . .
C25 C 1.01779(14) 0.9084(3) 0.45844(6) 0.0337(5) Uani 1 1 d . . . . .
H25 H 1.065024 0.974374 0.468012 0.040 Uiso 1 1 calc R . . . .
C26 C 1.01171(15) 0.7583(3) 0.47519(7) 0.0366(5) Uani 1 1 d . . . . .
H26 H 1.054822 0.724177 0.496468 0.044 Uiso 1 1 calc R . . . .
C49 C 0.30591(15) 0.1668(3) 0.42293(7) 0.0374(5) Uani 1 1 d . . . . .
H49 H 0.339984 0.098442 0.410951 0.045 Uiso 1 1 calc R . . . .
C35 C 0.21727(17) 0.1437(3) 0.27882(7) 0.0401(5) Uani 1 1 d . . . . .
C32 C 0.88731(16) 1.3621(3) 0.35263(7) 0.0401(5) Uani 1 1 d . . . . .
H32 H 0.870169 1.447858 0.335387 0.048 Uiso 1 1 calc R . . . .
C30 C 0.99145(15) 1.2447(3) 0.40677(7) 0.0384(5) Uani 1 1 d . . . . .
H30 H 1.043259 1.250827 0.425584 0.046 Uiso 1 1 calc R . . . .
C52 C 0.20230(15) 0.3713(3) 0.45910(7) 0.0421(6) Uani 1 1 d . . . . .
H52 H 0.168060 0.438990 0.471181 0.051 Uiso 1 1 calc R . . . .
C19 C 0.60566(16) 1.0356(3) 0.41491(8) 0.0433(6) Uani 1 1 d . . . . .
C65 C 0.55945(16) 0.4598(3) 0.38661(7) 0.0410(5) Uani 1 1 d . . . . .
C36 C 0.14652(17) 0.0660(3) 0.25497(7) 0.0437(6) Uani 1 1 d . . . . .
H36 H 0.153952 0.005283 0.232883 0.052 Uiso 1 1 calc R . . . .
C31 C 0.96371(16) 1.3719(3) 0.38130(8) 0.0421(5) Uani 1 1 d . . . . .
H31 H 0.996649 1.464997 0.383420 0.050 Uiso 1 1 calc R . . . .
C7 C 0.8270(2) 0.5941(3) 0.25715(7) 0.0474(6) Uani 1 1 d . . . . .
H7 H 0.794081 0.535760 0.236148 0.057 Uiso 1 1 calc R . . . .
C50 C 0.27323(17) 0.1179(3) 0.45640(7) 0.0467(6) Uani 1 1 d . . . . .
H50 H 0.285630 0.015776 0.466826 0.056 Uiso 1 1 calc R . . . .
C40 C 0.2052(2) 0.2370(3) 0.31228(7) 0.0506(7) Uani 1 1 d . . . . .
C64 C 0.63595(16) 0.5278(3) 0.40758(7) 0.0426(5) Uani 1 1 d . . . . .
H64 H 0.687765 0.512920 0.398752 0.051 Uiso 1 1 calc R . . . .
C1 C 0.72854(15) 0.9705(3) 0.39084(8) 0.0460(6) Uani 1 1 d . . . . .
C41 C 0.28528(19) 0.3004(3) 0.33346(6) 0.0433(6) Uani 1 1 d . . . . .
C43 C 0.41005(15) 0.4062(3) 0.37365(9) 0.0470(6) Uani 1 1 d . . . . .
C56 C 0.26988(18) 0.6873(3) 0.34519(7) 0.0428(6) Uani 1 1 d . . . . .
H56 H 0.301990 0.682330 0.324918 0.051 Uiso 1 1 calc R . . . .
C59 C 0.17416(17) 0.7068(3) 0.40674(8) 0.0462(6) Uani 1 1 d . . . . .
H59 H 0.142449 0.713226 0.427137 0.055 Uiso 1 1 calc R . . . .
N20 N 0.5859(3) 0.9467(5) 0.38250(13) 0.0365(9) Uani 0.646(5) 1 d . U P A 1
C12 C 0.7882(2) 0.8438(3) 0.34136(7) 0.0533(8) Uani 1 1 d . . . . .
C14 C 0.69810(17) 1.0569(3) 0.42189(9) 0.0523(7) Uani 1 1 d . . . . .
C51 C 0.22275(17) 0.2192(3) 0.47419(7) 0.0475(6) Uani 1 1 d . . . . .
H51 H 0.202110 0.184885 0.496673 0.057 Uiso 1 1 calc R . . . .
C6 C 0.7854(2) 0.6804(3) 0.28364(7) 0.0488(7) Uani 1 1 d . . . . .
C60 C 0.47993(16) 0.4830(3) 0.39971(10) 0.0540(7) Uani 1 1 d . . . . .
C18 C 0.55884(18) 1.1066(3) 0.44093(9) 0.0523(7) Uani 1 1 d . . . . .
H18 H 0.499184 1.091463 0.437351 0.063 Uiso 1 1 calc R . . . .
C57 C 0.2216(2) 0.8236(3) 0.35020(8) 0.0550(7) Uani 1 1 d . . . . .
H57 H 0.221247 0.909832 0.332824 0.066 Uiso 1 1 calc R . . . .
C58 C 0.17465(19) 0.8323(3) 0.38044(9) 0.0556(7) Uani 1 1 d . . . . .
H58 H 0.142865 0.924032 0.383108 0.067 Uiso 1 1 calc R . . . .
C11 C 0.8350(3) 0.7701(3) 0.31543(7) 0.0573(8) Uani 1 1 d . . . . .
C63 C 0.63424(19) 0.6156(3) 0.44093(8) 0.0523(7) Uani 1 1 d . . . . .
H63 H 0.685223 0.661922 0.454874 0.063 Uiso 1 1 calc R . . . .
C39 C 0.1224(3) 0.2509(4) 0.32078(9) 0.0668(9) Uani 1 1 d . . . . .
H39 H 0.113386 0.313332 0.342319 0.080 Uiso 1 1 calc R . . . .
C3 C 0.6883(3) 0.8254(5) 0.33636(16) 0.0300(9) Uani 0.646(5) 1 d . U P A 1
C15 C 0.7385(2) 1.1523(4) 0.45433(11) 0.0657(9) Uani 1 1 d . . . . .
H15 H 0.798335 1.167141 0.459281 0.079 Uiso 1 1 calc R . . . .
C62 C 0.5567(3) 0.6379(4) 0.45485(10) 0.0667(9) Uani 1 1 d . . . . .
H62 H 0.557139 0.697999 0.478010 0.080 Uiso 1 1 calc R . . . .
C61 C 0.4800(2) 0.5719(4) 0.43463(11) 0.0678(9) Uani 1 1 d . . . . .
H61 H 0.428919 0.586375 0.444115 0.081 Uiso 1 1 calc R . . . .
C10 C 0.9244(3) 0.7743(3) 0.31912(8) 0.0708(11) Uani 1 1 d . . . . .
H10 H 0.957427 0.836491 0.339287 0.085 Uiso 1 1 calc R . . . .
C8 C 0.9151(2) 0.5957(4) 0.26210(9) 0.0597(8) Uani 1 1 d . . . . .
H8 H 0.942357 0.536340 0.244974 0.072 Uiso 1 1 calc R . . . .
C17 C 0.6015(2) 1.1986(4) 0.47171(9) 0.0653(8) Uani 1 1 d . . . . .
H17 H 0.569736 1.246988 0.488858 0.078 Uiso 1 1 calc R . . . .
C2 C 0.6624(3) 0.9107(5) 0.36921(15) 0.0297(9) Uani 0.646(5) 1 d . U P A 1
C37 C 0.0663(2) 0.0801(4) 0.26443(9) 0.0607(8) Uani 1 1 d . . . . .
H37 H 0.019104 0.027827 0.248829 0.073 Uiso 1 1 calc R . . . .
N66 N 0.5321(3) 0.3763(5) 0.35450(13) 0.0315(11) Uani 0.474(5) 1 d . . P B -1
C9 C 0.9654(2) 0.6886(4) 0.29367(10) 0.0722(10) Uani 1 1 d . . . . .
H9 H 1.025534 0.691241 0.297026 0.087 Uiso 1 1 calc R . . . .
C45 C 0.3764(6) 0.2666(7) 0.32114(19) 0.0232(13) Uani 0.474(5) 1 d . . P B -1
C16 C 0.6901(3) 1.2231(4) 0.47851(10) 0.0726(10) Uani 1 1 d . . . . .
H16 H 0.716645 1.288214 0.499681 0.087 Uiso 1 1 calc R . . . .
C38 C 0.0545(2) 0.1723(4) 0.29728(12) 0.0744(10) Uani 1 1 d . . . . .
H38 H -0.000519 0.180326 0.303285 0.089 Uiso 1 1 calc R . . . .
C5 C 0.6866(4) 0.6629(6) 0.27750(15) 0.0405(10) Uani 0.646(5) 1 d . U P A 1
H5 H 0.656673 0.603255 0.255964 0.049 Uiso 0.646(5) 1 calc R . P A 1
C4 C 0.6424(2) 0.7346(4) 0.30359(11) 0.0380(9) Uani 0.646(5) 1 d . U P A 1
H4 H 0.582410 0.723887 0.299865 0.046 Uiso 0.646(5) 1 calc R . P A 1
C21 C 0.4987(3) 0.8920(5) 0.36470(13) 0.0441(10) Uani 0.646(5) 1 d . U P A 1
H21A H 0.470556 0.853922 0.385596 0.066 Uiso 0.646(5) 1 calc GR . P A 1
H21B H 0.502078 0.807051 0.346019 0.066 Uiso 0.646(5) 1 calc GR . P A 1
H21C H 0.465926 0.979161 0.350770 0.066 Uiso 0.646(5) 1 calc GR . P A 1
C67 C 0.5922(3) 0.3137(7) 0.33070(18) 0.0362(12) Uani 0.474(5) 1 d . . P B -1
H67A H 0.637528 0.390235 0.330297 0.054 Uiso 0.474(5) 1 calc GR . P B -1
H67B H 0.561635 0.293886 0.303647 0.054 Uiso 0.474(5) 1 calc GR . P B -1
H67C H 0.617062 0.215688 0.342473 0.054 Uiso 0.474(5) 1 calc GR . P B -1
C46 C 0.3795(3) 0.1719(5) 0.28677(13) 0.0341(12) Uani 0.474(5) 1 d . . P B -1
H46 H 0.431956 0.152466 0.278919 0.041 Uiso 0.474(5) 1 calc R . P B -1
C4AA C 0.3036(4) 0.1094(8) 0.2653(2) 0.0363(13) Uani 0.474(5) 1 d . . P B -1
H4AA H 0.304122 0.046588 0.242662 0.044 Uiso 0.474(5) 1 calc R . P B -1
C1BA C 0.4454(4) 0.3478(8) 0.3500(2) 0.0283(13) Uani 0.474(5) 1 d . . P B -1
C21A C 0.6385(8) 0.6411(13) 0.2674(3) 0.072(3) Uani 0.354(5) 1 d . U P A 2
H21D H 0.624122 0.701004 0.242806 0.108 Uiso 0.354(5) 1 calc GR . P A 2
H21E H 0.591644 0.648071 0.281707 0.108 Uiso 0.354(5) 1 calc GR . P A 2
H21F H 0.647976 0.531205 0.261343 0.108 Uiso 0.354(5) 1 calc GR . P A 2
N20A N 0.7181(6) 0.7071(8) 0.2927(2) 0.047(2) Uani 0.354(5) 1 d . U P A 2
C2A C 0.7250(7) 0.8047(10) 0.3257(3) 0.0384(18) Uani 0.354(5) 1 d . U P A 2
C3A C 0.6689(6) 0.8698(11) 0.3520(3) 0.0326(19) Uani 0.354(5) 1 d . U P A 2
C4A C 0.5796(4) 0.8620(9) 0.3499(2) 0.048(2) Uani 0.354(5) 1 d . U P A 2
H4A H 0.543704 0.806194 0.329311 0.058 Uiso 0.354(5) 1 calc R . P A 2
C5A C 0.5469(7) 0.9390(13) 0.3789(3) 0.050(3) Uani 0.354(5) 1 d . U P A 2
H5A H 0.487288 0.935193 0.377725 0.060 Uiso 0.354(5) 1 calc R . P A 2
C67A C 0.3487(5) 0.0642(7) 0.25650(16) 0.0533(14) Uani 0.526(5) 1 d . . P B -2
H67D H 0.346070 -0.047582 0.262589 0.080 Uiso 0.526(5) 1 calc GR . P B -2
H67E H 0.408228 0.098354 0.261675 0.080 Uiso 0.526(5) 1 calc GR . P B -2
H67F H 0.323297 0.081861 0.228627 0.080 Uiso 0.526(5) 1 calc GR . P B -2
C1BB C 0.3363(4) 0.2490(7) 0.31461(19) 0.0287(12) Uani 0.526(5) 1 d . . P B -2
N66A N 0.3011(3) 0.1552(5) 0.28174(14) 0.0343(11) Uani 0.526(5) 1 d . . P B -2
C45A C 0.4215(5) 0.3065(7) 0.3351(2) 0.0267(12) Uani 0.526(5) 1 d . . P B -2
C46A C 0.5040(3) 0.2884(5) 0.32492(13) 0.0387(11) Uani 0.526(5) 1 d . . P B -2
H46A H 0.511386 0.229545 0.302530 0.046 Uiso 0.526(5) 1 calc R . P B -2
C4AB C 0.5726(4) 0.3618(7) 0.34958(18) 0.0393(12) Uani 0.526(5) 1 d . . P B -2
H4AB H 0.627985 0.352383 0.343960 0.047 Uiso 0.526(5) 1 calc R . 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
C24 C29 1.398(3) . ?
C24 C23 1.467(3) . ?
C24 C25 1.396(3) . ?
C29 C13 1.533(3) . ?
C29 C28 1.382(3) . ?
C22 C23 1.401(3) . ?
C22 C13 1.528(3) . ?
C22 C33 1.381(3) . ?
C42 C48 1.522(3) . ?
C42 C55 1.528(3) . ?
C42 C41 1.516(3) . ?
C42 C43 1.516(3) . ?
C23 C30 1.390(3) . ?
C13 C1 1.518(3) . ?
C13 C12 1.512(3) . ?
C28 H28 0.9300 . ?
C28 C27 1.395(3) . ?
C48 C53 1.400(3) . ?
C48 C49 1.378(3) . ?
C55 C54 1.400(3) . ?
C55 C56 1.382(3) . ?
C53 C54 1.467(3) . ?
C53 C52 1.395(3) . ?
C27 H27 0.9300 . ?
C27 C26 1.393(3) . ?
C33 H33 0.9300 . ?
C33 C32 1.390(3) . ?
C54 C59 1.391(3) . ?
C25 H25 0.9300 . ?
C25 C26 1.389(3) . ?
C26 H26 0.9300 . ?
C49 H49 0.9300 . ?
C49 C50 1.395(3) . ?
C35 C36 1.398(3) . ?
C35 C40 1.419(3) . ?
C35 C4AA 1.543(8) . ?
C35 N66A 1.305(5) . ?
C32 H32 0.9300 . ?
C32 C31 1.388(4) . ?
C30 H30 0.9300 . ?
C30 C31 1.384(3) . ?
C52 H52 0.9300 . ?
C52 C51 1.385(4) . ?
C19 N20 1.310(5) . ?
C19 C14 1.436(4) . ?
C19 C18 1.388(4) . ?
C19 C5A 1.594(12) . ?
C65 C64 1.390(3) . ?
C65 C60 1.420(4) . ?
C65 N66 1.291(5) . ?
C65 C4AB 1.546(7) . ?
C36 H36 0.9300 . ?
C36 C37 1.366(4) . ?
C31 H31 0.9300 . ?
C7 H7 0.9300 . ?
C7 C6 1.409(4) . ?
C7 C8 1.361(4) . ?
C50 H50 0.9300 . ?
C50 C51 1.379(4) . ?
C40 C41 1.422(4) . ?
C40 C39 1.392(5) . ?
C64 H64 0.9300 . ?
C64 C63 1.351(4) . ?
C1 C14 1.433(4) . ?
C1 C2 1.251(5) . ?
C1 C3A 1.680(9) . ?
C41 C45 1.594(8) . ?
C41 C1BB 1.200(7) . ?
C43 C60 1.418(4) . ?
C43 C1BA 1.169(7) . ?
C43 C45A 1.589(7) . ?
C56 H56 0.9300 . ?
C56 C57 1.398(4) . ?
C59 H59 0.9300 . ?
C59 C58 1.377(4) . ?
N20 C2 1.397(6) . ?
N20 C21 1.457(5) . ?
C12 C11 1.396(4) . ?
C12 C3 1.554(6) . ?
C12 C2A 1.080(9) . ?
C12 C3A 1.991(12) . ?
C14 C15 1.403(5) . ?
C51 H51 0.9300 . ?
C6 C11 1.412(4) . ?
C6 C5 1.533(7) . ?
C6 N20A 1.180(9) . ?
C60 C61 1.396(5) . ?
C60 C1BA 2.011(8) . ?
C18 H18 0.9300 . ?
C18 C17 1.360(5) . ?
C57 H57 0.9300 . ?
C57 C58 1.378(4) . ?
C58 H58 0.9300 . ?
C11 C10 1.386(5) . ?
C11 N20A 1.919(10) . ?
C11 C2A 1.854(12) . ?
C63 H63 0.9300 . ?
C63 C62 1.404(4) . ?
C39 H39 0.9300 . ?
C39 C38 1.366(5) . ?
C3 C2 1.446(6) . ?
C3 C4 1.417(6) . ?
C15 H15 0.9300 . ?
C15 C16 1.360(5) . ?
C62 H62 0.9300 . ?
C62 C61 1.378(5) . ?
C61 H61 0.9300 . ?
C10 H10 0.9300 . ?
C10 C9 1.375(5) . ?
C8 H8 0.9300 . ?
C8 C9 1.426(5) . ?
C17 H17 0.9300 . ?
C17 C16 1.380(5) . ?
C37 H37 0.9300 . ?
C37 C38 1.395(5) . ?
N66 C67 1.455(7) . ?
N66 C1BA 1.362(9) . ?
C9 H9 0.9300 . ?
C45 C46 1.416(8) . ?
C45 C1BA 1.472(8) . ?
C16 H16 0.9300 . ?
C38 H38 0.9300 . ?
C5 H5 0.9300 . ?
C5 C4 1.367(6) . ?
C4 H4 0.9300 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C67 H67A 0.9600 . ?
C67 H67B 0.9600 . ?
C67 H67C 0.9600 . ?
C46 H46 0.9300 . ?
C46 C4AA 1.371(8) . ?
C4AA H4AA 0.9300 . ?
C21A H21D 0.9600 . ?
C21A H21E 0.9600 . ?
C21A H21F 0.9600 . ?
C21A N20A 1.474(11) . ?
N20A C2A 1.372(12) . ?
C2A C3A 1.476(13) . ?
C3A C4A 1.392(12) . ?
C4A H4A 0.9300 . ?
C4A C5A 1.359(14) . ?
C5A H5A 0.9300 . ?
C67A H67D 0.9600 . ?
C67A H67E 0.9600 . ?
C67A H67F 0.9600 . ?
C67A N66A 1.457(7) . ?
C1BB N66A 1.384(9) . ?
C1BB C45A 1.461(8) . ?
C45A C46A 1.415(7) . ?
C46A H46A 0.9300 . ?
C46A C4AB 1.370(7) . ?
C4AB H4AB 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C29 C24 C23 108.76(17) . . ?
C25 C24 C29 120.29(19) . . ?
C25 C24 C23 130.94(19) . . ?
C24 C29 C13 110.59(17) . . ?
C28 C29 C24 120.94(19) . . ?
C28 C29 C13 128.47(19) . . ?
C23 C22 C13 110.70(17) . . ?
C33 C22 C23 120.48(19) . . ?
C33 C22 C13 128.71(19) . . ?
C48 C42 C55 101.47(16) . . ?
C41 C42 C48 112.30(17) . . ?
C41 C42 C55 114.41(18) . . ?
C43 C42 C48 114.82(18) . . ?
C43 C42 C55 114.20(18) . . ?
C43 C42 C41 100.2(2) . . ?
C22 C23 C24 108.64(18) . . ?
C30 C23 C24 131.0(2) . . ?
C30 C23 C22 120.3(2) . . ?
C22 C13 C29 101.19(16) . . ?
C1 C13 C29 112.67(17) . . ?
C1 C13 C22 111.58(17) . . ?
C12 C13 C29 114.74(18) . . ?
C12 C13 C22 116.61(18) . . ?
C12 C13 C1 100.6(2) . . ?
C29 C28 H28 120.7 . . ?
C29 C28 C27 118.7(2) . . ?
C27 C28 H28 120.7 . . ?
C53 C48 C42 110.71(18) . . ?
C49 C48 C42 128.2(2) . . ?
C49 C48 C53 121.0(2) . . ?
C54 C55 C42 110.51(18) . . ?
C56 C55 C42 129.0(2) . . ?
C56 C55 C54 120.5(2) . . ?
C48 C53 C54 108.63(18) . . ?
C52 C53 C48 119.9(2) . . ?
C52 C53 C54 131.5(2) . . ?
C28 C27 H27 119.7 . . ?
C26 C27 C28 120.6(2) . . ?
C26 C27 H27 119.7 . . ?
C22 C33 H33 120.5 . . ?
C22 C33 C32 119.0(2) . . ?
C32 C33 H33 120.5 . . ?
C55 C54 C53 108.66(19) . . ?
C59 C54 C55 120.4(2) . . ?
C59 C54 C53 130.9(2) . . ?
C24 C25 H25 120.6 . . ?
C26 C25 C24 118.8(2) . . ?
C26 C25 H25 120.6 . . ?
C27 C26 H26 119.7 . . ?
C25 C26 C27 120.7(2) . . ?
C25 C26 H26 119.7 . . ?
C48 C49 H49 120.7 . . ?
C48 C49 C50 118.5(2) . . ?
C50 C49 H49 120.7 . . ?
C36 C35 C40 119.9(3) . . ?
C36 C35 C4AA 112.8(3) . . ?
C40 C35 C4AA 127.2(3) . . ?
N66A C35 C36 138.8(3) . . ?
N66A C35 C40 101.1(3) . . ?
C33 C32 H32 119.7 . . ?
C31 C32 C33 120.6(2) . . ?
C31 C32 H32 119.7 . . ?
C23 C30 H30 120.6 . . ?
C31 C30 C23 118.9(2) . . ?
C31 C30 H30 120.6 . . ?
C53 C52 H52 120.6 . . ?
C51 C52 C53 118.8(2) . . ?
C51 C52 H52 120.6 . . ?
N20 C19 C14 105.7(3) . . ?
N20 C19 C18 135.0(3) . . ?
C14 C19 C5A 127.0(5) . . ?
C18 C19 C14 119.3(3) . . ?
C18 C19 C5A 113.7(5) . . ?
C64 C65 C60 120.7(3) . . ?
C64 C65 C4AB 112.9(3) . . ?
C60 C65 C4AB 126.4(3) . . ?
N66 C65 C64 139.4(3) . . ?
N66 C65 C60 99.8(3) . . ?
C35 C36 H36 120.3 . . ?
C37 C36 C35 119.3(2) . . ?
C37 C36 H36 120.3 . . ?
C32 C31 H31 119.6 . . ?
C30 C31 C32 120.8(2) . . ?
C30 C31 H31 119.6 . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C8 C7 C6 120.4(3) . . ?
C49 C50 H50 119.6 . . ?
C51 C50 C49 120.8(2) . . ?
C51 C50 H50 119.6 . . ?
C35 C40 C41 111.2(3) . . ?
C39 C40 C35 119.4(3) . . ?
C39 C40 C41 129.4(2) . . ?
C65 C64 H64 120.4 . . ?
C63 C64 C65 119.3(2) . . ?
C63 C64 H64 120.4 . . ?
C13 C1 C3A 96.4(5) . . ?
C14 C1 C13 136.0(2) . . ?
C14 C1 C3A 127.6(5) . . ?
C2 C1 C13 118.3(3) . . ?
C2 C1 C14 105.7(3) . . ?
C42 C41 C45 101.4(3) . . ?
C40 C41 C42 134.8(2) . . ?
C40 C41 C45 123.6(4) . . ?
C1BB C41 C42 122.5(4) . . ?
C1BB C41 C40 102.5(4) . . ?
C42 C43 C45A 102.5(3) . . ?
C60 C43 C42 134.2(3) . . ?
C60 C43 C45A 123.3(4) . . ?
C1BA C43 C42 124.2(4) . . ?
C1BA C43 C60 101.6(4) . . ?
C55 C56 H56 120.9 . . ?
C55 C56 C57 118.2(2) . . ?
C57 C56 H56 120.9 . . ?
C54 C59 H59 120.6 . . ?
C58 C59 C54 118.8(2) . . ?
C58 C59 H59 120.6 . . ?
C19 N20 C2 108.4(4) . . ?
C19 N20 C21 124.8(4) . . ?
C2 N20 C21 126.7(4) . . ?
C13 C12 C3 105.0(3) . . ?
C13 C12 C3A 84.7(3) . . ?
C11 C12 C13 132.5(3) . . ?
C11 C12 C3 122.4(3) . . ?
C11 C12 C3A 142.7(4) . . ?
C2A C12 C13 131.3(6) . . ?
C2A C12 C11 96.1(6) . . ?
C2A C12 C3A 46.7(6) . . ?
C1 C14 C19 107.0(3) . . ?
C15 C14 C19 119.0(3) . . ?
C15 C14 C1 134.0(3) . . ?
C52 C51 H51 119.5 . . ?
C50 C51 C52 121.0(2) . . ?
C50 C51 H51 119.5 . . ?
C7 C6 C11 120.1(3) . . ?
C7 C6 C5 116.8(3) . . ?
C11 C6 C5 123.0(3) . . ?
N20A C6 C7 144.6(5) . . ?
N20A C6 C11 95.1(5) . . ?
C65 C60 C1BA 76.7(3) . . ?
C43 C60 C65 111.4(3) . . ?
C43 C60 C1BA 34.7(2) . . ?
C61 C60 C65 119.0(3) . . ?
C61 C60 C43 129.6(3) . . ?
C61 C60 C1BA 164.3(3) . . ?
C19 C18 H18 120.5 . . ?
C17 C18 C19 119.0(3) . . ?
C17 C18 H18 120.5 . . ?
C56 C57 H57 119.4 . . ?
C58 C57 C56 121.1(2) . . ?
C58 C57 H57 119.4 . . ?
C59 C58 C57 120.8(2) . . ?
C59 C58 H58 119.6 . . ?
C57 C58 H58 119.6 . . ?
C12 C11 C6 115.7(3) . . ?
C12 C11 N20A 78.0(3) . . ?
C12 C11 C2A 35.4(3) . . ?
C6 C11 N20A 37.8(3) . . ?
C6 C11 C2A 80.4(3) . . ?
C10 C11 C12 125.7(3) . . ?
C10 C11 C6 118.5(3) . . ?
C10 C11 N20A 156.3(3) . . ?
C10 C11 C2A 161.1(3) . . ?
C2A C11 N20A 42.6(4) . . ?
C64 C63 H63 119.5 . . ?
C64 C63 C62 121.1(3) . . ?
C62 C63 H63 119.5 . . ?
C40 C39 H39 120.2 . . ?
C38 C39 C40 119.5(3) . . ?
C38 C39 H39 120.2 . . ?
C2 C3 C12 107.5(4) . . ?
C4 C3 C12 119.0(5) . . ?
C4 C3 C2 133.5(5) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 C14 119.9(3) . . ?
C16 C15 H15 120.1 . . ?
C63 C62 H62 119.6 . . ?
C61 C62 C63 120.8(3) . . ?
C61 C62 H62 119.6 . . ?
C60 C61 H61 120.4 . . ?
C62 C61 C60 119.1(3) . . ?
C62 C61 H61 120.4 . . ?
C11 C10 H10 119.2 . . ?
C9 C10 C11 121.5(3) . . ?
C9 C10 H10 119.2 . . ?
C7 C8 H8 120.1 . . ?
C7 C8 C9 119.7(3) . . ?
C9 C8 H8 120.1 . . ?
C18 C17 H17 118.7 . . ?
C18 C17 C16 122.6(3) . . ?
C16 C17 H17 118.7 . . ?
C1 C2 N20 113.2(4) . . ?
C1 C2 C3 108.6(4) . . ?
N20 C2 C3 138.2(5) . . ?
C36 C37 H37 119.7 . . ?
C36 C37 C38 120.6(3) . . ?
C38 C37 H37 119.7 . . ?
C65 N66 C67 121.1(4) . . ?
C65 N66 C1BA 110.3(5) . . ?
C1BA N66 C67 128.3(5) . . ?
C10 C9 C8 119.6(3) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C46 C45 C41 119.6(7) . . ?
C46 C45 C1BA 131.4(6) . . ?
C1BA C45 C41 109.1(5) . . ?
C15 C16 C17 120.1(3) . . ?
C15 C16 H16 119.9 . . ?
C17 C16 H16 119.9 . . ?
C39 C38 C37 121.2(3) . . ?
C39 C38 H38 119.4 . . ?
C37 C38 H38 119.4 . . ?
C6 C5 H5 119.9 . . ?
C4 C5 C6 120.2(5) . . ?
C4 C5 H5 119.9 . . ?
C3 C4 H4 120.1 . . ?
C5 C4 C3 119.7(5) . . ?
C5 C4 H4 120.1 . . ?
N20 C21 H21A 109.5 . . ?
N20 C21 H21B 109.5 . . ?
N20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N66 C67 H67A 109.5 . . ?
N66 C67 H67B 109.5 . . ?
N66 C67 H67C 109.5 . . ?
H67A C67 H67B 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C45 C46 H46 120.6 . . ?
C4AA C46 C45 118.7(6) . . ?
C4AA C46 H46 120.6 . . ?
C35 C4AA H4AA 120.2 . . ?
C46 C4AA C35 119.7(6) . . ?
C46 C4AA H4AA 120.2 . . ?
C43 C1BA C60 43.7(3) . . ?
C43 C1BA N66 116.8(6) . . ?
C43 C1BA C45 105.0(5) . . ?
N66 C1BA C60 73.1(4) . . ?
N66 C1BA C45 138.1(6) . . ?
C45 C1BA C60 148.7(5) . . ?
H21D C21A H21E 109.5 . . ?
H21D C21A H21F 109.5 . . ?
H21E C21A H21F 109.5 . . ?
N20A C21A H21D 109.5 . . ?
N20A C21A H21E 109.5 . . ?
N20A C21A H21F 109.5 . . ?
C6 N20A C11 47.1(4) . . ?
C6 N20A C21A 118.7(8) . . ?
C6 N20A C2A 113.2(8) . . ?
C21A N20A C11 165.8(8) . . ?
C2A N20A C11 66.2(6) . . ?
C2A N20A C21A 128.0(10) . . ?
C12 C2A C11 48.5(5) . . ?
C12 C2A N20A 119.7(11) . . ?
C12 C2A C3A 101.2(7) . . ?
N20A C2A C11 71.3(6) . . ?
N20A C2A C3A 138.8(9) . . ?
C3A C2A C11 149.6(6) . . ?
C1 C3A C12 78.3(3) . . ?
C2A C3A C1 110.5(6) . . ?
C2A C3A C12 32.1(4) . . ?
C4A C3A C1 117.7(10) . . ?
C4A C3A C12 164.0(9) . . ?
C4A C3A C2A 131.9(9) . . ?
C3A C4A H4A 121.2 . . ?
C5A C4A C3A 117.6(9) . . ?
C5A C4A H4A 121.2 . . ?
C19 C5A H5A 118.4 . . ?
C4A C5A C19 123.2(8) . . ?
C4A C5A H5A 118.4 . . ?
H67D C67A H67E 109.5 . . ?
H67D C67A H67F 109.5 . . ?
H67E C67A H67F 109.5 . . ?
N66A C67A H67D 109.5 . . ?
N66A C67A H67E 109.5 . . ?
N66A C67A H67F 109.5 . . ?
C41 C1BB N66A 115.3(6) . . ?
C41 C1BB C45A 106.0(5) . . ?
N66A C1BB C45A 138.6(6) . . ?
C35 N66A C67A 123.1(4) . . ?
C35 N66A C1BB 109.8(5) . . ?
C1BB N66A C67A 126.7(5) . . ?
C1BB C45A C43 108.6(5) . . ?
C46A C45A C43 121.0(6) . . ?
C46A C45A C1BB 130.4(6) . . ?
C45A C46A H46A 121.5 . . ?
C4AB C46A C45A 116.9(6) . . ?
C4AB C46A H46A 121.5 . . ?
C65 C4AB H4AB 119.5 . . ?
C46A C4AB C65 121.0(6) . . ?
C46A C4AB H4AB 119.5 . . ?

_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
;
_oxdiff_exptl_absorpt_empirical_full_max 3.164
_oxdiff_exptl_absorpt_empirical_full_min 0.458
####################################################################### 
# 
# 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_kato_201027_2
_database_code_depnum_ccdc_archive 'CCDC 2305240'
loop_
_audit_author_name
_audit_author_address
'Koji Hirano'
;Osaka University
Japan
;
_audit_update_record             
;
2023-11-02 deposited with the CCDC.	2024-01-02 downloaded from the CCDC.
;
_audit_creation_date             2020-10-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C72 H76 N2)'
_chemical_formula_sum            'C18 H19 N0.50'
_chemical_formula_weight         242.34
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C17 H18 N2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   15.0249(2)
_cell_length_b                   11.65340(10)
_cell_length_c                   16.3566(2)
_cell_angle_alpha                90
_cell_angle_beta                 97.3120(10)
_cell_angle_gamma                90
_cell_volume                     2840.61(6)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    25676
_cell_measurement_temperature    263(2)
_cell_measurement_theta_max      73.8440
_cell_measurement_theta_min      3.7420
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.484
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62426
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.43a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1044
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-10 0 -1 0.0205
10 0 1 0.1061
0 -6 -6 0.0861
0 0 10 0.1412
0 7 4 0.1532
0 0 -10 0.1181

_exptl_crystal_size_max          0.482
_exptl_crystal_size_mid          0.275
_exptl_crystal_size_min          0.129
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-9.5715 -0.1918 -0.6710 -0.0785 0.9936 0.0816
9.5596 0.2947 0.7144 0.0784 -0.9923 -0.0957
-0.1173 -6.1663 -6.0879 -0.3115 0.0410 0.9494
0.3172 0.3385 10.4698 0.9337 -0.1227 -0.3364
0.0548 6.8994 4.3178 0.1230 -0.0162 -0.9923
-0.3252 0.3937 -10.4642 -0.9616 0.1264 0.2438

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            54897
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.170
_diffrn_reflns_theta_min         4.672
_diffrn_ambient_temperature      263(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_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    -42.00 -17.00   0.50    0.13    --  -42.93  22.00-102.00   50
  2  ω    -86.00 -60.00   0.50    0.13    --  -42.93 -22.00  91.00   52
  3  ω     15.00  40.00   0.50    0.13    --   42.93 -22.00  91.00   50
  4  ω     16.00  79.00   0.50    0.13    --   42.93  22.00-102.00  126
  5  ω     82.00 108.00   0.50    0.48    --   76.50  22.00-102.00   52
  6  ω     27.00  52.00   0.50    0.48    --   76.50 -22.00  91.00   50
  7  ω    -55.00 -30.00   0.50    0.48    -- -106.00  22.00-102.00   50
  8  ω   -127.00 -93.00   0.50    0.48    -- -106.00 -22.00  91.00   68
  9  ω    -93.00 -12.00   0.50    0.13    --  -42.93 125.00 -30.00  162
 10  ω   -115.00 -70.00   0.50    0.13    --  -42.93-125.00-120.00   90
 11  ω     94.00 120.00   0.50    0.13    --   42.93  37.00 -30.00   52
 12  ω     65.00  91.00   0.50    0.13    --   42.93  37.00 -30.00   52
 13  ω     16.00  74.00   0.50    0.13    --   42.93  77.00 -30.00  116
 14  ω     16.00 116.00   0.50    0.13    --   42.93  77.00  30.00  200
 15  ω     29.00  60.00   0.50    0.13    --   42.93  37.00 -30.00   62
 16  ω     49.00  87.00   0.50    0.48    --   76.50  77.00 -60.00   76
 17  ω     48.00  84.00   0.50    0.48    --   76.50  77.00 -30.00   72
 18  ω     49.00  75.00   0.50    0.48    --   76.50  77.00  60.00   52
 19  ω     48.00 136.00   0.50    0.48    --   76.50  77.00  90.00  176
 20  ω     48.00  73.00   0.50    0.48    --   76.50  77.00  30.00   50
 21  ω     48.00 140.00   0.50    0.48    --   76.50  77.00   0.00  184
 22  ω     52.00  92.00   0.50    0.48    --   76.50  67.00  63.12   80
 23  ω     54.00  80.00   0.50    0.48    --   76.50  57.00  60.00   52
 24  ω    -99.00 -74.00   0.50    0.48    -- -106.00 -83.00 -11.83   50
 25  ω   -175.00-149.00   0.50    0.48    -- -106.00 -83.00 -11.83   52
 26  ω   -128.00 -80.00   0.50    0.48    -- -106.00  37.00  90.00   96
 27  ω   -100.00 -75.00   0.50    0.48    -- -106.00 -81.00  51.78   50
 28  ω   -135.00 -84.00   0.50    0.48    -- -106.00  77.00  30.00  102
 29  ω   -176.00-137.00   0.50    0.48    -- -106.00 -81.00  51.78   78
 30  ω    -76.00 -41.00   0.50    0.48    -- -106.00 125.00 -90.00   70
 31  ω   -119.00 -80.00   0.50    0.48    -- -106.00 -70.00  44.16   78
 32  ω    -78.00 -52.00   0.50    0.48    -- -106.00  77.00  30.00   52
 33  ω   -176.00 -82.00   0.50    0.48    -- -106.00 -69.00 -16.86  188
 34  ω   -175.00 -77.00   0.50    0.48    -- -106.00 -77.00  60.00  196
 35  ω   -173.00 -82.00   0.50    0.48    -- -106.00 -65.00  24.26  182
 36  ω   -106.00 -77.00   0.50    0.48    -- -106.00 -79.00  35.95   58
 37  ω   -177.00-151.00   0.50    0.48    -- -106.00 -77.00   0.00   52
 38  ω   -113.00 -79.00   0.50    0.48    -- -106.00 -77.00   0.00   68
 39  ω   -102.00 -77.00   0.50    0.48    -- -106.00 -76.00 -37.73   50
 40  ω   -101.00 -76.00   0.50    0.48    -- -106.00 -79.00 -22.45   50
 41  ω   -156.00-130.00   0.50    0.48    -- -106.00 -76.00 -37.73   52
 42  ω   -125.00 -42.00   0.50    0.48    -- -106.00  57.00-120.00  166
 43  ω   -107.00 -78.00   0.50    0.48    -- -106.00 -75.00  17.43   58
 44  ω   -167.00 -80.00   0.50    0.48    -- -106.00 -71.00   3.31  174
 45  ω   -166.00-128.00   0.50    0.48    -- -106.00 -77.00  90.00   76
 46  ω   -147.00-110.00   0.50    0.48    -- -106.00 -75.00  17.43   74
 47  ω   -177.00 -93.00   0.50    0.48    -- -106.00 -99.00  90.00  168
 48  ω   -109.00 -50.00   0.50    0.48    -- -106.00  37.00  30.00  118
 49  ω   -168.00 -79.00   0.50    0.48    -- -106.00 -72.00 -72.33  178
 50  ω   -173.00-147.00   0.50    0.48    -- -106.00 -79.00 -22.45   52
 51  ω   -102.00 -77.00   0.50    0.48    -- -106.00 -79.00  28.86   50
 52  ω    -80.00 -35.00   0.50    0.48    -- -106.00 125.00-150.00   90
 53  ω   -112.00 -87.00   0.50    0.48    -- -106.00 125.00 -30.00   50
 54  ω    -66.00 -41.00   0.50    0.48    -- -106.00 125.00 -30.00   50
 55  ω   -170.00-144.00   0.50    0.48    -- -106.00 -79.00  28.86   52
 56  ω   -126.00 -81.00   0.50    0.48    -- -106.00 -75.00 -42.88   90
 57  ω   -103.00 -78.00   0.50    0.48    -- -106.00 -77.00 -30.00   50
 58  ω   -177.00-108.00   0.50    0.48    -- -106.00 -89.00 -36.55  138
 59  ω   -101.00 -76.00   0.50    0.48    -- -106.00 -89.00 -36.55   50
 60  ω   -170.00-145.00   0.50    0.48    -- -106.00 -84.00  73.94   50
 61  ω   -102.00 -77.00   0.50    0.48    -- -106.00 -84.00  73.94   50
 62  ω   -103.00 -77.00   0.50    0.48    -- -106.00 -77.00 -60.00   52
 63  ω   -149.00-113.00   0.50    0.48    -- -106.00 -77.00 -60.00   72
 64  ω   -114.00 -75.00   0.50    0.48    -- -106.00 125.00-120.00   78
 65  ω    -71.00 -40.00   0.50    0.48    -- -106.00  37.00  90.00   62
 66  ω   -104.00 -79.00   0.50    0.48    -- -106.00 -74.00  48.18   50
 67  ω   -103.00 -78.00   0.50    0.48    -- -106.00 -74.00   0.45   50
 68  ω   -103.00 -78.00   0.50    0.48    -- -106.00 -74.00 -18.07   50
 69  ω   -104.00 -79.00   0.50    0.48    -- -106.00 -77.00  17.44   50
 70  ω   -101.00 -76.00   0.50    0.48    -- -106.00 -89.00  74.68   50
 71  ω   -125.00 -34.00   0.50    0.48    -- -106.00  57.00  90.00  182
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0026383000
_diffrn_orient_matrix_UB_12      -0.0387312000
_diffrn_orient_matrix_UB_13      0.0903505000
_diffrn_orient_matrix_UB_21      -0.1032730000
_diffrn_orient_matrix_UB_22      0.0039229000
_diffrn_orient_matrix_UB_23      -0.0087193000
_diffrn_orient_matrix_UB_31      -0.0040326000
_diffrn_orient_matrix_UB_32      -0.1263099000
_diffrn_orient_matrix_UB_33      -0.0279267000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5029
_reflns_number_total             5760
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.213
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.037
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         5760
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0530
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0791P)²+0.3871P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1437
_refine_ls_wR_factor_ref         0.1500
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C0AA) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C9)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
3. Others
 Sof(H00C)=Sof(H00D)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C5)=Sof(H5A)=Sof(H5B)=
 Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8A)=Sof(H8B)=
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C0AA)=Sof(H0AB)=
 Sof(H0AC)=Sof(H0AD)=1-FVAR(1)
 Sof(H00A)=Sof(H00B)=Sof(C00R)=Sof(H00H)=Sof(H00R)=Sof(C00S)=Sof(H00S)=
 Sof(H00T)=Sof(C00T)=Sof(H00U)=Sof(H00V)=Sof(C00U)=Sof(H00W)=Sof(H00X)=
 Sof(C00V)=Sof(H00Y)=Sof(H)=Sof(C00W)=Sof(H00Z)=Sof(HA)=Sof(C00X)=Sof(H00)=
 Sof(HB)=Sof(C00Y)=Sof(H0AA)=Sof(HC)=Sof(C00Z)=Sof(H1AA)=Sof(HD)=Sof(C010)=
 Sof(H01A)=Sof(H01B)=Sof(C011)=Sof(H01C)=Sof(H01D)=Sof(H01E)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C00H(H00A,H00B), C00H(H00C,H00D), C00R(H00H,H00R), C00S(H00S,H00T), C00T(H00U,
 H00V), C00U(H00W,H00X), C00V(H00Y,H), C00W(H00Z,HA), C00X(H00,HB), C00Y(H0AA,
 HC), C00Z(H1AA,HD), C010(H01A,H01B), C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B),
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B),
 C11(H11A,H11B)
4.b Aromatic/amide H refined with riding coordinates:
 C004(H004), C00E(H00E), C00F(H00F), C00G(H00G), C00I(H00I), C00J(H00J),
 C00K(H00K), C00L(H00L), C00M(H00M), C00N(H00N), C00O(H00O), C00P(H00P),
 C00Q(H00Q)
4.c Idealised Me refined as rotating group:
 C011(H01C,H01D,H01E), C0AA(H0AB,H0AC,H0AD)
;
_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
N001 N 0.82491(7) 0.45545(8) 0.43570(7) 0.0546(3) Uani 1 1 d . . . . .
C002 C 1.05905(7) 0.41584(9) 0.53634(6) 0.0438(2) Uani 1 1 d . . . . .
C003 C 0.91458(8) 0.46615(9) 0.47000(6) 0.0455(3) Uani 1 1 d . . . . .
C004 C 0.97197(8) 0.38211(9) 0.50579(6) 0.0457(3) Uani 1 1 d . . . . .
H004 H 0.953299 0.306390 0.509348 0.055 Uiso 1 1 calc R . . . .
C005 C 0.86346(8) 0.64156(10) 0.42407(7) 0.0487(3) Uani 1 1 d . . . . .
C006 C 0.79653(8) 0.56256(10) 0.40843(8) 0.0547(3) Uani 1 1 d . . . . .
C007 C 0.83198(8) 0.75897(10) 0.39373(7) 0.0509(3) Uani 1 1 d . . . . .
C008 C 0.84184(9) 0.85716(10) 0.45594(7) 0.0540(3) Uani 1 1 d . . . . .
C009 C 0.88120(8) 0.80805(11) 0.32525(7) 0.0536(3) Uani 1 1 d . . . . .
C00A C 0.73325(9) 0.73281(12) 0.36282(8) 0.0591(3) Uani 1 1 d . . . . .
C00B C 0.71342(9) 0.61555(12) 0.37092(9) 0.0631(3) Uani 1 1 d . . . . .
C00C C 0.90989(10) 0.91945(11) 0.34398(8) 0.0605(3) Uani 1 1 d . . . . .
C00D C 0.88547(10) 0.95034(10) 0.42505(8) 0.0600(3) Uani 1 1 d . . . . .
C00E C 0.81233(11) 0.86358(13) 0.53239(8) 0.0672(4) Uani 1 1 d . . . . .
H00E H 0.783388 0.801732 0.553420 0.081 Uiso 1 1 calc R . . . .
C00F C 0.89686(10) 0.75687(13) 0.25191(8) 0.0654(4) Uani 1 1 d . . . . .
H00F H 0.877817 0.682203 0.239581 0.078 Uiso 1 1 calc R . . . .
C00G C 0.66718(10) 0.80895(15) 0.33197(10) 0.0753(4) Uani 1 1 d . . . . .
H00G H 0.680328 0.886344 0.326508 0.090 Uiso 1 1 calc R . . . .
C00H C 0.77762(11) 0.34697(12) 0.42234(12) 0.0809(5) Uani 1 1 d . . . . .
H00A H 0.791092 0.302213 0.472387 0.097 Uiso 0.641(4) 1 calc R . P A 1
H00B H 0.713913 0.363900 0.416524 0.097 Uiso 0.641(4) 1 calc R . P A 1
H00C H 0.714011 0.354610 0.426260 0.097 Uiso 0.359(4) 1 calc R . P A 2
H00D H 0.803229 0.287708 0.459829 0.097 Uiso 0.359(4) 1 calc R . P A 2
C00I C 0.87051(14) 1.05653(14) 0.54688(11) 0.0837(5) Uani 1 1 d . . . . .
H00I H 0.879808 1.123252 0.577991 0.100 Uiso 1 1 calc R . . . .
C00J C 0.82699(13) 0.96517(14) 0.57735(10) 0.0809(5) Uani 1 1 d . . . . .
H00J H 0.807015 0.971167 0.628712 0.097 Uiso 1 1 calc R . . . .
C00K C 0.90045(13) 1.05039(12) 0.47095(10) 0.0760(4) Uani 1 1 d . . . . .
H00K H 0.930202 1.112128 0.450682 0.091 Uiso 1 1 calc R . . . .
C00L C 0.94135(13) 0.81889(16) 0.19734(10) 0.0805(5) Uani 1 1 d . . . . .
H00L H 0.952574 0.785359 0.148081 0.097 Uiso 1 1 calc R . . . .
C00M C 0.96915(14) 0.92965(17) 0.21525(10) 0.0892(5) Uani 1 1 d . . . . .
H00M H 0.998239 0.970386 0.177571 0.107 Uiso 1 1 calc R . . . .
C00N C 0.95440(13) 0.98121(14) 0.28856(10) 0.0818(5) Uani 1 1 d . . . . .
H00N H 0.973862 1.055787 0.300614 0.098 Uiso 1 1 calc R . . . .
C00O C 0.62675(11) 0.57593(16) 0.34737(12) 0.0867(5) Uani 1 1 d . . . . .
H00O H 0.612831 0.498670 0.352221 0.104 Uiso 1 1 calc R . . . .
C00P C 0.56150(12) 0.65412(19) 0.31648(15) 0.1042(7) Uani 1 1 d . . . . .
H00P H 0.503290 0.628519 0.300313 0.125 Uiso 1 1 calc R . . . .
C00Q C 0.58085(12) 0.76842(19) 0.30923(14) 0.0970(6) Uani 1 1 d . . . . .
H00Q H 0.535633 0.819181 0.288857 0.116 Uiso 1 1 calc R . . . .
C00R C 0.79247(18) 0.2751(2) 0.35574(17) 0.0668(7) Uani 0.641(4) 1 d . . P A 1
H00H H 0.768069 0.199559 0.364027 0.080 Uiso 0.641(4) 1 calc R . P A 1
H00R H 0.856504 0.266994 0.354335 0.080 Uiso 0.641(4) 1 calc R . P A 1
C00S C 0.7490(3) 0.3233(2) 0.27358(18) 0.0864(9) Uani 0.641(4) 1 d . . P A 1
H00S H 0.684644 0.328046 0.274566 0.104 Uiso 0.641(4) 1 calc R . P A 1
H00T H 0.771001 0.400654 0.267247 0.104 Uiso 0.641(4) 1 calc R . P A 1
C00T C 0.6127(4) -0.0758(4) 0.1007(3) 0.0958(12) Uani 0.641(4) 1 d . . P A 1
H00U H 0.588101 -0.055777 0.150785 0.115 Uiso 0.641(4) 1 calc R . P A 1
H00V H 0.584249 -0.027259 0.056738 0.115 Uiso 0.641(4) 1 calc R . P A 1
C00U C 0.5905(3) -0.2014(5) 0.0794(3) 0.0950(11) Uani 0.641(4) 1 d . . P A 1
H00W H 0.614605 -0.220201 0.028779 0.114 Uiso 0.641(4) 1 calc R . P A 1
H00X H 0.621014 -0.249328 0.122680 0.114 Uiso 0.641(4) 1 calc R . P A 1
C00V C 0.7275(2) 0.1337(3) 0.19955(18) 0.0840(9) Uani 0.641(4) 1 d . . P A 1
H00Y H 0.663556 0.138670 0.202418 0.101 Uiso 0.641(4) 1 calc R . P A 1
H H 0.754711 0.091979 0.247657 0.101 Uiso 0.641(4) 1 calc R . P A 1
C00W C 0.4931(5) -0.2315(5) 0.0688(3) 0.1097(14) Uani 0.641(4) 1 d . . P A 1
H00Z H 0.461684 -0.184014 0.025680 0.132 Uiso 0.641(4) 1 calc R . P A 1
HA H 0.468469 -0.215141 0.119573 0.132 Uiso 0.641(4) 1 calc R . P A 1
C00X C 0.7666(3) 0.2536(3) 0.2007(2) 0.0991(11) Uani 0.641(4) 1 d . . P A 1
H00 H 0.830959 0.247874 0.200226 0.119 Uiso 0.641(4) 1 calc R . P A 1
HB H 0.741744 0.293287 0.150874 0.119 Uiso 0.641(4) 1 calc R . P A 1
C00Y C 0.7146(3) -0.0519(4) 0.1128(2) 0.0968(10) Uani 0.641(4) 1 d . . P A 1
H0AA H 0.740555 -0.092184 0.161990 0.116 Uiso 0.641(4) 1 calc R . P A 1
HC H 0.739832 -0.085393 0.066582 0.116 Uiso 0.641(4) 1 calc R . P A 1
C00Z C 0.7437(3) 0.0669(3) 0.1203(2) 0.1002(11) Uani 0.641(4) 1 d . . P A 1
H1AA H 0.713869 0.108497 0.073219 0.120 Uiso 0.641(4) 1 calc R . P A 1
HD H 0.807504 0.068793 0.116235 0.120 Uiso 0.641(4) 1 calc R . P A 1
C010 C 0.4775(4) -0.3569(6) 0.0466(5) 0.146(2) Uani 0.641(4) 1 d . . P A 1
H01A H 0.504462 -0.372995 -0.002954 0.175 Uiso 0.641(4) 1 calc R . P A 1
H01B H 0.508245 -0.403508 0.090579 0.175 Uiso 0.641(4) 1 calc R . P A 1
C011 C 0.3823(5) -0.3925(8) 0.0328(8) 0.178(4) Uani 0.641(4) 1 d . . P A 1
H01C H 0.377143 -0.463553 0.002909 0.267 Uiso 0.641(4) 1 calc GR . P A 1
H01D H 0.347602 -0.334475 0.001554 0.267 Uiso 0.641(4) 1 calc GR . P A 1
H01E H 0.360319 -0.402439 0.084937 0.267 Uiso 0.641(4) 1 calc GR . P A 1
C1 C 0.8001(5) 0.3211(5) 0.3150(4) 0.0871(16) Uani 0.359(4) 1 d . . P A 2
H1A H 0.775202 0.383547 0.280116 0.105 Uiso 0.359(4) 1 calc R . P A 2
H1B H 0.864404 0.319512 0.313339 0.105 Uiso 0.359(4) 1 calc R . P A 2
C2 C 0.7603(5) 0.2109(5) 0.2827(4) 0.119(3) Uani 0.359(4) 1 d . . P A 2
H2A H 0.695353 0.217187 0.275321 0.143 Uiso 0.359(4) 1 calc R . P A 2
H2B H 0.777017 0.150348 0.322352 0.143 Uiso 0.359(4) 1 calc R . P A 2
C3 C 0.7947(6) 0.1773(10) 0.1940(4) 0.122(3) Uani 0.359(4) 1 d . . P A 2
H3A H 0.773072 0.231912 0.151287 0.147 Uiso 0.359(4) 1 calc R . P A 2
H3B H 0.859650 0.173604 0.198838 0.147 Uiso 0.359(4) 1 calc R . P A 2
C4 C 0.6863(5) 0.0400(12) 0.1417(5) 0.150(5) Uani 0.359(4) 1 d . U P A 2
H4A H 0.677279 0.094230 0.096424 0.180 Uiso 0.359(4) 1 calc R . P A 2
H4B H 0.641353 0.056758 0.177725 0.180 Uiso 0.359(4) 1 calc R . P A 2
C5 C 0.7520(18) 0.0575(12) 0.1762(8) 0.325(14) Uani 0.359(4) 1 d . U P A 2
H5A H 0.794700 0.014309 0.148682 0.390 Uiso 0.359(4) 1 calc R . P A 2
H5B H 0.751269 0.021547 0.229637 0.390 Uiso 0.359(4) 1 calc R . P A 2
C6 C 0.5760(8) -0.1224(14) 0.0804(7) 0.133(3) Uani 0.359(4) 1 d . . P A 2
H6A H 0.551863 -0.070956 0.036503 0.160 Uiso 0.359(4) 1 calc R . P A 2
H6B H 0.544647 -0.105538 0.127327 0.160 Uiso 0.359(4) 1 calc R . P A 2
C7 C 0.4210(16) -0.354(2) 0.003(2) 0.35(2) Uani 0.359(4) 1 d . U P A 2
H7A H 0.454685 -0.387085 -0.037650 0.415 Uiso 0.359(4) 1 calc R . P A 2
H7B H 0.358302 -0.345986 -0.019200 0.415 Uiso 0.359(4) 1 calc R . P A 2
C8 C 0.6650(10) -0.0916(11) 0.1026(7) 0.144(4) Uani 0.359(4) 1 d . . P A 2
H8A H 0.695699 -0.099005 0.054120 0.172 Uiso 0.359(4) 1 calc R . P A 2
H8B H 0.691709 -0.146874 0.142724 0.172 Uiso 0.359(4) 1 calc R . P A 2
C9 C 0.5508(13) -0.2366(12) 0.0540(10) 0.169(6) Uani 0.359(4) 1 d . U P A 2
H9A H 0.573595 -0.289574 0.097392 0.203 Uiso 0.359(4) 1 calc R . P A 2
H9B H 0.580197 -0.254599 0.006074 0.203 Uiso 0.359(4) 1 calc R . P A 2
C11 C 0.4559(14) -0.257(3) 0.0333(19) 0.317(17) Uani 0.359(4) 1 d . U P A 2
H11A H 0.428954 -0.241901 0.083103 0.381 Uiso 0.359(4) 1 calc R . P A 2
H11B H 0.434004 -0.197502 -0.005732 0.381 Uiso 0.359(4) 1 calc R . P A 2
C0AA C 0.435(2) -0.4245(18) 0.0920(14) 0.270(12) Uani 0.359(4) 1 d . U P A 2
H0AB H 0.497776 -0.430458 0.111324 0.406 Uiso 0.359(4) 1 calc GR . P A 2
H0AC H 0.409631 -0.499921 0.084073 0.406 Uiso 0.359(4) 1 calc GR . P A 2
H0AD H 0.405303 -0.383928 0.131951 0.406 Uiso 0.359(4) 1 calc GR . 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
N001 C003 1.3976(15) . ?
N001 C006 1.3750(16) . ?
N001 C00H 1.4530(16) . ?
C002 C003 1.4386(15) 3_766 ?
C002 C004 1.3963(16) . ?
C002 C005 1.4250(16) 3_766 ?
C003 C004 1.3844(16) . ?
C005 C006 1.3634(17) . ?
C005 C007 1.5106(15) . ?
C006 C00B 1.4567(18) . ?
C007 C008 1.5259(17) . ?
C007 C009 1.5296(16) . ?
C007 C00A 1.5356(18) . ?
C008 C00D 1.3959(18) . ?
C008 C00E 1.3809(18) . ?
C009 C00C 1.3897(18) . ?
C009 C00F 1.3862(18) . ?
C00A C00B 1.4085(19) . ?
C00A C00G 1.3783(19) . ?
C00B C00O 1.389(2) . ?
C00C C00D 1.4651(18) . ?
C00C C00N 1.3934(19) . ?
C00D C00K 1.3894(19) . ?
C00E C00J 1.396(2) . ?
C00F C00L 1.385(2) . ?
C00G C00Q 1.386(2) . ?
C00H C00R 1.414(3) . ?
C00H C1 1.855(6) . ?
C00I C00J 1.376(3) . ?
C00I C00K 1.376(2) . ?
C00L C00M 1.377(3) . ?
C00M C00N 1.384(2) . ?
C00O C00P 1.386(3) . ?
C00P C00Q 1.372(3) . ?
C00R C00S 1.525(4) . ?
C00S C00X 1.494(5) . ?
C00T C00U 1.531(6) . ?
C00T C00Y 1.543(6) . ?
C00U C00W 1.493(8) . ?
C00V C00X 1.514(5) . ?
C00V C00Z 1.558(5) . ?
C00W C010 1.517(8) . ?
C00Y C00Z 1.452(6) . ?
C010 C011 1.478(10) . ?
C1 C2 1.485(8) . ?
C2 C3 1.648(11) . ?
C3 C5 1.549(18) . ?
C4 C5 1.09(2) . ?
C4 C8 1.677(17) . ?
C6 C8 1.387(13) . ?
C6 C9 1.435(17) . ?
C7 C11 1.31(4) . ?
C7 C0AA 1.66(4) . ?
C9 C11 1.44(2) . ?

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
C003 N001 C00H 124.47(11) . . ?
C006 N001 C003 107.02(9) . . ?
C006 N001 C00H 127.99(11) . . ?
C004 C002 C003 119.83(10) . 3_766 ?
C004 C002 C005 134.80(10) . 3_766 ?
C005 C002 C003 105.37(10) 3_766 3_766 ?
N001 C003 C002 108.45(9) . 3_766 ?
C004 C003 N001 128.56(10) . . ?
C004 C003 C002 122.98(10) . 3_766 ?
C003 C004 C002 117.19(10) . . ?
C002 C005 C007 141.08(11) 3_766 . ?
C006 C005 C002 107.98(10) . 3_766 ?
C006 C005 C007 110.94(11) . . ?
N001 C006 C00B 137.33(12) . . ?
C005 C006 N001 111.17(11) . . ?
C005 C006 C00B 111.41(11) . . ?
C005 C007 C008 117.41(10) . . ?
C005 C007 C009 114.77(10) . . ?
C005 C007 C00A 100.21(10) . . ?
C008 C007 C009 101.13(10) . . ?
C008 C007 C00A 112.09(10) . . ?
C009 C007 C00A 111.71(10) . . ?
C00D C008 C007 110.62(11) . . ?
C00E C008 C007 129.01(12) . . ?
C00E C008 C00D 120.35(12) . . ?
C00C C009 C007 110.68(10) . . ?
C00F C009 C007 128.60(12) . . ?
C00F C009 C00C 120.71(12) . . ?
C00B C00A C007 111.64(11) . . ?
C00G C00A C007 127.83(13) . . ?
C00G C00A C00B 120.52(14) . . ?
C00A C00B C006 105.70(11) . . ?
C00O C00B C006 134.35(14) . . ?
C00O C00B C00A 119.90(13) . . ?
C009 C00C C00D 108.83(11) . . ?
C009 C00C C00N 120.01(13) . . ?
C00N C00C C00D 131.16(14) . . ?
C008 C00D C00C 108.64(11) . . ?
C00K C00D C008 120.57(13) . . ?
C00K C00D C00C 130.78(13) . . ?
C008 C00E C00J 118.40(14) . . ?
C00L C00F C009 118.83(14) . . ?
C00A C00G C00Q 118.99(16) . . ?
N001 C00H C1 98.0(2) . . ?
C00R C00H N001 120.59(18) . . ?
C00J C00I C00K 120.80(15) . . ?
C00I C00J C00E 121.05(14) . . ?
C00I C00K C00D 118.83(15) . . ?
C00M C00L C00F 120.69(15) . . ?
C00L C00M C00N 120.92(14) . . ?
C00M C00N C00C 118.84(16) . . ?
C00P C00O C00B 118.51(17) . . ?
C00Q C00P C00O 121.47(17) . . ?
C00P C00Q C00G 120.61(16) . . ?
C00H C00R C00S 111.6(2) . . ?
C00X C00S C00R 113.7(3) . . ?
C00U C00T C00Y 112.7(4) . . ?
C00W C00U C00T 115.6(4) . . ?
C00X C00V C00Z 111.7(3) . . ?
C00U C00W C010 111.9(5) . . ?
C00S C00X C00V 113.8(3) . . ?
C00Z C00Y C00T 117.8(4) . . ?
C00Y C00Z C00V 118.0(3) . . ?
C011 C010 C00W 115.1(5) . . ?
C2 C1 C00H 111.3(5) . . ?
C1 C2 C3 111.2(6) . . ?
C5 C3 C2 102.2(10) . . ?
C5 C4 C8 118.9(13) . . ?
C4 C5 C3 126.2(15) . . ?
C8 C6 C9 121.8(16) . . ?
C11 C7 C0AA 96(3) . . ?
C6 C8 C4 117.8(14) . . ?
C6 C9 C11 116(2) . . ?
C7 C11 C9 124(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.416
_oxdiff_exptl_absorpt_empirical_full_min 0.534
####################################################################### 
# 
# 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_kato_210209_1
_database_code_depnum_ccdc_archive 'CCDC 2305245'
loop_
_audit_author_name
_audit_author_address
'Koji Hirano'
;Osaka University
Japan
;
_audit_update_record             
;
2023-11-02 deposited with the CCDC.	2024-01-02 downloaded from the CCDC.
;
_audit_creation_date             2021-02-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C26 H21)'
_chemical_formula_sum            'C52 H42'
_chemical_formula_weight         666.85
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C52 H42'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   12.0253(5)
_cell_length_b                   14.2850(8)
_cell_length_c                   15.2395(6)
_cell_angle_alpha                63.792(5)
_cell_angle_beta                 67.462(4)
_cell_angle_gamma                77.789(4)
_cell_volume                     2166.5(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    10135
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      73.8600
_cell_measurement_theta_min      3.7680
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88352
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.43a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.022
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             708
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
6 -3 4 0.0505
-2 -9 -7 0.0533
-5 -6 -9 0.0524
-6 4 -3 0.0874
5 7 9 0.0301
2 0 -7 0.0076
-2 -1 7 0.0396
2 6 -3 0.0324
7 -2 0 0.0299
0 -1 -9 0.0076

_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.049
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
6.2819 -2.7418 4.2746 0.8506 -0.2043 0.4845
-1.7991 -8.7916 -6.8823 -0.3464 0.0826 0.9344
-5.4588 -6.0328 -8.6865 -0.8295 0.1987 0.5220
-5.8467 3.8884 -3.1889 -0.7773 0.1868 -0.6008
4.6150 7.1299 8.5429 0.7230 -0.1731 -0.6688
2.3514 0.0078 -7.0615 -0.4185 -0.8777 0.2337
-2.3408 -0.5187 6.8814 0.4235 0.8882 -0.1781
1.5770 6.3747 -2.8900 -0.3669 -0.7698 -0.5223
6.9346 -1.6932 -0.1839 0.4943 -0.7190 0.4887
0.0188 -0.9104 -8.6928 -0.6664 -0.7022 0.2508

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32393
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.217
_diffrn_reflns_theta_min         3.425
_diffrn_ambient_temperature      273(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -35.00  65.00   0.50    1.72    --   42.80 -37.00 120.00  200
  2  ω     62.00  92.00   0.50    1.72    --   42.80-117.00   3.00   60
  3  ω     34.00  59.00   0.50    7.06    --   76.50-117.00   3.00   50
  4  ω    -10.00  61.00   0.50    1.72    --   42.80 -57.00  60.00  142
  5  ω     54.00 126.00   0.50    7.06    --   76.50  37.00 -90.00  144
  6  ω     69.00  97.00   0.50    1.72    --   42.80 161.00-118.00   56
  7  ω     75.00 100.00   0.50    7.06    --   76.50 161.00-118.00   50
  8  ω    103.00 150.00   0.50    7.06    --   76.50 117.00  90.00   94
  9  ω     79.00 116.00   0.50    1.72    --   42.80 125.00 120.00   74
 10  ω     72.00 116.00   0.50    1.72    --   42.80 125.00 150.00   88
 11  ω    -58.00 -29.00   0.50    7.06    -- -106.00  37.00 120.00   58
 12  ω    -72.00 -47.00   0.50    1.72    --  -42.80 117.00  90.00   50
 13  ω   -112.00 -84.00   0.50    7.06    -- -106.00 117.00  90.00   56
 14  ω   -113.00 -32.00   0.50    7.06    -- -106.00 125.00 120.00  162
 15  ω   -115.00 -54.00   0.50    7.06    -- -106.00 125.00 150.00  122
 16  ω   -123.00 -97.00   0.50    7.06    -- -106.00  37.00 120.00   52
 17  ω   -123.00 -33.00   0.50    7.06    -- -106.00  77.00 120.00  180
 18  ω   -114.00 -51.00   0.50    7.06    -- -106.00 125.00   0.00  126
 19  ω   -103.00 -50.00   0.50    7.06    -- -106.00  77.00 -30.00  106
 20  ω    -93.00 -32.00   0.50    7.06    -- -106.00  57.00 -60.00  122
 21  ω    -85.00 -42.00   0.50    7.06    -- -106.00 125.00-180.00   86
 22  ω    -98.00 -73.00   0.50    1.72    --  -42.80 161.00-118.00   50
 23  ω   -121.00 -78.00   0.50    7.06    -- -106.00 161.00-118.00   86
 24  ω   -117.00 -33.00   0.50    7.06    -- -106.00 125.00-150.00  168
 25  ω   -112.00 -33.00   0.50    7.06    -- -106.00 125.00 -60.00  158
 26  ω   -125.00 -27.00   0.50    7.06    -- -106.00  19.00-120.00  196
 27  ω   -121.00 -95.00   0.50    7.06    -- -106.00 -57.00-150.00   52
 28  ω   -130.00 -84.00   0.50    7.06    -- -106.00 -37.00-150.00   92
 29  ω   -142.00-116.00   0.50    7.06    -- -106.00 -57.00 -90.00   52
 30  ω   -156.00 -93.00   0.50    7.06    -- -106.00 -99.00 -30.00  126
 31  ω   -141.00-115.00   0.50    7.06    -- -106.00 -37.00  60.00   52
 32  ω   -159.00-126.00   0.50    7.06    -- -106.00-117.00   3.00   66
 33  ω   -167.00-125.00   0.50    7.06    -- -106.00-125.00  60.00   84
 34  ω   -174.00 -83.00   0.50    7.06    -- -106.00 -57.00  60.00  182
 35  ω   -108.00 -70.00   0.50    1.72    --  -42.80-125.00  60.00   76
 36  ω   -115.00 -73.00   0.50    1.72    --  -42.80-125.00  90.00   84
 37  ω   -176.00 -89.00   0.50    7.06    -- -106.00 -37.00 -60.00  174
 38  ω   -112.00 -32.00   0.50    7.06    -- -106.00  57.00  30.00  160
 39  ω   -120.00 -63.00   0.50    7.06    -- -106.00  57.00 120.00  114
 40  ω   -117.00 -91.00   0.50    7.06    -- -106.00 125.00 -90.00   52
 41  ω   -116.00 -62.00   0.50    7.06    -- -106.00  57.00-150.00  108
 42  ω   -169.00-144.00   0.50    7.06    -- -106.00 -57.00-150.00   50
 43  ω   -171.00 -75.00   0.50    7.06    -- -106.00 -19.00 -30.00  192
 44  ω   -103.00 -76.00   0.50    1.72    --  -42.80-161.00-147.00   54
 45  ω     50.00  75.00   0.50    1.72    --   42.80-161.00-147.00   50
 46  ω     60.00  85.00   0.50    7.06    --   76.50-161.00-147.00   50
 47  ω   -127.00-102.00   0.50    7.06    -- -106.00-161.00-147.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0643990000
_diffrn_orient_matrix_UB_12      -0.0369213000
_diffrn_orient_matrix_UB_13      0.0806631000
_diffrn_orient_matrix_UB_21      -0.1144327000
_diffrn_orient_matrix_UB_22      -0.0534026000
_diffrn_orient_matrix_UB_23      0.0861241000
_diffrn_orient_matrix_UB_31      0.0452419000
_diffrn_orient_matrix_UB_32      -0.1013470000
_diffrn_orient_matrix_UB_33      -0.0181377000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6871
_reflns_number_total             8698
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         8698
_refine_ls_number_restraints     214
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0539
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0984P)²+0.1584P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1612
_refine_ls_wR_factor_ref         0.1699
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C0, C1AA, C2AA, C3AA, C4AA, C5AA, C2, C6AA, C3, C7AA, C8AA, C9AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C00L, C00Q, C00W, C010, C014, C019, C01B, C01D, C01F, C01G, C01H, C01I
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C0 \\sim C1AA \\sim C2AA \\sim C3AA \\sim C4AA \\sim C5AA \\sim C2 \\sim C6AA
\\sim C3 \\sim C7AA \\sim C8AA \\sim C9AA: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C00L \\sim C00Q \\sim C00W \\sim C010 \\sim C014 \\sim C019 \\sim C01B \\sim
C01D \\sim C01F \\sim C01G \\sim C01H \\sim C01I: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
4. Others
 Sof(C0)=Sof(H0)=Sof(C1AA)=Sof(H1AA)=Sof(C2AA)=Sof(H2AA)=Sof(C3AA)=Sof(H3AA)=
 Sof(C4AA)=Sof(C5AA)=Sof(C2)=Sof(C6AA)=Sof(C3)=Sof(H3)=Sof(C7AA)=Sof(H7AA)=
 Sof(C8AA)=Sof(H8AA)=Sof(C9AA)=Sof(H9AA)=1-FVAR(1)
 Sof(C00L)=Sof(C00Q)=Sof(C00W)=Sof(C010)=Sof(C014)=Sof(H014)=Sof(C019)=
 Sof(H019)=Sof(C01B)=Sof(H01J)=Sof(C01D)=Sof(H01K)=Sof(C01F)=Sof(H01L)=
 Sof(C01G)=Sof(H01M)=Sof(C01H)=Sof(H01N)=Sof(C01I)=Sof(H01O)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C007(H007), C008(H008), C009(H009), C00E(H00E), C00J(H00J), C00M(H00M),
 C00O(H00O), C00P(H00P), C00R(H00R), C00U(H00U), C00V(H00V), C00X(H00X),
 C00Y(H00Y), C00Z(H00Z), C013(H013), C014(H014), C016(H016), C019(H019),
 C01B(H01J), C01D(H01K), C01F(H01L), C01G(H01M), C01H(H01N), C01I(H01O), C0(H0),
  C1AA(H1AA), C2AA(H2AA), C3AA(H3AA), C3(H3), C7AA(H7AA), C8AA(H8AA), C9AA(H9AA)
5.b Idealised Me refined as rotating group:
 C011(H01A,H01B,H01C), C012(H01D,H01E,H01F), C017(H01P,H01Q,H01R), C01A(H01G,
 H01H,H01I), C01C(H01S,H01T,H01U), C01E(H01V,H01W,H01X)
;
_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
C001 C 0.11931(11) 0.46465(10) 0.47083(10) 0.0440(3) Uani 1 1 d . . . . .
C002 C 0.05989(12) 0.51775(10) 0.39741(11) 0.0449(3) Uani 1 1 d . . . . .
C003 C 0.26074(12) 0.47437(10) 0.31159(11) 0.0471(3) Uani 1 1 d . . . . .
C004 C 0.24417(11) 0.43823(10) 0.41658(11) 0.0449(3) Uani 1 1 d . . . . .
C005 C 0.14278(12) 0.52344(11) 0.29060(11) 0.0508(3) Uani 1 1 d . . . . .
C006 C 0.55106(13) -0.05555(10) 0.57733(11) 0.0485(3) Uani 1 1 d . . . . .
C007 C -0.05978(12) 0.55396(10) 0.42542(11) 0.0469(3) Uani 1 1 d . . . . .
H007 H -0.098575 0.589393 0.376413 0.056 Uiso 1 1 calc R . . . .
C008 C 0.34110(13) 0.39020(11) 0.45161(12) 0.0514(3) Uani 1 1 d . . . . .
H008 H 0.331619 0.364724 0.521611 0.062 Uiso 1 1 calc R . . . .
C009 C 0.45229(13) 0.38092(12) 0.38032(12) 0.0551(4) Uani 1 1 d . . . . .
H009 H 0.517318 0.349625 0.403820 0.066 Uiso 1 1 calc R . . . .
C00A C 0.49944(13) 0.07490(11) 0.64849(11) 0.0501(3) Uani 1 1 d . . . . .
C00B C 0.59230(14) -0.09606(11) 0.66688(12) 0.0524(3) Uani 1 1 d . . . . .
C00C C 0.49281(12) 0.04372(10) 0.56699(11) 0.0470(3) Uani 1 1 d . . . . .
C00D C 0.55953(13) -0.02346(10) 0.71203(11) 0.0502(3) Uani 1 1 d . . . . .
C00E C 0.37162(13) 0.46398(12) 0.24075(11) 0.0526(3) Uani 1 1 d . . . . .
H00E H 0.380407 0.488259 0.171004 0.063 Uiso 1 1 calc R . . . .
C00F C 0.57248(14) 0.17131(11) 0.60138(12) 0.0526(3) Uani 1 1 d . . . . .
C00G C 0.47051(12) 0.41658(12) 0.27494(12) 0.0545(3) Uani 1 1 d . . . . .
C00H C 0.50343(16) 0.24901(11) 0.63488(13) 0.0581(4) Uani 1 1 d . . . . .
C00I C 0.37946(14) 0.11008(12) 0.71127(12) 0.0551(4) Uani 1 1 d . . . . .
C00J C 0.44154(13) 0.09948(10) 0.49032(12) 0.0512(3) Uani 1 1 d . . . . .
H00J H 0.403013 0.164744 0.483925 0.061 Uiso 1 1 calc R . . . .
C00K C 0.38380(16) 0.21090(12) 0.70211(12) 0.0597(4) Uani 1 1 d . . . . .
C00L C 0.0898(11) 0.4569(8) 0.2586(9) 0.0548(17) Uani 0.646(15) 1 d . U P A 1
C00M C 0.58252(15) -0.04431(12) 0.80101(12) 0.0570(4) Uani 1 1 d . . . . .
H00M H 0.559850 0.005150 0.829707 0.068 Uiso 1 1 calc R . . . .
C00N C 0.63990(15) -0.13967(12) 0.84865(13) 0.0599(4) Uani 1 1 d . . . . .
C00O C 0.65087(17) -0.19015(12) 0.71214(14) 0.0651(4) Uani 1 1 d . . . . .
H00O H 0.674567 -0.239039 0.682697 0.078 Uiso 1 1 calc R . . . .
C00P C 0.67346(17) -0.21026(13) 0.80109(14) 0.0676(4) Uani 1 1 d . . . . .
H00P H 0.712701 -0.273467 0.830727 0.081 Uiso 1 1 calc R . . . .
C00Q C 0.1497(9) 0.6268(7) 0.1977(7) 0.0591(15) Uani 0.646(15) 1 d . U P A 1
C00R C 0.2809(2) 0.25881(17) 0.75159(15) 0.0783(6) Uani 1 1 d . . . . .
H00R H 0.282521 0.326062 0.745981 0.094 Uiso 1 1 calc R . . . .
C00S C 0.59705(14) 0.40713(15) 0.19999(14) 0.0698(5) Uani 1 1 d . . . . .
C00T C 0.65822(19) -0.16736(15) 0.95140(15) 0.0749(5) Uani 1 1 d . . . . .
C00U C 0.27541(17) 0.05611(17) 0.77010(15) 0.0761(5) Uani 1 1 d . . . . .
H00U H 0.273110 -0.011441 0.776758 0.091 Uiso 1 1 calc R . . . .
C00V C 0.68824(17) 0.18812(15) 0.53409(16) 0.0706(4) Uani 1 1 d . . . . .
H00V H 0.733839 0.137038 0.511118 0.085 Uiso 1 1 calc R . . . .
C00W C 0.1061(8) 0.6214(6) 0.1262(6) 0.0725(16) Uani 0.646(15) 1 d . U P A 1
C00X C 0.5529(2) 0.34336(15) 0.60113(18) 0.0827(6) Uani 1 1 d . . . . .
H00X H 0.508191 0.395067 0.623505 0.099 Uiso 1 1 calc R . . . .
C00Y C 0.1775(2) 0.2051(2) 0.80848(16) 0.0908(7) Uani 1 1 d . . . . .
H00Y H 0.108329 0.237202 0.840468 0.109 Uiso 1 1 calc R . . . .
C00Z C 0.17363(19) 0.1050(2) 0.81944(17) 0.0926(7) Uani 1 1 d . . . . .
H00Z H 0.102828 0.069582 0.859932 0.111 Uiso 1 1 calc R . . . .
C010 C 0.0689(10) 0.5139(6) 0.1667(7) 0.0747(17) Uani 0.646(15) 1 d . U P A 1
C011 C 0.65053(18) 0.29483(17) 0.23924(18) 0.0896(7) Uani 1 1 d . . . . .
H01A H 0.652142 0.275133 0.307685 0.134 Uiso 1 1 calc GR . . . .
H01B H 0.731097 0.290791 0.193536 0.134 Uiso 1 1 calc GR . . . .
H01C H 0.601805 0.248331 0.241032 0.134 Uiso 1 1 calc GR . . . .
C012 C 0.67691(18) 0.48021(19) 0.1985(2) 0.0957(7) Uani 1 1 d . . . . .
H01D H 0.641007 0.549942 0.179739 0.143 Uiso 1 1 calc GR . . . .
H01E H 0.755670 0.479963 0.148809 0.143 Uiso 1 1 calc GR . . . .
H01F H 0.683543 0.456009 0.266009 0.143 Uiso 1 1 calc GR . . . .
C013 C 0.7363(2) 0.28374(19) 0.5007(2) 0.0906(6) Uani 1 1 d . . . . .
H013 H 0.814846 0.296353 0.455291 0.109 Uiso 1 1 calc R . . . .
C014 C 0.0652(11) 0.3511(5) 0.3122(7) 0.0681(15) Uani 0.646(15) 1 d . U P A 1
H014 H 0.081350 0.311235 0.373804 0.082 Uiso 0.646(15) 1 calc R . P A 1
C016 C 0.6691(3) 0.35876(18) 0.5341(2) 0.0955(7) Uani 1 1 d . . . . .
H016 H 0.702836 0.421831 0.510916 0.115 Uiso 1 1 calc R . . . .
C017 C 0.7621(2) -0.2471(2) 0.96697(19) 0.0996(8) Uani 1 1 d . . . . .
H01P H 0.746332 -0.310145 0.966806 0.149 Uiso 1 1 calc GR . . . .
H01Q H 0.770395 -0.261978 1.032115 0.149 Uiso 1 1 calc GR . . . .
H01R H 0.835195 -0.219616 0.911849 0.149 Uiso 1 1 calc GR . . . .
C019 C 0.1903(6) 0.7184(6) 0.1783(7) 0.0884(17) Uani 0.646(15) 1 d . U P A 1
H019 H 0.218328 0.723260 0.225169 0.106 Uiso 0.646(15) 1 calc R . P A 1
C01A C 0.5972(2) 0.4404(2) 0.09062(17) 0.1044(8) Uani 1 1 d . . . . .
H01G H 0.551189 0.393549 0.089968 0.157 Uiso 1 1 calc GR . . . .
H01H H 0.678647 0.438587 0.045398 0.157 Uiso 1 1 calc GR . . . .
H01I H 0.562041 0.510105 0.067276 0.157 Uiso 1 1 calc GR . . . .
C01B C 0.0190(8) 0.4696(8) 0.1273(9) 0.111(3) Uani 0.646(15) 1 d . U P A 1
H01J H 0.002668 0.509585 0.065714 0.134 Uiso 0.646(15) 1 calc R . P A 1
C01C C 0.6799(3) -0.0715(2) 0.9608(2) 0.1216(11) Uani 1 1 d . . . . .
H01S H 0.749675 -0.038278 0.904534 0.182 Uiso 1 1 calc GR . . . .
H01T H 0.692743 -0.092218 1.025388 0.182 Uiso 1 1 calc GR . . . .
H01U H 0.610864 -0.023404 0.958233 0.182 Uiso 1 1 calc GR . . . .
C01D C 0.1892(8) 0.8061(7) 0.0857(8) 0.120(3) Uani 0.646(15) 1 d . U P A 1
H01K H 0.217181 0.868948 0.071431 0.144 Uiso 0.646(15) 1 calc R . P A 1
C01E C 0.5423(3) -0.2146(3) 1.03977(19) 0.1163(9) Uani 1 1 d . . . . .
H01V H 0.474783 -0.166410 1.029749 0.174 Uiso 1 1 calc GR . . . .
H01W H 0.549563 -0.227813 1.104882 0.174 Uiso 1 1 calc GR . . . .
H01X H 0.530234 -0.278894 1.039807 0.174 Uiso 1 1 calc GR . . . .
C01F C 0.1478(8) 0.7992(8) 0.0180(6) 0.131(3) Uani 0.646(15) 1 d . U P A 1
H01L H 0.149056 0.857345 -0.042854 0.157 Uiso 0.646(15) 1 calc R . P A 1
C01G C 0.0172(8) 0.3077(6) 0.2721(8) 0.100(2) Uani 0.646(15) 1 d . U P A 1
H01M H -0.000238 0.237519 0.307023 0.120 Uiso 0.646(15) 1 calc R . P A 1
C01H C 0.1036(8) 0.7076(7) 0.0369(5) 0.113(2) Uani 0.646(15) 1 d . U P A 1
H01N H 0.073198 0.704348 -0.009304 0.135 Uiso 0.646(15) 1 calc R . P A 1
C01I C -0.0063(7) 0.3676(8) 0.1789(9) 0.118(3) Uani 0.646(15) 1 d . U P A 1
H01O H -0.039292 0.336960 0.152345 0.141 Uiso 0.646(15) 1 calc R . P A 1
C0 C 0.2018(14) 0.7195(8) 0.2188(11) 0.095(3) Uani 0.354(15) 1 d . U P A 2
H0 H 0.224734 0.710886 0.273842 0.114 Uiso 0.354(15) 1 calc R . P A 2
C1AA C 0.2075(17) 0.8139(11) 0.1352(15) 0.147(6) Uani 0.354(15) 1 d . U P A 2
H1AA H 0.228074 0.870785 0.139173 0.176 Uiso 0.354(15) 1 calc R . P A 2
C2AA C 0.186(2) 0.8320(15) 0.0479(16) 0.175(8) Uani 0.354(15) 1 d . U P A 2
H2AA H 0.198920 0.896378 -0.008257 0.210 Uiso 0.354(15) 1 calc R . P A 2
C3AA C 0.1413(14) 0.7445(16) 0.0463(11) 0.144(7) Uani 0.354(15) 1 d . U P A 2
H3AA H 0.120836 0.752022 -0.009539 0.173 Uiso 0.354(15) 1 calc R . P A 2
C4AA C 0.1311(15) 0.6505(15) 0.1319(12) 0.091(3) Uani 0.354(15) 1 d . U P A 2
C5AA C 0.161(2) 0.6408(15) 0.2156(14) 0.072(3) Uani 0.354(15) 1 d . U P A 2
C2 C 0.0864(16) 0.5532(17) 0.1507(11) 0.087(4) Uani 0.354(15) 1 d . U P A 2
C6AA C 0.102(2) 0.4767(18) 0.2454(19) 0.069(4) Uani 0.354(15) 1 d . U P A 2
C3 C 0.063(2) 0.3837(18) 0.2849(15) 0.087(4) Uani 0.354(15) 1 d . U P A 2
H3 H 0.067732 0.337158 0.349581 0.105 Uiso 0.354(15) 1 calc R . P A 2
C7AA C 0.0114(18) 0.349(2) 0.2294(13) 0.128(5) Uani 0.354(15) 1 d . U P A 2
H7AA H -0.011900 0.281325 0.253328 0.153 Uiso 0.354(15) 1 calc R . P A 2
C8AA C 0.003(3) 0.433(3) 0.1349(19) 0.160(7) Uani 0.354(15) 1 d . U P A 2
H8AA H -0.033642 0.419346 0.097691 0.192 Uiso 0.354(15) 1 calc R . P A 2
C9AA C 0.0414(16) 0.526(2) 0.0970(11) 0.146(5) Uani 0.354(15) 1 d . U P A 2
H9AA H 0.037922 0.574478 0.032473 0.175 Uiso 0.354(15) 1 calc R . 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
C001 C002 1.4042(18) . ?
C001 C004 1.4713(17) . ?
C001 C007 1.3872(19) 2_566 ?
C002 C005 1.5242(19) . ?
C002 C007 1.3893(18) . ?
C003 C004 1.391(2) . ?
C003 C005 1.5280(18) . ?
C003 C00E 1.3856(19) . ?
C004 C008 1.3891(18) . ?
C005 C00L 1.566(11) . ?
C005 C00Q 1.519(9) . ?
C005 C5AA 1.560(18) . ?
C005 C6AA 1.40(2) . ?
C006 C00B 1.464(2) . ?
C006 C00C 1.4120(17) . ?
C006 C00J 1.394(2) 2_656 ?
C007 H007 0.9300 . ?
C008 H008 0.9300 . ?
C008 C009 1.387(2) . ?
C009 H009 0.9300 . ?
C009 C00G 1.393(2) . ?
C00A C00C 1.525(2) . ?
C00A C00D 1.5294(19) . ?
C00A C00F 1.529(2) . ?
C00A C00I 1.520(2) . ?
C00B C00D 1.398(2) . ?
C00B C00O 1.390(2) . ?
C00C C00J 1.379(2) . ?
C00D C00M 1.378(2) . ?
C00E H00E 0.9300 . ?
C00E C00G 1.403(2) . ?
C00F C00H 1.403(2) . ?
C00F C00V 1.370(2) . ?
C00G C00S 1.535(2) . ?
C00H C00K 1.457(3) . ?
C00H C00X 1.388(3) . ?
C00I C00K 1.395(2) . ?
C00I C00U 1.379(3) . ?
C00J H00J 0.9300 . ?
C00K C00R 1.397(2) . ?
C00L C010 1.365(13) . ?
C00L C014 1.398(10) . ?
C00M H00M 0.9300 . ?
C00M C00N 1.404(2) . ?
C00N C00P 1.398(2) . ?
C00N C00T 1.529(2) . ?
C00O H00O 0.9300 . ?
C00O C00P 1.378(2) . ?
C00P H00P 0.9300 . ?
C00Q C00W 1.413(8) . ?
C00Q C019 1.363(10) . ?
C00R H00R 0.9300 . ?
C00R C00Y 1.369(4) . ?
C00S C011 1.535(3) . ?
C00S C012 1.549(3) . ?
C00S C01A 1.517(3) . ?
C00T C017 1.516(3) . ?
C00T C01C 1.522(3) . ?
C00T C01E 1.539(4) . ?
C00U H00U 0.9300 . ?
C00U C00Z 1.395(3) . ?
C00V H00V 0.9300 . ?
C00V C013 1.398(3) . ?
C00W C010 1.477(9) . ?
C00W C01H 1.380(10) . ?
C00X H00X 0.9300 . ?
C00X C016 1.371(3) . ?
C00Y H00Y 0.9300 . ?
C00Y C00Z 1.374(4) . ?
C00Z H00Z 0.9300 . ?
C010 C01B 1.376(10) . ?
C011 H01A 0.9600 . ?
C011 H01B 0.9600 . ?
C011 H01C 0.9600 . ?
C012 H01D 0.9600 . ?
C012 H01E 0.9600 . ?
C012 H01F 0.9600 . ?
C013 H013 0.9300 . ?
C013 C016 1.364(3) . ?
C014 H014 0.9300 . ?
C014 C01G 1.357(12) . ?
C016 H016 0.9300 . ?
C017 H01P 0.9600 . ?
C017 H01Q 0.9600 . ?
C017 H01R 0.9600 . ?
C019 H019 0.9300 . ?
C019 C01D 1.417(9) . ?
C01A H01G 0.9600 . ?
C01A H01H 0.9600 . ?
C01A H01I 0.9600 . ?
C01B H01J 0.9300 . ?
C01B C01I 1.352(11) . ?
C01C H01S 0.9600 . ?
C01C H01T 0.9600 . ?
C01C H01U 0.9600 . ?
C01D H01K 0.9300 . ?
C01D C01F 1.352(13) . ?
C01E H01V 0.9600 . ?
C01E H01W 0.9600 . ?
C01E H01X 0.9600 . ?
C01F H01L 0.9300 . ?
C01F C01H 1.385(11) . ?
C01G H01M 0.9300 . ?
C01G C01I 1.401(10) . ?
C01H H01N 0.9300 . ?
C01I H01O 0.9300 . ?
C0 H0 0.9300 . ?
C0 C1AA 1.379(14) . ?
C0 C5AA 1.346(19) . ?
C1AA H1AA 0.9300 . ?
C1AA C2AA 1.36(3) . ?
C2AA H2AA 0.9300 . ?
C2AA C3AA 1.47(3) . ?
C3AA H3AA 0.9300 . ?
C3AA C4AA 1.385(18) . ?
C4AA C5AA 1.397(16) . ?
C4AA C2 1.465(19) . ?
C2 C6AA 1.43(3) . ?
C2 C9AA 1.35(2) . ?
C6AA C3 1.30(2) . ?
C3 H3 0.9300 . ?
C3 C7AA 1.50(3) . ?
C7AA H7AA 0.9300 . ?
C7AA C8AA 1.44(3) . ?
C8AA H8AA 0.9300 . ?
C8AA C9AA 1.31(3) . ?
C9AA H9AA 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C002 C001 C004 108.17(12) . . ?
C007 C001 C002 120.85(12) 2_566 . ?
C007 C001 C004 130.98(12) 2_566 . ?
C001 C002 C005 110.54(11) . . ?
C007 C002 C001 121.58(13) . . ?
C007 C002 C005 127.83(12) . . ?
C004 C003 C005 110.45(11) . . ?
C00E C003 C004 121.74(12) . . ?
C00E C003 C005 127.80(13) . . ?
C003 C004 C001 109.08(11) . . ?
C008 C004 C001 131.58(13) . . ?
C008 C004 C003 119.28(12) . . ?
C002 C005 C003 101.53(11) . . ?
C002 C005 C00L 108.2(4) . . ?
C002 C005 C5AA 108.4(7) . . ?
C003 C005 C00L 112.4(4) . . ?
C003 C005 C5AA 108.7(8) . . ?
C00Q C005 C002 118.8(4) . . ?
C00Q C005 C003 117.0(4) . . ?
C00Q C005 C00L 99.1(5) . . ?
C6AA C005 C002 115.6(10) . . ?
C6AA C005 C003 114.7(10) . . ?
C6AA C005 C5AA 107.5(11) . . ?
C00C C006 C00B 108.32(12) . . ?
C00J C006 C00B 131.08(12) 2_656 . ?
C00J C006 C00C 120.57(13) 2_656 . ?
C001 C007 C002 117.57(12) 2_566 . ?
C001 C007 H007 121.2 2_566 . ?
C002 C007 H007 121.2 . . ?
C004 C008 H008 120.6 . . ?
C009 C008 C004 118.83(14) . . ?
C009 C008 H008 120.6 . . ?
C008 C009 H009 118.7 . . ?
C008 C009 C00G 122.67(13) . . ?
C00G C009 H009 118.7 . . ?
C00C C00A C00D 101.68(10) . . ?
C00C C00A C00F 112.91(12) . . ?
C00F C00A C00D 112.22(12) . . ?
C00I C00A C00C 114.90(12) . . ?
C00I C00A C00D 114.56(12) . . ?
C00I C00A C00F 101.09(11) . . ?
C00D C00B C006 109.24(12) . . ?
C00O C00B C006 131.73(14) . . ?
C00O C00B C00D 118.99(14) . . ?
C006 C00C C00A 110.28(12) . . ?
C00J C00C C006 121.12(13) . . ?
C00J C00C C00A 128.60(12) . . ?
C00B C00D C00A 110.23(12) . . ?
C00M C00D C00A 128.53(12) . . ?
C00M C00D C00B 121.24(13) . . ?
C003 C00E H00E 120.2 . . ?
C003 C00E C00G 119.55(14) . . ?
C00G C00E H00E 120.2 . . ?
C00H C00F C00A 110.64(14) . . ?
C00V C00F C00A 128.76(14) . . ?
C00V C00F C00H 120.60(15) . . ?
C009 C00G C00E 117.93(13) . . ?
C009 C00G C00S 119.80(13) . . ?
C00E C00G C00S 122.22(14) . . ?
C00F C00H C00K 108.33(14) . . ?
C00X C00H C00F 120.01(18) . . ?
C00X C00H C00K 131.64(16) . . ?
C00K C00I C00A 110.87(14) . . ?
C00U C00I C00A 128.22(15) . . ?
C00U C00I C00K 120.91(15) . . ?
C006 C00J H00J 120.8 2_656 . ?
C00C C00J C006 118.32(12) . 2_656 ?
C00C C00J H00J 120.8 . . ?
C00I C00K C00H 109.06(13) . . ?
C00I C00K C00R 119.70(19) . . ?
C00R C00K C00H 131.22(18) . . ?
C010 C00L C005 112.3(7) . . ?
C010 C00L C014 120.3(9) . . ?
C014 C00L C005 127.4(9) . . ?
C00D C00M H00M 119.8 . . ?
C00D C00M C00N 120.50(14) . . ?
C00N C00M H00M 119.8 . . ?
C00M C00N C00T 121.23(14) . . ?
C00P C00N C00M 117.14(15) . . ?
C00P C00N C00T 121.54(14) . . ?
C00B C00O H00O 120.3 . . ?
C00P C00O C00B 119.32(14) . . ?
C00P C00O H00O 120.3 . . ?
C00N C00P H00P 118.6 . . ?
C00O C00P C00N 122.79(14) . . ?
C00O C00P H00P 118.6 . . ?
C00W C00Q C005 112.2(5) . . ?
C019 C00Q C005 128.2(6) . . ?
C019 C00Q C00W 119.6(7) . . ?
C00K C00R H00R 120.5 . . ?
C00Y C00R C00K 118.9(2) . . ?
C00Y C00R H00R 120.5 . . ?
C00G C00S C011 110.32(14) . . ?
C00G C00S C012 107.03(16) . . ?
C011 C00S C012 108.34(17) . . ?
C01A C00S C00G 112.28(14) . . ?
C01A C00S C011 110.04(19) . . ?
C01A C00S C012 108.70(19) . . ?
C00N C00T C01E 108.05(19) . . ?
C017 C00T C00N 112.30(15) . . ?
C017 C00T C01C 108.7(2) . . ?
C017 C00T C01E 108.1(2) . . ?
C01C C00T C00N 112.00(17) . . ?
C01C C00T C01E 107.5(2) . . ?
C00I C00U H00U 120.7 . . ?
C00I C00U C00Z 118.6(2) . . ?
C00Z C00U H00U 120.7 . . ?
C00F C00V H00V 120.7 . . ?
C00F C00V C013 118.52(18) . . ?
C013 C00V H00V 120.7 . . ?
C00Q C00W C010 107.8(6) . . ?
C01H C00W C00Q 121.1(7) . . ?
C01H C00W C010 131.1(6) . . ?
C00H C00X H00X 120.7 . . ?
C016 C00X C00H 118.65(18) . . ?
C016 C00X H00X 120.7 . . ?
C00R C00Y H00Y 119.2 . . ?
C00R C00Y C00Z 121.55(18) . . ?
C00Z C00Y H00Y 119.2 . . ?
C00U C00Z H00Z 119.8 . . ?
C00Y C00Z C00U 120.3(2) . . ?
C00Y C00Z H00Z 119.8 . . ?
C00L C010 C00W 108.7(7) . . ?
C00L C010 C01B 120.8(7) . . ?
C01B C010 C00W 130.5(8) . . ?
C00S C011 H01A 109.5 . . ?
C00S C011 H01B 109.5 . . ?
C00S C011 H01C 109.5 . . ?
H01A C011 H01B 109.5 . . ?
H01A C011 H01C 109.5 . . ?
H01B C011 H01C 109.5 . . ?
C00S C012 H01D 109.5 . . ?
C00S C012 H01E 109.5 . . ?
C00S C012 H01F 109.5 . . ?
H01D C012 H01E 109.5 . . ?
H01D C012 H01F 109.5 . . ?
H01E C012 H01F 109.5 . . ?
C00V C013 H013 119.7 . . ?
C016 C013 C00V 120.7(2) . . ?
C016 C013 H013 119.7 . . ?
C00L C014 H014 120.8 . . ?
C01G C014 C00L 118.5(8) . . ?
C01G C014 H014 120.8 . . ?
C00X C016 H016 119.2 . . ?
C013 C016 C00X 121.6(2) . . ?
C013 C016 H016 119.2 . . ?
C00T C017 H01P 109.5 . . ?
C00T C017 H01Q 109.5 . . ?
C00T C017 H01R 109.5 . . ?
H01P C017 H01Q 109.5 . . ?
H01P C017 H01R 109.5 . . ?
H01Q C017 H01R 109.5 . . ?
C00Q C019 H019 120.6 . . ?
C00Q C019 C01D 118.9(7) . . ?
C01D C019 H019 120.6 . . ?
C00S C01A H01G 109.5 . . ?
C00S C01A H01H 109.5 . . ?
C00S C01A H01I 109.5 . . ?
H01G C01A H01H 109.5 . . ?
H01G C01A H01I 109.5 . . ?
H01H C01A H01I 109.5 . . ?
C010 C01B H01J 120.3 . . ?
C01I C01B C010 119.4(8) . . ?
C01I C01B H01J 120.3 . . ?
C00T C01C H01S 109.5 . . ?
C00T C01C H01T 109.5 . . ?
C00T C01C H01U 109.5 . . ?
H01S C01C H01T 109.5 . . ?
H01S C01C H01U 109.5 . . ?
H01T C01C H01U 109.5 . . ?
C019 C01D H01K 119.7 . . ?
C01F C01D C019 120.5(9) . . ?
C01F C01D H01K 119.7 . . ?
C00T C01E H01V 109.5 . . ?
C00T C01E H01W 109.5 . . ?
C00T C01E H01X 109.5 . . ?
H01V C01E H01W 109.5 . . ?
H01V C01E H01X 109.5 . . ?
H01W C01E H01X 109.5 . . ?
C01D C01F H01L 119.1 . . ?
C01D C01F C01H 121.7(8) . . ?
C01H C01F H01L 119.1 . . ?
C014 C01G H01M 119.6 . . ?
C014 C01G C01I 120.7(6) . . ?
C01I C01G H01M 119.6 . . ?
C00W C01H C01F 118.1(6) . . ?
C00W C01H H01N 121.0 . . ?
C01F C01H H01N 121.0 . . ?
C01B C01I C01G 120.2(6) . . ?
C01B C01I H01O 119.9 . . ?
C01G C01I H01O 119.9 . . ?
C1AA C0 H0 122.2 . . ?
C5AA C0 H0 122.2 . . ?
C5AA C0 C1AA 115.6(15) . . ?
C0 C1AA H1AA 116.8 . . ?
C2AA C1AA C0 126.5(16) . . ?
C2AA C1AA H1AA 116.8 . . ?
C1AA C2AA H2AA 121.7 . . ?
C1AA C2AA C3AA 116.6(12) . . ?
C3AA C2AA H2AA 121.7 . . ?
C2AA C3AA H3AA 121.5 . . ?
C4AA C3AA C2AA 116.9(16) . . ?
C4AA C3AA H3AA 121.5 . . ?
C3AA C4AA C5AA 120.9(16) . . ?
C3AA C4AA C2 127.7(15) . . ?
C5AA C4AA C2 111.4(11) . . ?
C0 C5AA C005 132.6(12) . . ?
C0 C5AA C4AA 123.3(14) . . ?
C4AA C5AA C005 104.0(11) . . ?
C6AA C2 C4AA 106.8(13) . . ?
C9AA C2 C4AA 133.4(14) . . ?
C9AA C2 C6AA 119.8(17) . . ?
C005 C6AA C2 109.9(16) . . ?
C3 C6AA C005 129(2) . . ?
C3 C6AA C2 121(2) . . ?
C6AA C3 H3 118.9 . . ?
C6AA C3 C7AA 122.1(17) . . ?
C7AA C3 H3 118.9 . . ?
C3 C7AA H7AA 124.3 . . ?
C8AA C7AA C3 111.4(17) . . ?
C8AA C7AA H7AA 124.3 . . ?
C7AA C8AA H8AA 117.5 . . ?
C9AA C8AA C7AA 125(2) . . ?
C9AA C8AA H8AA 117.5 . . ?
C2 C9AA H9AA 119.7 . . ?
C8AA C9AA C2 120.6(16) . . ?
C8AA C9AA H9AA 119.7 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.500 391.9 120.3 ?
2 0.188 0.500 0.675 7.3 0.0 ?
3 0.406 0.785 0.894 8.2 0.0 ?
4 0.594 0.215 0.106 8.2 0.0 ?
5 0.813 0.500 0.325 7.3 0.0 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.341
_oxdiff_exptl_absorpt_empirical_full_min 0.476
####################################################################### 
# 
# 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_kato_210302_1
_database_code_depnum_ccdc_archive 'CCDC 2305242'
loop_
_audit_author_name
_audit_author_address
'Koji Hirano'
;Osaka University
Japan
;
_audit_update_record             
;
2023-11-02 deposited with the CCDC.	2024-01-02 downloaded from the CCDC.
;
_audit_creation_date             2021-03-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C2 H4 Cl2, C56 H41 N'
_chemical_formula_sum            'C58 H45 Cl2 N'
_chemical_formula_weight         826.85
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C58 H45 N Cl2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      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                   10.38100(10)
_cell_length_b                   14.3480(2)
_cell_length_c                   15.61030(10)
_cell_angle_alpha                94.9290(10)
_cell_angle_beta                 102.9010(10)
_cell_angle_gamma                107.0460(10)
_cell_volume                     2138.07(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    17419
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      74.1000
_cell_measurement_theta_min      4.0130
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.674
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.43a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             868
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 -8 3 0.0293
-1 0 -9 0.0669
-4 8 -2 0.0509
1 0 9 0.0503
6 -6 -1 0.0323
4 5 -4 0.0305
-5 8 1 0.0418
-5 -4 4 0.0278
-6 6 -1 0.0431

_exptl_crystal_size_max          0.147
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.063
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
4.2013 -7.9799 3.0142 -0.3074 -0.0239 0.9513
-0.9041 0.0577 -9.2927 0.9927 0.0783 -0.0914
-4.2739 8.3673 -1.7666 0.1734 0.0133 -0.9848
1.0189 -0.2958 9.2699 -0.9899 -0.0780 0.1187
6.0048 -6.4695 -1.4822 -0.0330 0.4077 0.9125
3.9726 5.4873 -3.8903 -0.0759 0.9650 -0.2512
-5.3318 7.6049 0.7618 0.0190 -0.2295 -0.9731
-4.8712 -4.0712 3.9787 0.0784 -0.9941 0.0754
-5.7562 6.4672 -1.0904 0.2743 -0.3210 -0.9065

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33580
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.235
_diffrn_reflns_theta_min         3.265
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -29.00  64.00   0.50    0.27    --   42.80 -57.00  60.00  186
  2  ω     56.00  84.00   0.50    0.27    --   42.80-130.00 -24.00   56
  3  ω     42.00  67.00   0.50    1.08    --   76.50-130.00 -24.00   50
  4  ω     54.00  89.00   0.50    0.27    --   42.80-140.00 161.00   70
  5  ω     49.00  74.00   0.50    1.08    --   76.50-140.00 161.00   50
  6  ω    116.00 151.00   0.50    1.08    --   76.50  77.00   0.00   70
  7  ω     85.00 110.00   0.50    1.08    --   76.50 130.00  47.00   50
  8  ω     68.00  93.00   0.50    0.27    --   42.80 130.00  47.00   50
  9  ω     54.00 111.00   0.50    1.08    --   76.50  77.00   0.00  114
 10  ω     71.00 102.00   0.50    0.27    --   42.80 125.00 -60.00   62
 11  ω     62.00 113.00   0.50    0.27    --   42.80 140.00-138.00  102
 12  ω     82.00 107.00   0.50    1.08    --   76.50 140.00-138.00   50
 13  ω    -61.00 -34.00   0.50    1.08    -- -106.00 125.00 -90.00   54
 14  ω    -63.00 -37.00   0.50    1.08    -- -106.00 125.00-150.00   52
 15  ω    -77.00 -35.00   0.50    1.08    -- -106.00  77.00 -90.00   84
 16  ω   -104.00 -21.00   0.50    0.27    --  -42.80 140.00-138.00  166
 17  ω    -86.00 -58.00   0.50    0.27    --  -42.80 130.00  47.00   56
 18  ω   -111.00 -40.00   0.50    1.08    -- -106.00 130.00  47.00  142
 19  ω    -67.00 -32.00   0.50    1.08    -- -106.00 125.00  90.00   70
 20  ω    -57.00 -32.00   0.50    1.08    -- -106.00  77.00  90.00   50
 21  ω    -86.00 -40.00   0.50    1.08    -- -106.00 125.00  30.00   92
 22  ω   -103.00 -77.00   0.50    1.08    -- -106.00 125.00 -90.00   52
 23  ω   -104.00 -78.00   0.50    1.08    -- -106.00 140.00-138.00   52
 24  ω   -115.00 -33.00   0.50    1.08    -- -106.00 125.00 -60.00  164
 25  ω   -101.00 -76.00   0.50    1.08    -- -106.00 125.00 -30.00   50
 26  ω   -126.00 -71.00   0.50    1.08    -- -106.00  57.00 -90.00  110
 27  ω   -128.00 -81.00   0.50    1.08    -- -106.00  77.00 -90.00   94
 28  ω   -112.00 -86.00   0.50    1.08    -- -106.00 125.00-150.00   52
 29  ω   -117.00 -82.00   0.50    1.08    -- -106.00 125.00-120.00   70
 30  ω   -128.00 -32.00   0.50    1.08    -- -106.00  57.00 -30.00  192
 31  ω    -99.00 -58.00   0.50    1.08    -- -106.00  57.00  90.00   82
 32  ω   -106.00 -75.00   0.50    1.08    -- -106.00  77.00  90.00   62
 33  ω   -104.00 -31.00   0.50    1.08    -- -106.00  37.00  90.00  146
 34  ω    -94.00 -60.00   0.50    1.08    -- -106.00 125.00 150.00   68
 35  ω   -114.00 -77.00   0.50    1.08    -- -106.00 125.00  90.00   74
 36  ω   -129.00 -35.00   0.50    1.08    -- -106.00 142.00  -4.72  188
 37  ω   -127.00-101.00   0.50    1.08    -- -106.00 139.00 128.10   52
 38  ω   -177.00 -75.00   0.50    1.08    -- -106.00 -19.00-120.00  204
 39  ω   -117.00 -84.00   0.50    1.08    -- -106.00 -37.00-150.00   66
 40  ω   -133.00 -28.00   0.50    1.08    -- -106.00  19.00-150.00  210
 41  ω   -115.00 -15.00   0.50    0.27    --  -42.80 -77.00 -30.00  200
 42  ω    -99.00 -70.00   0.50    1.08    -- -106.00-125.00   0.00   58
 43  ω   -116.00 -88.00   0.50    1.08    -- -106.00-130.00 -24.00   56
 44  ω   -130.00-105.00   0.50    1.08    -- -106.00-125.00   0.00   50
 45  ω   -143.00 -99.00   0.50    1.08    -- -106.00 -77.00  60.00   88
 46  ω   -123.00 -98.00   0.50    1.08    -- -106.00-140.00 161.00   50
 47  ω   -112.00 -87.00   0.50    0.27    --  -42.80-140.00 161.00   50
 48  ω   -115.00 -70.00   0.50    0.27    --  -42.80-125.00  60.00   90
 49  ω   -108.00 -83.00   0.50    0.27    --  -42.80-130.00 -24.00   50
 50  ω   -112.00 -71.00   0.50    1.08    -- -106.00-125.00-150.00   82
 51  ω   -173.00-137.00   0.50    1.08    -- -106.00-125.00   0.00   72
 52  ω   -174.00-115.00   0.50    1.08    -- -106.00-125.00-150.00  118
 53  ω   -177.00 -84.00   0.50    1.08    -- -106.00 -37.00-180.00  186
 54  ω   -166.00-125.00   0.50    1.08    -- -106.00 -37.00-150.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0684576000
_diffrn_orient_matrix_UB_12      -0.0354427000
_diffrn_orient_matrix_UB_13      -0.1003888000
_diffrn_orient_matrix_UB_21      0.1326946000
_diffrn_orient_matrix_UB_22      0.0649464000
_diffrn_orient_matrix_UB_23      -0.0209309000
_diffrn_orient_matrix_UB_31      0.0596509000
_diffrn_orient_matrix_UB_32      -0.0864867000
_diffrn_orient_matrix_UB_33      0.0034904000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7638
_reflns_number_total             8587
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         8587
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0396
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0547P)²+0.6346P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1104
_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. Others
 Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=1-FVAR(1)
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C2)=Sof(H2A)=Sof(H2B)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,
 H60B), C3(H3A,H3B), C2(H2A,H2B), C2A(H2AA,H2AB), C3A(H3AA,H3AB)
3.b Aromatic/amide H refined with riding coordinates:
 C34(H34), C31(H31), C12(H12), C9(H9), C29(H29), C47(H47), C28(H28), C21(H21),
 C39(H39), C18(H18), C24(H24), C27(H27), C52(H52), C42(H42), C22(H22), C15(H15),
  C23(H23), C26(H26), C50(H50), C48(H48), C41(H41), C17(H17), C40(H40),
 C55(H55), C53(H53), C16(H16), C49(H49), C54(H54)
3.c Idealised Me refined as rotating group:
 C61(H61A,H61B,H61C)
;
_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
Cl4 Cl -0.58816(5) 0.21166(3) -0.03097(3) 0.05017(13) Uani 1 1 d . . . . .
Cl1 Cl -0.34300(6) 0.43102(3) 0.06431(3) 0.05766(14) Uani 1 1 d . . . . .
N36 N 0.61467(11) 0.67938(8) 0.54196(7) 0.0215(2) Uani 1 1 d . . . . .
C11 C 0.45926(12) 0.75687(9) 0.56498(8) 0.0195(2) Uani 1 1 d . . . . .
C19 C 0.41149(13) 1.01744(9) 0.72973(8) 0.0208(2) Uani 1 1 d . . . . .
C35 C 0.50094(12) 0.64698(9) 0.46783(8) 0.0197(2) Uani 1 1 d . . . . .
C43 C -0.11201(13) 0.56570(9) 0.26134(8) 0.0221(2) Uani 1 1 d . . . . .
C25 C 0.31318(12) 0.87356(9) 0.78612(8) 0.0201(2) Uani 1 1 d . . . . .
C20 C 0.21471(13) 0.92316(9) 0.76807(8) 0.0219(2) Uani 1 1 d . . . . .
C32 C 0.25336(12) 0.60876(9) 0.33848(8) 0.0202(2) Uani 1 1 d . . . . .
C46 C 0.16348(13) 0.50551(9) 0.19881(8) 0.0217(2) Uani 1 1 d . . . . .
C34 C 0.47634(13) 0.57901(9) 0.39116(8) 0.0210(2) Uani 1 1 d . . . . .
H34 H 0.540557 0.547562 0.383506 0.025 Uiso 1 1 calc R . . . .
C31 C 0.27713(12) 0.67488(9) 0.41432(8) 0.0205(2) Uani 1 1 d . . . . .
H31 H 0.211977 0.705527 0.421734 0.025 Uiso 1 1 calc R . . . .
C45 C 0.08144(13) 0.65658(9) 0.21746(8) 0.0218(2) Uani 1 1 d . . . . .
C38 C -0.00791(12) 0.52258(9) 0.28853(8) 0.0207(2) Uani 1 1 d . . . . .
C5 C 0.44725(12) 0.92895(9) 0.76263(8) 0.0194(2) Uani 1 1 d . . . . .
C10 C 0.59008(12) 0.74494(9) 0.60266(8) 0.0200(2) Uani 1 1 d . . . . .
C13 C 0.48595(12) 0.86444(9) 0.69670(8) 0.0200(2) Uani 1 1 d . . . . .
C14 C 0.27734(13) 1.01408(9) 0.73502(8) 0.0224(2) Uani 1 1 d . . . . .
C8 C 0.61551(12) 0.85158(9) 0.73483(8) 0.0209(2) Uani 1 1 d . . . . .
C30 C 0.40241(12) 0.69437(9) 0.47975(8) 0.0192(2) Uani 1 1 d . . . . .
C7 C 0.66978(13) 0.90870(9) 0.82568(8) 0.0215(2) Uani 1 1 d . . . . .
C12 C 0.40768(12) 0.81842(9) 0.61245(8) 0.0202(2) Uani 1 1 d . . . . .
H12 H 0.323125 0.827845 0.587737 0.024 Uiso 1 1 calc R . . . .
C44 C -0.05678(13) 0.64887(9) 0.21691(8) 0.0233(3) Uani 1 1 d . . . . .
C9 C 0.67026(13) 0.79222(9) 0.68817(8) 0.0221(2) Uani 1 1 d . . . . .
H9 H 0.756003 0.784450 0.712735 0.027 Uiso 1 1 calc R . . . .
C6 C 0.57477(12) 0.95590(9) 0.84163(8) 0.0203(2) Uani 1 1 d . . . . .
C33 C 0.35048(13) 0.56087(9) 0.32681(8) 0.0203(2) Uani 1 1 d . . . . .
C29 C 0.59892(13) 1.01585(9) 0.92182(8) 0.0231(3) Uani 1 1 d . . . . .
H29 H 0.535971 1.047765 0.931215 0.028 Uiso 1 1 calc R . . . .
C37 C 0.12352(13) 0.57465(9) 0.26034(8) 0.0211(2) Uani 1 1 d . . . . .
C51 C 0.29281(13) 0.49559(9) 0.23969(8) 0.0221(2) Uani 1 1 d . . . . .
C47 C 0.08957(14) 0.45641(10) 0.11359(9) 0.0256(3) Uani 1 1 d . . . . .
H47 H 0.005335 0.464807 0.086281 0.031 Uiso 1 1 calc R . . . .
C28 C 0.71980(14) 1.02724(10) 0.98811(9) 0.0264(3) Uani 1 1 d . . . . .
H28 H 0.737976 1.067264 1.042396 0.032 Uiso 1 1 calc R . . . .
C21 C 0.08290(13) 0.88355(10) 0.78248(9) 0.0267(3) Uani 1 1 d . . . . .
H21 H 0.016489 0.915530 0.769870 0.032 Uiso 1 1 calc R . . . .
C39 C -0.02964(14) 0.44501(10) 0.33608(9) 0.0268(3) Uani 1 1 d . . . . .
H39 H 0.040122 0.417031 0.354337 0.032 Uiso 1 1 calc R . . . .
C18 C 0.49456(14) 1.09529(10) 0.69965(9) 0.0269(3) Uani 1 1 d . . . . .
H18 H 0.582849 1.096654 0.695011 0.032 Uiso 1 1 calc R . . . .
C24 C 0.28397(14) 0.78607(9) 0.82035(9) 0.0249(3) Uani 1 1 d . . . . .
H24 H 0.350238 0.753976 0.832963 0.030 Uiso 1 1 calc R . . . .
C27 C 0.81341(14) 0.97921(10) 0.97367(9) 0.0271(3) Uani 1 1 d . . . . .
H27 H 0.892836 0.986747 1.018921 0.033 Uiso 1 1 calc R . . . .
C52 C 0.16050(15) 0.73189(10) 0.18266(9) 0.0281(3) Uani 1 1 d . . . . .
H52 H 0.251979 0.736830 0.183047 0.034 Uiso 1 1 calc R . . . .
C56 C 0.73542(13) 0.64457(10) 0.55556(9) 0.0240(3) Uani 1 1 d . . . . .
H56A H 0.702483 0.572945 0.543065 0.029 Uiso 1 1 calc R . . . .
H56B H 0.787031 0.664168 0.617745 0.029 Uiso 1 1 calc R . . . .
C57 C 0.83468(13) 0.68302(10) 0.49835(9) 0.0252(3) Uani 1 1 d . . . . .
H57A H 0.780853 0.667324 0.436590 0.030 Uiso 1 1 calc R . . . .
H57B H 0.901119 0.646957 0.504355 0.030 Uiso 1 1 calc R . . . .
C42 C -0.24089(14) 0.52879(10) 0.28039(9) 0.0272(3) Uani 1 1 d . . . . .
H42 H -0.311142 0.556239 0.261764 0.033 Uiso 1 1 calc R . . . .
C22 C 0.05308(14) 0.79517(11) 0.81612(9) 0.0296(3) Uani 1 1 d . . . . .
H22 H -0.034381 0.767682 0.825860 0.036 Uiso 1 1 calc R . . . .
C15 C 0.22608(15) 1.09065(11) 0.71227(9) 0.0293(3) Uani 1 1 d . . . . .
H15 H 0.137525 1.089196 0.716372 0.035 Uiso 1 1 calc R . . . .
C23 C 0.15266(15) 0.74732(10) 0.83541(9) 0.0291(3) Uani 1 1 d . . . . .
H23 H 0.131226 0.688794 0.858629 0.035 Uiso 1 1 calc R . . . .
C26 C 0.79028(13) 0.91998(10) 0.89261(9) 0.0252(3) Uani 1 1 d . . . . .
H26 H 0.853802 0.888590 0.883245 0.030 Uiso 1 1 calc R . . . .
C50 C 0.34550(14) 0.43205(10) 0.19576(9) 0.0282(3) Uani 1 1 d . . . . .
H50 H 0.429803 0.423605 0.222814 0.034 Uiso 1 1 calc R . . . .
C48 C 0.14352(15) 0.39424(10) 0.06946(9) 0.0302(3) Uani 1 1 d . . . . .
H48 H 0.095166 0.361035 0.012169 0.036 Uiso 1 1 calc R . . . .
C58 C 0.91656(14) 0.79328(10) 0.51841(10) 0.0298(3) Uani 1 1 d . . . . .
H58A H 0.964005 0.812180 0.581340 0.036 Uiso 1 1 calc R . . . .
H58B H 0.852864 0.830850 0.504238 0.036 Uiso 1 1 calc R . . . .
C41 C -0.26247(14) 0.45020(10) 0.32774(10) 0.0296(3) Uani 1 1 d . . . . .
H41 H -0.348115 0.424665 0.340491 0.035 Uiso 1 1 calc R . . . .
C17 C 0.44280(16) 1.17152(11) 0.67648(10) 0.0326(3) Uani 1 1 d . . . . .
H17 H 0.497201 1.224464 0.656259 0.039 Uiso 1 1 calc R . . . .
C40 C -0.15718(15) 0.40946(10) 0.35620(10) 0.0302(3) Uani 1 1 d . . . . .
H40 H -0.172340 0.357979 0.388978 0.036 Uiso 1 1 calc R . . . .
C55 C -0.11647(15) 0.71633(11) 0.18023(10) 0.0306(3) Uani 1 1 d . . . . .
H55 H -0.208286 0.711121 0.179102 0.037 Uiso 1 1 calc R . . . .
C53 C 0.10139(16) 0.80014(11) 0.14709(10) 0.0338(3) Uani 1 1 d . . . . .
H53 H 0.154178 0.851612 0.124431 0.041 Uiso 1 1 calc R . . . .
C59 C 1.02378(15) 0.81684(11) 0.46337(10) 0.0331(3) Uani 1 1 d . . . . .
H59A H 1.088409 0.780539 0.480345 0.040 Uiso 1 1 calc R . . . .
H59B H 0.975012 0.792171 0.401165 0.040 Uiso 1 1 calc R . . . .
C16 C 0.31066(16) 1.16929(11) 0.68328(10) 0.0337(3) Uani 1 1 d . . . . .
H16 H 0.278348 1.221230 0.668200 0.040 Uiso 1 1 calc R . . . .
C49 C 0.26952(15) 0.38159(11) 0.11074(10) 0.0322(3) Uani 1 1 d . . . . .
H49 H 0.303386 0.338814 0.081086 0.039 Uiso 1 1 calc R . . . .
C54 C -0.03617(17) 0.79183(11) 0.14523(10) 0.0348(3) Uani 1 1 d . . . . .
H54 H -0.075023 0.837201 0.120324 0.042 Uiso 1 1 calc R . . . .
C60 C 1.10788(18) 0.92477(12) 0.47166(12) 0.0412(4) Uani 1 1 d . . . . .
H60A H 1.155373 0.950806 0.533845 0.049 Uiso 1 1 calc R . . . .
H60B H 1.044664 0.961397 0.452004 0.049 Uiso 1 1 calc R . . . .
C61 C 1.2150(2) 0.94101(15) 0.41770(14) 0.0531(5) Uani 1 1 d . . . . .
H61A H 1.168729 0.915663 0.355995 0.080 Uiso 1 1 calc GR . . . .
H61B H 1.280347 0.907230 0.438470 0.080 Uiso 1 1 calc GR . . . .
H61C H 1.263770 1.010421 0.424480 0.080 Uiso 1 1 calc GR . . . .
C3 C -0.4510(3) 0.2759(3) -0.0719(2) 0.0467(10) Uani 0.699(8) 1 d . . P A 1
H3A H -0.368047 0.259969 -0.044988 0.056 Uiso 0.699(8) 1 calc R . P A 1
H3B H -0.473997 0.254684 -0.135735 0.056 Uiso 0.699(8) 1 calc R . P A 1
C2 C -0.4207(5) 0.3846(2) -0.05348(19) 0.0529(10) Uani 0.699(8) 1 d . . P A 1
H2A H -0.506563 0.400188 -0.072254 0.063 Uiso 0.699(8) 1 calc R . P A 1
H2B H -0.357390 0.416631 -0.087277 0.063 Uiso 0.699(8) 1 calc R . P A 1
C2A C -0.3489(9) 0.3592(6) -0.0365(4) 0.047(2) Uani 0.301(8) 1 d . . P A 2
H2AA H -0.294718 0.400348 -0.070538 0.057 Uiso 0.301(8) 1 calc R . P A 2
H2AB H -0.310193 0.306574 -0.023247 0.057 Uiso 0.301(8) 1 calc R . P A 2
C3A C -0.4986(9) 0.3166(6) -0.0886(4) 0.046(2) Uani 0.301(8) 1 d . . P A 2
H3AA H -0.504891 0.290982 -0.149472 0.055 Uiso 0.301(8) 1 calc R . P A 2
H3AB H -0.543611 0.367147 -0.089595 0.055 Uiso 0.301(8) 1 calc R . 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
Cl4 C3 1.739(3) . ?
Cl4 C3A 1.931(7) . ?
Cl1 C2 1.813(3) . ?
Cl1 C2A 1.784(6) . ?
N36 C35 1.3873(16) . ?
N36 C10 1.3942(15) . ?
N36 C56 1.4601(15) . ?
C11 C10 1.4200(16) . ?
C11 C30 1.4341(17) . ?
C11 C12 1.3991(17) . ?
C19 C5 1.5221(16) . ?
C19 C14 1.4005(17) . ?
C19 C18 1.3850(18) . ?
C35 C34 1.4021(17) . ?
C35 C30 1.4191(16) . ?
C43 C38 1.4010(17) . ?
C43 C44 1.4672(18) . ?
C43 C42 1.3958(18) . ?
C25 C20 1.4012(17) . ?
C25 C5 1.5272(16) . ?
C25 C24 1.3848(18) . ?
C20 C14 1.4694(18) . ?
C20 C21 1.3962(18) . ?
C32 C31 1.3790(17) . ?
C32 C33 1.4101(17) . ?
C32 C37 1.5234(17) . ?
C46 C37 1.5278(16) . ?
C46 C51 1.4055(18) . ?
C46 C47 1.3860(18) . ?
C34 H34 0.9300 . ?
C34 C33 1.3977(17) . ?
C31 H31 0.9300 . ?
C31 C30 1.3991(17) . ?
C45 C44 1.4045(18) . ?
C45 C37 1.5253(17) . ?
C45 C52 1.3843(18) . ?
C38 C37 1.5298(17) . ?
C38 C39 1.3820(18) . ?
C5 C13 1.5220(16) . ?
C5 C6 1.5204(16) . ?
C10 C9 1.3971(17) . ?
C13 C8 1.4157(17) . ?
C13 C12 1.3730(17) . ?
C14 C15 1.3935(18) . ?
C8 C7 1.4741(17) . ?
C8 C9 1.3932(17) . ?
C7 C6 1.4021(17) . ?
C7 C26 1.3969(17) . ?
C12 H12 0.9300 . ?
C44 C55 1.3917(18) . ?
C9 H9 0.9300 . ?
C6 C29 1.3849(17) . ?
C33 C51 1.4744(17) . ?
C29 H29 0.9300 . ?
C29 C28 1.3939(18) . ?
C51 C50 1.3975(18) . ?
C47 H47 0.9300 . ?
C47 C48 1.3941(19) . ?
C28 H28 0.9300 . ?
C28 C27 1.391(2) . ?
C21 H21 0.9300 . ?
C21 C22 1.392(2) . ?
C39 H39 0.9300 . ?
C39 C40 1.3890(19) . ?
C18 H18 0.9300 . ?
C18 C17 1.393(2) . ?
C24 H24 0.9300 . ?
C24 C23 1.3941(19) . ?
C27 H27 0.9300 . ?
C27 C26 1.3932(19) . ?
C52 H52 0.9300 . ?
C52 C53 1.392(2) . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C56 C57 1.5251(18) . ?
C57 H57A 0.9700 . ?
C57 H57B 0.9700 . ?
C57 C58 1.5267(19) . ?
C42 H42 0.9300 . ?
C42 C41 1.392(2) . ?
C22 H22 0.9300 . ?
C22 C23 1.394(2) . ?
C15 H15 0.9300 . ?
C15 C16 1.390(2) . ?
C23 H23 0.9300 . ?
C26 H26 0.9300 . ?
C50 H50 0.9300 . ?
C50 C49 1.393(2) . ?
C48 H48 0.9300 . ?
C48 C49 1.394(2) . ?
C58 H58A 0.9700 . ?
C58 H58B 0.9700 . ?
C58 C59 1.5323(19) . ?
C41 H41 0.9300 . ?
C41 C40 1.391(2) . ?
C17 H17 0.9300 . ?
C17 C16 1.391(2) . ?
C40 H40 0.9300 . ?
C55 H55 0.9300 . ?
C55 C54 1.394(2) . ?
C53 H53 0.9300 . ?
C53 C54 1.391(2) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C59 C60 1.516(2) . ?
C16 H16 0.9300 . ?
C49 H49 0.9300 . ?
C54 H54 0.9300 . ?
C60 H60A 0.9700 . ?
C60 H60B 0.9700 . ?
C60 C61 1.517(2) . ?
C61 H61A 0.9600 . ?
C61 H61B 0.9600 . ?
C61 H61C 0.9600 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C2 1.487(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C2A C3A 1.498(13) . ?
C3A H3AA 0.9700 . ?
C3A H3AB 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
C35 N36 C10 108.89(10) . . ?
C35 N36 C56 124.83(10) . . ?
C10 N36 C56 126.16(10) . . ?
C10 C11 C30 107.03(10) . . ?
C12 C11 C10 120.52(11) . . ?
C12 C11 C30 132.41(11) . . ?
C14 C19 C5 110.96(11) . . ?
C18 C19 C5 128.09(11) . . ?
C18 C19 C14 120.93(12) . . ?
N36 C35 C34 129.64(11) . . ?
N36 C35 C30 108.73(10) . . ?
C34 C35 C30 121.63(11) . . ?
C38 C43 C44 108.57(11) . . ?
C42 C43 C38 119.97(12) . . ?
C42 C43 C44 131.44(12) . . ?
C20 C25 C5 110.82(11) . . ?
C24 C25 C20 121.26(12) . . ?
C24 C25 C5 127.92(11) . . ?
C25 C20 C14 108.42(11) . . ?
C21 C20 C25 120.20(12) . . ?
C21 C20 C14 131.38(12) . . ?
C31 C32 C33 121.68(11) . . ?
C31 C32 C37 126.79(11) . . ?
C33 C32 C37 111.49(10) . . ?
C51 C46 C37 110.85(11) . . ?
C47 C46 C37 128.15(12) . . ?
C47 C46 C51 121.00(12) . . ?
C35 C34 H34 121.7 . . ?
C33 C34 C35 116.66(11) . . ?
C33 C34 H34 121.7 . . ?
C32 C31 H31 121.1 . . ?
C32 C31 C30 117.87(11) . . ?
C30 C31 H31 121.1 . . ?
C44 C45 C37 110.84(11) . . ?
C52 C45 C44 120.55(12) . . ?
C52 C45 C37 128.61(12) . . ?
C43 C38 C37 110.84(11) . . ?
C39 C38 C43 120.88(12) . . ?
C39 C38 C37 128.27(11) . . ?
C19 C5 C25 101.25(9) . . ?
C13 C5 C19 115.95(10) . . ?
C13 C5 C25 112.21(10) . . ?
C6 C5 C19 114.18(10) . . ?
C6 C5 C25 112.39(10) . . ?
C6 C5 C13 101.36(9) . . ?
N36 C10 C11 108.40(10) . . ?
N36 C10 C9 129.87(11) . . ?
C9 C10 C11 121.70(11) . . ?
C8 C13 C5 110.99(10) . . ?
C12 C13 C5 127.22(11) . . ?
C12 C13 C8 121.71(11) . . ?
C19 C14 C20 108.50(11) . . ?
C15 C14 C19 120.48(12) . . ?
C15 C14 C20 131.00(12) . . ?
C13 C8 C7 107.80(10) . . ?
C9 C8 C13 121.47(11) . . ?
C9 C8 C7 130.73(11) . . ?
C35 C30 C11 106.92(10) . . ?
C31 C30 C11 132.49(11) . . ?
C31 C30 C35 120.58(11) . . ?
C6 C7 C8 108.58(11) . . ?
C26 C7 C8 131.75(12) . . ?
C26 C7 C6 119.66(11) . . ?
C11 C12 H12 121.1 . . ?
C13 C12 C11 117.83(11) . . ?
C13 C12 H12 121.1 . . ?
C45 C44 C43 108.53(11) . . ?
C55 C44 C43 131.19(12) . . ?
C55 C44 C45 120.25(12) . . ?
C10 C9 H9 121.6 . . ?
C8 C9 C10 116.75(11) . . ?
C8 C9 H9 121.6 . . ?
C7 C6 C5 111.16(10) . . ?
C29 C6 C5 127.24(11) . . ?
C29 C6 C7 121.56(11) . . ?
C32 C33 C51 107.67(11) . . ?
C34 C33 C32 121.57(11) . . ?
C34 C33 C51 130.76(11) . . ?
C6 C29 H29 120.8 . . ?
C6 C29 C28 118.44(12) . . ?
C28 C29 H29 120.8 . . ?
C32 C37 C46 101.03(10) . . ?
C32 C37 C45 115.67(10) . . ?
C32 C37 C38 112.13(10) . . ?
C46 C37 C38 112.93(10) . . ?
C45 C37 C46 114.49(10) . . ?
C45 C37 C38 101.14(9) . . ?
C46 C51 C33 108.78(10) . . ?
C50 C51 C46 119.84(12) . . ?
C50 C51 C33 131.38(12) . . ?
C46 C47 H47 120.5 . . ?
C46 C47 C48 118.93(13) . . ?
C48 C47 H47 120.5 . . ?
C29 C28 H28 119.8 . . ?
C27 C28 C29 120.49(12) . . ?
C27 C28 H28 119.8 . . ?
C20 C21 H21 120.7 . . ?
C22 C21 C20 118.54(12) . . ?
C22 C21 H21 120.7 . . ?
C38 C39 H39 120.5 . . ?
C38 C39 C40 119.04(12) . . ?
C40 C39 H39 120.5 . . ?
C19 C18 H18 120.8 . . ?
C19 C18 C17 118.46(13) . . ?
C17 C18 H18 120.8 . . ?
C25 C24 H24 120.9 . . ?
C25 C24 C23 118.30(12) . . ?
C23 C24 H24 120.8 . . ?
C28 C27 H27 119.4 . . ?
C28 C27 C26 121.15(12) . . ?
C26 C27 H27 119.4 . . ?
C45 C52 H52 120.4 . . ?
C45 C52 C53 119.19(13) . . ?
C53 C52 H52 120.4 . . ?
N36 C56 H56A 108.6 . . ?
N36 C56 H56B 108.6 . . ?
N36 C56 C57 114.61(10) . . ?
H56A C56 H56B 107.6 . . ?
C57 C56 H56A 108.6 . . ?
C57 C56 H56B 108.6 . . ?
C56 C57 H57A 108.0 . . ?
C56 C57 H57B 108.0 . . ?
C56 C57 C58 117.01(11) . . ?
H57A C57 H57B 107.3 . . ?
C58 C57 H57A 108.0 . . ?
C58 C57 H57B 108.0 . . ?
C43 C42 H42 120.6 . . ?
C41 C42 C43 118.86(12) . . ?
C41 C42 H42 120.6 . . ?
C21 C22 H22 119.6 . . ?
C21 C22 C23 120.82(12) . . ?
C23 C22 H22 119.6 . . ?
C14 C15 H15 120.8 . . ?
C16 C15 C14 118.32(13) . . ?
C16 C15 H15 120.8 . . ?
C24 C23 H23 119.6 . . ?
C22 C23 C24 120.86(13) . . ?
C22 C23 H23 119.6 . . ?
C7 C26 H26 120.7 . . ?
C27 C26 C7 118.67(12) . . ?
C27 C26 H26 120.7 . . ?
C51 C50 H50 120.6 . . ?
C49 C50 C51 118.84(13) . . ?
C49 C50 H50 120.6 . . ?
C47 C48 H48 119.8 . . ?
C49 C48 C47 120.35(13) . . ?
C49 C48 H48 119.8 . . ?
C57 C58 H58A 109.6 . . ?
C57 C58 H58B 109.6 . . ?
C57 C58 C59 110.11(11) . . ?
H58A C58 H58B 108.2 . . ?
C59 C58 H58A 109.6 . . ?
C59 C58 H58B 109.6 . . ?
C42 C41 H41 119.7 . . ?
C40 C41 C42 120.66(12) . . ?
C40 C41 H41 119.7 . . ?
C18 C17 H17 119.6 . . ?
C16 C17 C18 120.70(13) . . ?
C16 C17 H17 119.6 . . ?
C39 C40 C41 120.57(13) . . ?
C39 C40 H40 119.7 . . ?
C41 C40 H40 119.7 . . ?
C44 C55 H55 120.6 . . ?
C44 C55 C54 118.81(13) . . ?
C54 C55 H55 120.6 . . ?
C52 C53 H53 119.8 . . ?
C54 C53 C52 120.40(13) . . ?
C54 C53 H53 119.8 . . ?
C58 C59 H59A 108.2 . . ?
C58 C59 H59B 108.2 . . ?
H59A C59 H59B 107.3 . . ?
C60 C59 C58 116.54(12) . . ?
C60 C59 H59A 108.2 . . ?
C60 C59 H59B 108.2 . . ?
C15 C16 C17 121.07(13) . . ?
C15 C16 H16 119.5 . . ?
C17 C16 H16 119.5 . . ?
C50 C49 C48 120.98(13) . . ?
C50 C49 H49 119.5 . . ?
C48 C49 H49 119.5 . . ?
C55 C54 H54 119.6 . . ?
C53 C54 C55 120.79(13) . . ?
C53 C54 H54 119.6 . . ?
C59 C60 H60A 109.0 . . ?
C59 C60 H60B 109.0 . . ?
C59 C60 C61 113.03(14) . . ?
H60A C60 H60B 107.8 . . ?
C61 C60 H60A 109.0 . . ?
C61 C60 H60B 109.0 . . ?
C60 C61 H61A 109.5 . . ?
C60 C61 H61B 109.5 . . ?
C60 C61 H61C 109.5 . . ?
H61A C61 H61B 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
Cl4 C3 H3A 109.1 . . ?
Cl4 C3 H3B 109.1 . . ?
H3A C3 H3B 107.9 . . ?
C2 C3 Cl4 112.3(3) . . ?
C2 C3 H3A 109.1 . . ?
C2 C3 H3B 109.1 . . ?
Cl1 C2 H2A 109.5 . . ?
Cl1 C2 H2B 109.5 . . ?
C3 C2 Cl1 110.6(3) . . ?
C3 C2 H2A 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
Cl1 C2A H2AA 110.2 . . ?
Cl1 C2A H2AB 110.2 . . ?
H2AA C2A H2AB 108.5 . . ?
C3A C2A Cl1 107.7(7) . . ?
C3A C2A H2AA 110.2 . . ?
C3A C2A H2AB 110.2 . . ?
Cl4 C3A H3AA 110.2 . . ?
Cl4 C3A H3AB 110.2 . . ?
C2A C3A Cl4 107.4(6) . . ?
C2A C3A H3AA 110.2 . . ?
C2A C3A H3AB 110.2 . . ?
H3AA C3A H3AB 108.5 . . ?

_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.609
_oxdiff_exptl_absorpt_empirical_full_min 0.710
####################################################################### 
# 
# 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_kato_210212_1
_database_code_depnum_ccdc_archive 'CCDC 2305243'
loop_
_audit_author_name
_audit_author_address
'Koji Hirano'
;Osaka University
Japan
;
_audit_update_record             
;
2023-11-02 deposited with the CCDC.	2024-01-02 downloaded from the CCDC.
;
_audit_creation_date             2021-02-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H24 S, 2(C H Cl3)'
_chemical_formula_sum            'C44 H26 Cl6 S'
_chemical_formula_weight         799.41
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C44 H26 S Cl6'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   12.2354(4)
_cell_length_b                   14.2615(4)
_cell_length_c                   20.8253(6)
_cell_angle_alpha                90
_cell_angle_beta                 98.248(3)
_cell_angle_gamma                90
_cell_volume                     3596.33(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12940
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.9840
_cell_measurement_theta_min      2.2940
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67386
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-12 14 4 0.0794
-13 -12 10 0.0464
13 -13 -4 0.1188
12 14 -10 0.1333
-10 16 7 0.1019
-1 -1 29 0.0241
10 -16 -4 0.1172
1 1 -29 0.0613

_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.089
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-12.3982 13.9695 3.5542 0.1879 0.0566 0.9806
-13.3124 -11.8838 10.1511 0.9575 0.2842 -0.0493
13.1188 -13.0341 -4.1726 -0.2479 -0.0744 -0.9659
12.0295 13.6113 -9.8497 -0.9460 -0.2807 0.1623
-9.9481 16.0950 7.1165 0.0043 0.1910 0.9816
-1.2576 -0.5255 29.2583 0.0256 0.9996 -0.0091
9.9442 -16.3995 -3.6696 -0.0012 -0.0724 -0.9974
0.9576 1.0240 -29.1897 -0.0256 -0.9989 0.0394

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.798
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            28944
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.798
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.211
_diffrn_reflns_theta_min         1.976
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.798
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      7.00  67.00   0.50    6.87    --   -8.74  46.00  74.00  120
  2  ω    -25.00   1.00   0.50    6.87    --   -8.74 -99.00-120.00   52
  3  ω    -26.00  28.00   0.50    6.87    --   -8.74 -99.00   0.00  108
  4  ω    -19.00  31.00   0.50    6.87    --   -8.74 -99.00 150.00  100
  5  ω    -84.00   5.00   0.50    6.87    --   -8.74 -46.00 -75.00  178
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0477635000
_diffrn_orient_matrix_UB_12      -0.0285101000
_diffrn_orient_matrix_UB_13      -0.0016895000
_diffrn_orient_matrix_UB_21      0.0050558000
_diffrn_orient_matrix_UB_22      -0.0002099000
_diffrn_orient_matrix_UB_23      0.0343793000
_diffrn_orient_matrix_UB_31      -0.0334586000
_diffrn_orient_matrix_UB_32      0.0407564000
_diffrn_orient_matrix_UB_33      -0.0010173000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6525
_reflns_number_total             8538
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_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 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.858
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         8538
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0564
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0923P)²+3.1146P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1565
_refine_ls_wR_factor_ref         0.1728
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C2EA(H2EA), C3EA(H3EA)
2.b Aromatic/amide H refined with riding coordinates:
 C8AA(H8AA), C6BA(H6BA), C7BA(H7BA), C8BA(H8BA), C1CA(H1CA), C3CA(H3CA),
 C4CA(H4CA), C5CA(H5CA), C6CA(H6CA), C7CA(H7CA), C8CA(H8CA), C9CA(H9CA),
 C0DA(H0DA), C1DA(H1DA), C2DA(H2DA), C3DA(H3DA), C4DA(H4DA), C5DA(H5DA),
 C6DA(H6DA), C7DA(H7DA), C8DA(H8DA), C9DA(H9DA), C0EA(H0EA), C1EA(H1EA)
;
_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
S0AA S 0.15248(5) 0.55782(4) 0.30523(3) 0.01674(15) Uani 1 1 d . . . . .
Cl0A Cl 0.24576(7) 0.35005(6) 0.41809(4) 0.0422(2) Uani 1 1 d . . . . .
Cl1A Cl 0.00897(7) 0.36890(7) 0.40376(4) 0.0440(2) Uani 1 1 d . . . . .
Cl2A Cl 0.94824(7) 0.28080(7) 0.58377(4) 0.0506(3) Uani 1 1 d . . . . .
Cl3A Cl 0.78658(10) 0.13192(7) 0.57197(4) 0.0540(3) Uani 1 1 d . . . . .
Cl4A Cl 0.14598(9) 0.46446(7) 0.50757(5) 0.0568(3) Uani 1 1 d . . . . .
Cl5A Cl 0.75875(10) 0.29052(7) 0.48551(6) 0.0707(4) Uani 1 1 d . . . . .
C0AA C 0.10254(19) 0.57813(16) 0.18070(11) 0.0150(5) Uani 1 1 d . . . . .
C1AA C -0.1796(2) 0.62999(17) 0.30771(12) 0.0187(5) Uani 1 1 d . . . . .
C2AA C -0.0874(2) 0.59464(16) 0.15327(12) 0.0168(5) Uani 1 1 d . . . . .
C3AA C -0.11271(19) 0.66441(17) 0.26387(12) 0.0175(5) Uani 1 1 d . . . . .
C4AA C 0.3152(2) 0.55944(16) 0.15796(12) 0.0162(5) Uani 1 1 d . . . . .
C5AA C -0.06748(19) 0.58424(17) 0.22694(12) 0.0168(5) Uani 1 1 d . . . . .
C6AA C 0.01213(19) 0.58980(16) 0.12656(12) 0.0168(5) Uani 1 1 d . . . . .
C7AA C 0.21908(19) 0.56602(16) 0.19263(12) 0.0155(5) Uani 1 1 d . . . . .
C8AA C 0.5124(2) 0.53287(17) 0.18487(13) 0.0198(5) Uani 1 1 d . . . . .
H8AA H 0.574945 0.523760 0.215317 0.024 Uiso 1 1 calc R . . . .
C9AA C 0.38020(19) 0.54311(16) 0.27294(12) 0.0164(5) Uani 1 1 d . . . . .
C0BA C -0.12560(19) 0.50006(17) 0.25251(12) 0.0181(5) Uani 1 1 d . . . . .
C1BA C 0.05688(19) 0.57602(16) 0.23726(12) 0.0160(5) Uani 1 1 d . . . . .
C2BA C 0.4097(2) 0.54617(16) 0.20411(12) 0.0170(5) Uani 1 1 d . . . . .
C3BA C 0.2561(2) 0.55439(16) 0.25777(12) 0.0161(5) Uani 1 1 d . . . . .
C4BA C -0.1881(2) 0.52776(17) 0.30023(12) 0.0186(5) Uani 1 1 d . . . . .
C5BA C 0.4320(2) 0.61895(17) 0.31965(12) 0.0177(5) Uani 1 1 d . . . . .
C6BA C 0.3240(2) 0.56011(18) 0.09228(13) 0.0202(5) Uani 1 1 d . . . . .
H6BA H 0.261763 0.568875 0.061582 0.024 Uiso 1 1 calc R . . . .
C7BA C -0.1867(2) 0.60797(18) 0.11436(13) 0.0216(5) Uani 1 1 d . . . . .
H7BA H -0.251746 0.613057 0.132349 0.026 Uiso 1 1 calc R . . . .
C8BA C -0.2475(2) 0.46169(19) 0.33027(13) 0.0228(5) Uani 1 1 d . . . . .
H8BA H -0.289586 0.479676 0.362000 0.027 Uiso 1 1 calc R . . . .
C9BA C 0.4847(2) 0.57859(19) 0.37702(13) 0.0207(5) Uani 1 1 d . . . . .
C0CA C 0.4195(2) 0.45448(17) 0.31007(13) 0.0191(5) Uani 1 1 d . . . . .
C1CA C -0.2269(2) 0.69115(19) 0.34781(13) 0.0236(5) Uani 1 1 d . . . . .
H1CA H -0.270773 0.668717 0.377391 0.028 Uiso 1 1 calc R . . . .
C2CA C 0.4778(2) 0.47626(18) 0.37045(12) 0.0199(5) Uani 1 1 d . . . . .
C3CA C -0.0955(2) 0.75944(18) 0.25769(13) 0.0221(5) Uani 1 1 d . . . . .
H3CA H -0.053298 0.782272 0.227397 0.027 Uiso 1 1 calc R . . . .
C4CA C 0.5196(2) 0.53354(18) 0.11810(14) 0.0226(5) Uani 1 1 d . . . . .
H4CA H 0.587700 0.524418 0.104194 0.027 Uiso 1 1 calc R . . . .
C5CA C -0.1883(2) 0.61380(19) 0.04692(14) 0.0251(6) Uani 1 1 d . . . . .
H5CA H -0.255108 0.621278 0.019904 0.030 Uiso 1 1 calc R . . . .
C6CA C 0.0104(2) 0.59689(18) 0.05983(12) 0.0212(5) Uani 1 1 d . . . . .
H6CA H 0.075512 0.593976 0.041749 0.025 Uiso 1 1 calc R . . . .
C7CA C -0.0913(2) 0.60850(19) 0.02047(13) 0.0240(5) Uani 1 1 d . . . . .
H7CA H -0.093621 0.612713 -0.024268 0.029 Uiso 1 1 calc R . . . .
C8CA C -0.1211(2) 0.40717(18) 0.23387(13) 0.0224(5) Uani 1 1 d . . . . .
H8CA H -0.079612 0.389128 0.201879 0.027 Uiso 1 1 calc R . . . .
C9CA C 0.4271(2) 0.54751(18) 0.07296(13) 0.0232(5) Uani 1 1 d . . . . .
H9CA H 0.433739 0.548520 0.029040 0.028 Uiso 1 1 calc R . . . .
C0DA C -0.2427(2) 0.3684(2) 0.31186(14) 0.0269(6) Uani 1 1 d . . . . .
H0DA H -0.281696 0.323510 0.331672 0.032 Uiso 1 1 calc R . . . .
C1DA C 0.5326(2) 0.6348(2) 0.42790(14) 0.0280(6) Uani 1 1 d . . . . .
H1DA H 0.567729 0.608186 0.466147 0.034 Uiso 1 1 calc R . . . .
C2DA C -0.1433(2) 0.82020(19) 0.29810(14) 0.0264(6) Uani 1 1 d . . . . .
H2DA H -0.132019 0.884442 0.295031 0.032 Uiso 1 1 calc R . . . .
C3DA C -0.1806(2) 0.34123(19) 0.26441(14) 0.0262(6) Uani 1 1 d . . . . .
H3DA H -0.178529 0.278377 0.252758 0.031 Uiso 1 1 calc R . . . .
C4DA C 0.4046(2) 0.36226(18) 0.28957(14) 0.0242(5) Uani 1 1 d . . . . .
H4DA H 0.366586 0.348158 0.248786 0.029 Uiso 1 1 calc R . . . .
C5DA C 0.5216(2) 0.4047(2) 0.41200(14) 0.0286(6) Uani 1 1 d . . . . .
H5DA H 0.561108 0.418641 0.452415 0.034 Uiso 1 1 calc R . . . .
C6DA C -0.2071(2) 0.7865(2) 0.34269(14) 0.0278(6) Uani 1 1 d . . . . .
H6DA H -0.237222 0.828246 0.369626 0.033 Uiso 1 1 calc R . . . .
C7DA C 0.4275(2) 0.71548(18) 0.31209(14) 0.0249(6) Uani 1 1 d . . . . .
H7DA H 0.393170 0.742288 0.273726 0.030 Uiso 1 1 calc R . . . .
C8DA C 0.4483(2) 0.2910(2) 0.33177(17) 0.0324(7) Uani 1 1 d . . . . .
H8DA H 0.438895 0.228606 0.319170 0.039 Uiso 1 1 calc R . . . .
C9DA C 0.4759(2) 0.7716(2) 0.36342(16) 0.0323(7) Uani 1 1 d . . . . .
H9DA H 0.473761 0.836520 0.359311 0.039 Uiso 1 1 calc R . . . .
C0EA C 0.5052(2) 0.3127(2) 0.39199(16) 0.0330(7) Uani 1 1 d . . . . .
H0EA H 0.533063 0.264546 0.419687 0.040 Uiso 1 1 calc R . . . .
C1EA C 0.5272(3) 0.7310(2) 0.42057(16) 0.0349(7) Uani 1 1 d . . . . .
H1EA H 0.558341 0.769286 0.454475 0.042 Uiso 1 1 calc R . . . .
C2EA C 0.1314(2) 0.3636(2) 0.45855(15) 0.0310(6) Uani 1 1 d . . . . .
H2EA H 0.127361 0.309037 0.486688 0.037 Uiso 1 1 calc R . . . .
C3EA C 0.8078(3) 0.2537(2) 0.56457(18) 0.0424(8) Uani 1 1 d . . . . .
H3EA H 0.766880 0.286805 0.594805 0.051 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S0AA C1BA 1.722(2) . ?
S0AA C3BA 1.716(2) . ?
Cl0A C2EA 1.745(3) . ?
Cl1A C2EA 1.749(3) . ?
Cl2A C3EA 1.751(4) . ?
Cl3A C3EA 1.766(4) . ?
Cl4A C2EA 1.757(3) . ?
Cl5A C3EA 1.750(4) . ?
C0AA C6AA 1.471(3) . ?
C0AA C7AA 1.422(3) . ?
C0AA C1BA 1.374(3) . ?
C1AA C3AA 1.400(3) . ?
C1AA C4BA 1.468(4) . ?
C1AA C1CA 1.390(4) . ?
C2AA C5AA 1.526(3) . ?
C2AA C6AA 1.412(3) . ?
C2AA C7BA 1.373(4) . ?
C3AA C5AA 1.525(3) . ?
C3AA C3CA 1.380(4) . ?
C4AA C7AA 1.469(3) . ?
C4AA C2BA 1.406(4) . ?
C4AA C6BA 1.387(4) . ?
C5AA C0BA 1.529(3) . ?
C5AA C1BA 1.510(3) . ?
C6AA C6CA 1.390(4) . ?
C7AA C3BA 1.377(3) . ?
C8AA H8AA 0.9300 . ?
C8AA C2BA 1.386(3) . ?
C8AA C4CA 1.406(4) . ?
C9AA C2BA 1.528(3) . ?
C9AA C3BA 1.515(3) . ?
C9AA C5BA 1.530(3) . ?
C9AA C0CA 1.523(3) . ?
C0BA C4BA 1.395(3) . ?
C0BA C8CA 1.384(4) . ?
C4BA C8BA 1.392(4) . ?
C5BA C9BA 1.398(4) . ?
C5BA C7DA 1.386(4) . ?
C6BA H6BA 0.9300 . ?
C6BA C9CA 1.389(4) . ?
C7BA H7BA 0.9300 . ?
C7BA C5CA 1.404(4) . ?
C8BA H8BA 0.9300 . ?
C8BA C0DA 1.388(4) . ?
C9BA C2CA 1.467(4) . ?
C9BA C1DA 1.390(4) . ?
C0CA C2CA 1.389(4) . ?
C0CA C4DA 1.387(4) . ?
C1CA H1CA 0.9300 . ?
C1CA C6DA 1.387(4) . ?
C2CA C5DA 1.394(4) . ?
C3CA H3CA 0.9300 . ?
C3CA C2DA 1.393(4) . ?
C4CA H4CA 0.9300 . ?
C4CA C9CA 1.378(4) . ?
C5CA H5CA 0.9300 . ?
C5CA C7CA 1.380(4) . ?
C6CA H6CA 0.9300 . ?
C6CA C7CA 1.398(4) . ?
C7CA H7CA 0.9300 . ?
C8CA H8CA 0.9300 . ?
C8CA C3DA 1.397(4) . ?
C9CA H9CA 0.9300 . ?
C0DA H0DA 0.9300 . ?
C0DA C3DA 1.385(4) . ?
C1DA H1DA 0.9300 . ?
C1DA C1EA 1.381(5) . ?
C2DA H2DA 0.9300 . ?
C2DA C6DA 1.383(4) . ?
C3DA H3DA 0.9300 . ?
C4DA H4DA 0.9300 . ?
C4DA C8DA 1.399(4) . ?
C5DA H5DA 0.9300 . ?
C5DA C0EA 1.382(5) . ?
C6DA H6DA 0.9300 . ?
C7DA H7DA 0.9300 . ?
C7DA C9DA 1.397(4) . ?
C8DA H8DA 0.9300 . ?
C8DA C0EA 1.380(5) . ?
C9DA H9DA 0.9300 . ?
C9DA C1EA 1.390(5) . ?
C0EA H0EA 0.9300 . ?
C1EA H1EA 0.9300 . ?
C2EA H2EA 0.9800 . ?
C3EA H3EA 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
C3BA S0AA C1BA 90.10(11) . . ?
C7AA C0AA C6AA 140.6(2) . . ?
C1BA C0AA C6AA 107.8(2) . . ?
C1BA C0AA C7AA 111.6(2) . . ?
C3AA C1AA C4BA 108.6(2) . . ?
C1CA C1AA C3AA 120.3(2) . . ?
C1CA C1AA C4BA 131.1(2) . . ?
C6AA C2AA C5AA 111.6(2) . . ?
C7BA C2AA C5AA 127.4(2) . . ?
C7BA C2AA C6AA 121.0(2) . . ?
C1AA C3AA C5AA 110.8(2) . . ?
C3CA C3AA C1AA 121.1(2) . . ?
C3CA C3AA C5AA 128.2(2) . . ?
C2BA C4AA C7AA 108.1(2) . . ?
C6BA C4AA C7AA 131.7(2) . . ?
C6BA C4AA C2BA 120.1(2) . . ?
C2AA C5AA C0BA 114.3(2) . . ?
C3AA C5AA C2AA 114.6(2) . . ?
C3AA C5AA C0BA 101.10(19) . . ?
C1BA C5AA C2AA 99.39(19) . . ?
C1BA C5AA C3AA 114.7(2) . . ?
C1BA C5AA C0BA 113.5(2) . . ?
C2AA C6AA C0AA 107.5(2) . . ?
C6CA C6AA C0AA 132.6(2) . . ?
C6CA C6AA C2AA 120.0(2) . . ?
C0AA C7AA C4AA 140.8(2) . . ?
C3BA C7AA C0AA 111.5(2) . . ?
C3BA C7AA C4AA 107.7(2) . . ?
C2BA C8AA H8AA 120.9 . . ?
C2BA C8AA C4CA 118.2(2) . . ?
C4CA C8AA H8AA 120.9 . . ?
C2BA C9AA C5BA 116.39(19) . . ?
C3BA C9AA C2BA 99.54(19) . . ?
C3BA C9AA C5BA 111.65(19) . . ?
C3BA C9AA C0CA 115.32(19) . . ?
C0CA C9AA C2BA 113.59(19) . . ?
C0CA C9AA C5BA 101.08(19) . . ?
C4BA C0BA C5AA 110.8(2) . . ?
C8CA C0BA C5AA 127.9(2) . . ?
C8CA C0BA C4BA 121.2(2) . . ?
C0AA C1BA S0AA 113.33(18) . . ?
C0AA C1BA C5AA 113.7(2) . . ?
C5AA C1BA S0AA 132.87(18) . . ?
C4AA C2BA C9AA 111.3(2) . . ?
C8AA C2BA C4AA 120.8(2) . . ?
C8AA C2BA C9AA 127.8(2) . . ?
C7AA C3BA S0AA 113.46(18) . . ?
C7AA C3BA C9AA 113.3(2) . . ?
C9AA C3BA S0AA 133.18(18) . . ?
C0BA C4BA C1AA 108.6(2) . . ?
C8BA C4BA C1AA 131.1(2) . . ?
C8BA C4BA C0BA 120.2(2) . . ?
C9BA C5BA C9AA 110.5(2) . . ?
C7DA C5BA C9AA 128.6(2) . . ?
C7DA C5BA C9BA 120.8(2) . . ?
C4AA C6BA H6BA 120.4 . . ?
C4AA C6BA C9CA 119.1(2) . . ?
C9CA C6BA H6BA 120.4 . . ?
C2AA C7BA H7BA 120.6 . . ?
C2AA C7BA C5CA 118.9(2) . . ?
C5CA C7BA H7BA 120.6 . . ?
C4BA C8BA H8BA 120.7 . . ?
C0DA C8BA C4BA 118.6(2) . . ?
C0DA C8BA H8BA 120.7 . . ?
C5BA C9BA C2CA 108.4(2) . . ?
C1DA C9BA C5BA 120.4(3) . . ?
C1DA C9BA C2CA 131.1(3) . . ?
C2CA C0CA C9AA 111.0(2) . . ?
C4DA C0CA C9AA 127.8(2) . . ?
C4DA C0CA C2CA 121.2(2) . . ?
C1AA C1CA H1CA 120.8 . . ?
C6DA C1CA C1AA 118.5(2) . . ?
C6DA C1CA H1CA 120.8 . . ?
C0CA C2CA C9BA 108.8(2) . . ?
C0CA C2CA C5DA 120.0(3) . . ?
C5DA C2CA C9BA 131.1(3) . . ?
C3AA C3CA H3CA 120.9 . . ?
C3AA C3CA C2DA 118.2(2) . . ?
C2DA C3CA H3CA 120.9 . . ?
C8AA C4CA H4CA 119.5 . . ?
C9CA C4CA C8AA 120.9(2) . . ?
C9CA C4CA H4CA 119.5 . . ?
C7BA C5CA H5CA 119.8 . . ?
C7CA C5CA C7BA 120.4(2) . . ?
C7CA C5CA H5CA 119.8 . . ?
C6AA C6CA H6CA 120.7 . . ?
C6AA C6CA C7CA 118.7(2) . . ?
C7CA C6CA H6CA 120.7 . . ?
C5CA C7CA C6CA 121.1(3) . . ?
C5CA C7CA H7CA 119.5 . . ?
C6CA C7CA H7CA 119.5 . . ?
C0BA C8CA H8CA 120.9 . . ?
C0BA C8CA C3DA 118.2(2) . . ?
C3DA C8CA H8CA 120.9 . . ?
C6BA C9CA H9CA 119.6 . . ?
C4CA C9CA C6BA 120.8(3) . . ?
C4CA C9CA H9CA 119.6 . . ?
C8BA C0DA H0DA 119.5 . . ?
C3DA C0DA C8BA 121.0(2) . . ?
C3DA C0DA H0DA 119.5 . . ?
C9BA C1DA H1DA 120.6 . . ?
C1EA C1DA C9BA 118.7(3) . . ?
C1EA C1DA H1DA 120.6 . . ?
C3CA C2DA H2DA 119.5 . . ?
C6DA C2DA C3CA 121.0(3) . . ?
C6DA C2DA H2DA 119.5 . . ?
C8CA C3DA H3DA 119.6 . . ?
C0DA C3DA C8CA 120.7(3) . . ?
C0DA C3DA H3DA 119.6 . . ?
C0CA C4DA H4DA 120.8 . . ?
C0CA C4DA C8DA 118.3(3) . . ?
C8DA C4DA H4DA 120.8 . . ?
C2CA C5DA H5DA 120.6 . . ?
C0EA C5DA C2CA 118.8(3) . . ?
C0EA C5DA H5DA 120.6 . . ?
C1CA C6DA H6DA 119.5 . . ?
C2DA C6DA C1CA 120.9(2) . . ?
C2DA C6DA H6DA 119.5 . . ?
C5BA C7DA H7DA 120.8 . . ?
C5BA C7DA C9DA 118.5(3) . . ?
C9DA C7DA H7DA 120.8 . . ?
C4DA C8DA H8DA 119.8 . . ?
C0EA C8DA C4DA 120.3(3) . . ?
C0EA C8DA H8DA 119.8 . . ?
C7DA C9DA H9DA 119.8 . . ?
C1EA C9DA C7DA 120.4(3) . . ?
C1EA C9DA H9DA 119.8 . . ?
C5DA C0EA H0EA 119.3 . . ?
C8DA C0EA C5DA 121.3(3) . . ?
C8DA C0EA H0EA 119.3 . . ?
C1DA C1EA C9DA 121.2(3) . . ?
C1DA C1EA H1EA 119.4 . . ?
C9DA C1EA H1EA 119.4 . . ?
Cl0A C2EA Cl1A 111.14(17) . . ?
Cl0A C2EA Cl4A 110.45(17) . . ?
Cl0A C2EA H2EA 108.2 . . ?
Cl1A C2EA Cl4A 110.50(17) . . ?
Cl1A C2EA H2EA 108.2 . . ?
Cl4A C2EA H2EA 108.2 . . ?
Cl2A C3EA Cl3A 110.41(19) . . ?
Cl2A C3EA H3EA 108.8 . . ?
Cl3A C3EA H3EA 108.8 . . ?
Cl5A C3EA Cl2A 110.0(2) . . ?
Cl5A C3EA Cl3A 110.00(18) . . ?
Cl5A C3EA H3EA 108.8 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.628
_oxdiff_exptl_absorpt_empirical_full_min 0.680
####################################################################### 
# 
# 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_kato_210123_1
_database_code_depnum_ccdc_archive 'CCDC 2305244'
loop_
_audit_author_name
_audit_author_address
'Koji Hirano'
;Osaka University
Japan
;
_audit_update_record             
;
2023-11-02 deposited with the CCDC.	2024-01-02 downloaded from the CCDC.
;
_audit_creation_date             2021-01-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C84 H92 S2'
_chemical_formula_sum            'C84 H92 S2'
_chemical_formula_weight         1165.69
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C84 S2 H92'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   22.0314(4)
_cell_length_b                   12.4409(2)
_cell_length_c                   26.6247(4)
_cell_angle_alpha                90
_cell_angle_beta                 112.159(2)
_cell_angle_gamma                90
_cell_volume                     6758.6(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    38469
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      73.9500
_cell_measurement_theta_min      3.4360
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.039
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.43a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2512
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 -7 8 0.0499
3 -5 -13 0.1705
4 6 -12 0.0891
-1 7 7 0.1027
-1 -4 14 0.1155
13 0 -1 0.0389
-13 0 0 0.0519
2 -7 6 0.0406
6 3 -16 0.1127
-2 7 -6 0.0878
-10 4 -5 0.0630
-3 6 -10 0.0715

_exptl_crystal_size_max          0.353
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.092
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-3.0758 -7.1346 8.0590 0.5269 -0.0134 0.8498
3.0377 -5.3865 -12.8143 0.9532 -0.0249 -0.3013
3.9533 5.9795 -11.6041 -0.2990 0.0074 -0.9542
-1.1437 7.3755 6.9129 -0.9927 0.0258 -0.1180
-0.7979 -3.8670 14.3838 -0.0230 0.2802 0.9597
13.3980 0.4159 -0.5616 -0.0785 0.9953 -0.0565
-13.3503 -0.3675 0.3845 0.0785 -0.9959 0.0446
2.0928 -7.2643 5.6286 0.5950 0.3231 0.7359
6.0334 2.9375 -16.0398 0.1525 0.0830 -0.9848
-1.9778 7.2405 -5.8267 -0.5869 -0.3187 -0.7443
-9.5855 3.6904 -4.9901 -0.2047 -0.8539 -0.4785
-2.5714 5.5471 -10.0952 -0.2740 -0.4486 -0.8507

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1631
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            100922
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.927
_diffrn_reflns_theta_min         3.418
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -54.00  32.00   0.50    0.47    --  -42.80  49.00  37.00  172
  2  ω    -19.00  17.00   0.50    0.47    --   42.80 -49.00-109.00   72
  3  ω     26.00  51.00   0.50    1.93    --   76.50 -49.00-109.00   50
  4  ω     12.00  64.00   0.50    0.47    --   42.80 -57.00-180.00  104
  5  ω     14.00  89.00   0.50    0.47    --   42.80-125.00-180.00  150
  6  ω     69.00  94.00   0.50    0.47    --   42.80  49.00  37.00   50
  7  ω     97.00 123.00   0.50    1.93    --   76.50  49.00  37.00   52
  8  ω     87.00 116.00   0.50    0.47    --   42.80 125.00  90.00   58
  9  ω     71.00 126.00   0.50    1.93    --   76.50 125.00 -60.00  110
 10  ω    -55.00 -30.00   0.50    1.93    -- -106.00  19.00-120.00   50
 11  ω    -90.00 -32.00   0.50    1.93    -- -106.00  77.00 -90.00  116
 12  ω    -72.00 -32.00   0.50    1.93    -- -106.00 125.00-180.00   80
 13  ω    -84.00 -58.00   0.50    1.93    -- -106.00 125.00-150.00   52
 14  ω    -91.00 -32.00   0.50    1.93    -- -106.00  77.00-120.00  118
 15  ω    -85.00 -59.00   0.50    1.93    -- -106.00  49.00  37.00   52
 16  ω    -72.00 -40.00   0.50    1.93    -- -106.00  77.00  60.00   64
 17  ω    -95.00 -69.00   0.50    1.93    -- -106.00 125.00  60.00   52
 18  ω    -88.00 -62.00   0.50    1.93    -- -106.00  77.00  30.00   52
 19  ω   -111.00 -33.00   0.50    1.93    -- -106.00 125.00  90.00  156
 20  ω    -95.00 -10.00   0.50    0.47    --  -42.80 125.00  30.00  170
 21  ω   -117.00 -92.00   0.50    1.93    -- -106.00 125.00-180.00   50
 22  ω   -116.00 -32.00   0.50    1.93    -- -106.00 125.00-120.00  168
 23  ω   -107.00 -32.00   0.50    1.93    -- -106.00 125.00  30.00  150
 24  ω   -126.00 -82.00   0.50    1.93    -- -106.00  77.00  60.00   88
 25  ω   -125.00 -62.00   0.50    1.93    -- -106.00  57.00 150.00  126
 26  ω   -127.00 -94.00   0.50    1.93    -- -106.00 139.00 160.14   66
 27  ω   -129.00 -34.00   0.50    1.93    -- -106.00 142.00  80.73  190
 28  ω   -124.00 -38.00   0.50    1.93    -- -106.00 134.00 -83.91  172
 29  ω   -115.00 -63.00   0.50    1.93    -- -106.00 125.00 -90.00  104
 30  ω   -127.00 -79.00   0.50    1.93    -- -106.00  57.00 -90.00   96
 31  ω   -128.00-102.00   0.50    1.93    -- -106.00  19.00-120.00   52
 32  ω   -126.00 -61.00   0.50    1.93    -- -106.00  57.00-120.00  130
 33  ω   -127.00 -33.00   0.50    1.93    -- -106.00 139.00 -32.03  188
 34  ω   -135.00-110.00   0.50    1.93    -- -106.00  77.00-150.00   50
 35  ω   -131.00 -99.00   0.50    1.93    -- -106.00 145.00  -3.03   64
 36  ω   -135.00 -91.00   0.50    1.93    -- -106.00  77.00  30.00   88
 37  ω   -117.00 -20.00   0.50    0.47    --  -42.80 -49.00-109.00  194
 38  ω   -112.00 -78.00   0.50    0.47    --  -42.80-125.00-150.00   68
 39  ω   -139.00-113.00   0.50    1.93    -- -106.00 -49.00-109.00   52
 40  ω   -137.00-111.00   0.50    1.93    -- -106.00 -57.00 -90.00   52
 41  ω   -141.00 -84.00   0.50    1.93    -- -106.00 -99.00 -30.00  114
 42  ω   -127.00 -77.00   0.50    1.93    -- -106.00 -77.00  30.00  100
 43  ω   -177.00 -98.00   0.50    1.93    -- -106.00 -57.00-150.00  158
 44  ω   -177.00 -90.00   0.50    1.93    -- -106.00 -57.00-180.00  174
 45  ω   -176.00-150.00   0.50    1.93    -- -106.00 -57.00 -90.00   52
 46  ω   -166.00-141.00   0.50    1.93    -- -106.00 -77.00  30.00   50
 47  ω   -175.00 -83.00   0.50    1.93    -- -106.00 -37.00  60.00  184
 48  ω   -177.00 -86.00   0.50    1.93    -- -106.00 -37.00  90.00  182
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0038246000
_diffrn_orient_matrix_UB_12      -0.1066226000
_diffrn_orient_matrix_UB_13      -0.0304744000
_diffrn_orient_matrix_UB_21      0.0753906000
_diffrn_orient_matrix_UB_22      -0.0055881000
_diffrn_orient_matrix_UB_23      0.0221629000
_diffrn_orient_matrix_UB_31      -0.0001791000
_diffrn_orient_matrix_UB_32      -0.0627383000
_diffrn_orient_matrix_UB_33      0.0498410000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10865
_reflns_number_total             13697
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.324
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.384
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     890
_refine_ls_number_reflns         13697
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.1079
_refine_ls_R_factor_gt           0.0946
_refine_ls_restrained_S_all      1.382
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2904
_refine_ls_wR_factor_ref         0.3334
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C67, C66, C65, C64, C63, C62
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Rigid body (RIGU) restrains
 C62, C63, C64, C65, C66, C67
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H61C)=Sof(H61D)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=Sof(C67)=Sof(H67A)=
 Sof(H67B)=Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(C64)=
 Sof(H64A)=Sof(H64B)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(C62)=Sof(H62A)=Sof(H62B)=
 1-FVAR(1)
 Sof(H61A)=Sof(H61B)=Sof(C01U)=Sof(H01E)=Sof(H01F)=Sof(C01V)=Sof(H01G)=
 Sof(H01H)=Sof(C01X)=Sof(H01K)=Sof(H01L)=Sof(H01M)=Sof(C020)=Sof(H02A)=
 Sof(H02B)=Sof(C021)=Sof(H02C)=Sof(H02D)=Sof(C022)=Sof(H02E)=Sof(H02F)=
 Sof(C023)=Sof(H02G)=Sof(H02H)=FVAR(1)
 Fixed Sof: H02K(0.5) H02L(0.5) H02I(0.5) H02J(0.5) C7AA(0.5) H7AA(0.5)
 H7AB(0.5) C4AA(0.5) H4AA(0.5) H4AB(0.5) H4AC(0.5) C5AA(0.5) H5AA(0.5)
 H5AB(0.5) C6AA(0.5) H6AA(0.5) H6AB(0.5) C0AA(0.5) H0AA(0.5) H0AB(0.5)
 C1BA(0.5) H1BA(0.5) H1BB(0.5) C3BA(0.5) H3BA(0.5) H3BB(0.5) H3BC(0.5)
 C9AA(0.5) H9AA(0.5) H9AB(0.5) C2BA(0.5) H2BA(0.5) H2BB(0.5) C0BA(0.5)
 H0BA(0.5) H0BB(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C56(H56A,H56B), C54(H54A,H54B), C55(H55A,H55B), C58(H58A,H58B), C53(H53A,
 H53B), C57(H57A,H57B), C59(H59A,H59B), C01Q(H01A,H01B), C01R(H01C,H01D),
 C61(H61A,H61B), C61(H61C,H61D), C01U(H01E,H01F), C01V(H01G,H01H), C01W(H01I,
 H01J), C01Y(H01N,H01O), C01Z(H01P,H01Q), C020(H02A,H02B), C021(H02C,H02D),
 C022(H02E,H02F), C023(H02G,H02H), C029(H02K,H02L), C029(H02I,H02J), C02A(H02M,
 H02N), C7AA(H7AA,H7AB), C5AA(H5AA,H5AB), C6AA(H6AA,H6AB), C0AA(H0AA,H0AB),
 C67(H67A,H67B), C66(H66A,H66B), C65(H65A,H65B), C64(H64A,H64B), C63(H63A,H63B),
  C62(H62A,H62B), C3AA(H3AA,H3AB), C1AA(H1AA,H1AB), C2AA(H2AA,H2AB), C1BA(H1BA,
 H1BB), C9AA(H9AA,H9AB), C2BA(H2BA,H2BB), C0BA(H0BA,H0BB)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C16(H16), C17(H17), C13(H13), C42(H42), C30(H30), C3(H3), C6(H6),
 C49(H49), C24(H24), C39(H39), C2(H2), C27(H27), C36(H36), C51(H51), C1(H1),
 C25(H25), C33(H33), C43(H43), C26(H26), C52(H52), C32(H32), C45(H45), C37(H37)
5.c Idealised Me refined as rotating group:
 C60(H60A,H60B,H60C), C01X(H01K,H01L,H01M), C4AA(H4AA,H4AB,H4AC), C68(H68A,
 H68B,H68C), C8AA(H8AA,H8AB,H8AC), C3BA(H3BA,H3BB,H3BC)
;
_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
S001 S 0.26093(3) 0.62200(6) 0.28539(2) 0.0431(2) Uani 1 1 d . . . . .
S002 S 0.23693(3) 0.59804(6) 0.71729(2) 0.0475(2) Uani 1 1 d . . . . .
C14 C 0.22328(10) 0.55329(17) 0.51060(8) 0.0305(4) Uani 1 1 d . . . . .
C15 C 0.27605(11) 0.56130(17) 0.49121(8) 0.0309(5) Uani 1 1 d . . . . .
C7 C 0.19209(12) 0.57962(17) 0.34347(8) 0.0332(5) Uani 1 1 d . . . . .
C11 C 0.19411(11) 0.56201(18) 0.39863(8) 0.0329(5) Uani 1 1 d . . . . .
C10 C 0.25893(11) 0.56541(18) 0.43402(8) 0.0320(5) Uani 1 1 d . . . . .
C18 C 0.30487(12) 0.57073(17) 0.60267(8) 0.0334(5) Uani 1 1 d . . . . .
C5 C 0.14453(12) 0.58892(18) 0.28898(9) 0.0359(5) Uani 1 1 d . . . . .
C12 C 0.14280(11) 0.5497(2) 0.41757(9) 0.0372(5) Uani 1 1 d . . . . .
H12 H 0.099568 0.544596 0.393270 0.045 Uiso 1 1 calc R . . . .
C16 C 0.34171(11) 0.56949(19) 0.52860(9) 0.0359(5) Uani 1 1 d . . . . .
H16 H 0.375433 0.571629 0.515649 0.043 Uiso 1 1 calc R . . . .
C17 C 0.35676(12) 0.5744(2) 0.58368(9) 0.0369(5) Uani 1 1 d . . . . .
H17 H 0.400043 0.579897 0.607823 0.044 Uiso 1 1 calc R . . . .
C22 C 0.30617(12) 0.58332(18) 0.65778(9) 0.0343(5) Uani 1 1 d . . . . .
C19 C 0.24020(11) 0.55880(17) 0.56751(8) 0.0316(4) Uani 1 1 d . . . . .
C13 C 0.15770(11) 0.54524(19) 0.47265(9) 0.0361(5) Uani 1 1 d . . . . .
H13 H 0.123981 0.536764 0.485295 0.043 Uiso 1 1 calc R . . . .
C41 C 0.15079(12) 0.4667(2) 0.59663(8) 0.0371(5) Uani 1 1 d . . . . .
C23 C 0.35402(13) 0.59460(18) 0.71203(9) 0.0368(5) Uani 1 1 d . . . . .
C20 C 0.19372(11) 0.56586(19) 0.59827(8) 0.0354(5) Uani 1 1 d . . . . .
C9 C 0.30499(11) 0.58755(19) 0.40392(8) 0.0338(5) Uani 1 1 d . . . . .
C21 C 0.24352(12) 0.58362(19) 0.65504(9) 0.0371(5) Uani 1 1 d . . . . .
C8 C 0.25455(12) 0.59514(18) 0.34670(9) 0.0345(5) Uani 1 1 d . . . . .
C48 C 0.14190(12) 0.6534(2) 0.57759(8) 0.0400(5) Uani 1 1 d . . . . .
C29 C 0.35854(11) 0.5051(2) 0.40953(8) 0.0370(5) Uani 1 1 d . . . . .
C40 C 0.34537(12) 0.6903(2) 0.42317(8) 0.0397(5) Uani 1 1 d . . . . .
C42 C 0.17059(13) 0.3627(2) 0.61282(9) 0.0409(5) Uani 1 1 d . . . . .
H42 H 0.214529 0.344141 0.623245 0.049 Uiso 1 1 calc R . . . .
C34 C 0.42001(12) 0.5564(2) 0.42638(9) 0.0435(6) Uani 1 1 d . . . . .
C4 C 0.17619(14) 0.61287(19) 0.25284(9) 0.0403(5) Uani 1 1 d . . . . .
C28 C 0.32163(15) 0.6034(2) 0.74906(10) 0.0443(6) Uani 1 1 d . . . . .
C46 C 0.08495(12) 0.4969(2) 0.58045(8) 0.0426(6) Uani 1 1 d . . . . .
C30 C 0.35202(14) 0.3962(2) 0.39874(10) 0.0443(6) Uani 1 1 d . . . . .
H30 H 0.311190 0.363126 0.387366 0.053 Uiso 1 1 calc R . . . .
C47 C 0.07932(13) 0.6122(2) 0.56826(9) 0.0442(6) Uani 1 1 d . . . . .
C3 C 0.14037(15) 0.6268(2) 0.19711(10) 0.0470(6) Uani 1 1 d . . . . .
H3 H 0.161456 0.641686 0.173509 0.056 Uiso 1 1 calc R . . . .
C6 C 0.07619(14) 0.5797(2) 0.26843(10) 0.0456(6) Uani 1 1 d . . . . .
H6 H 0.054510 0.563492 0.291440 0.055 Uiso 1 1 calc R . . . .
C35 C 0.41164(12) 0.6710(2) 0.43528(9) 0.0431(6) Uani 1 1 d . . . . .
C49 C 0.15066(14) 0.7601(2) 0.56678(9) 0.0451(6) Uani 1 1 d . . . . .
H49 H 0.192393 0.786775 0.573313 0.054 Uiso 1 1 calc R . . . .
C44 C 0.12532(14) 0.2857(2) 0.61365(10) 0.0486(6) Uani 1 1 d . . . . .
C24 C 0.42234(14) 0.5955(2) 0.73189(10) 0.0460(6) Uani 1 1 d . . . . .
H24 H 0.444234 0.589622 0.708210 0.055 Uiso 1 1 calc R . . . .
C39 C 0.32374(15) 0.7904(2) 0.43124(10) 0.0472(6) Uani 1 1 d . . . . .
H39 H 0.279250 0.802128 0.422577 0.057 Uiso 1 1 calc R . . . .
C31 C 0.40964(15) 0.3360(2) 0.40554(11) 0.0517(7) Uani 1 1 d . . . . .
C2 C 0.07351(16) 0.6179(2) 0.17844(10) 0.0539(7) Uani 1 1 d . . . . .
H2 H 0.049105 0.627351 0.141657 0.065 Uiso 1 1 calc R . . . .
C27 C 0.35807(16) 0.6150(2) 0.80507(10) 0.0508(7) Uani 1 1 d . . . . .
H27 H 0.337070 0.622233 0.829326 0.061 Uiso 1 1 calc R . . . .
C36 C 0.45668(16) 0.7551(3) 0.45547(11) 0.0562(7) Uani 1 1 d . . . . .
H36 H 0.501058 0.744120 0.463230 0.067 Uiso 1 1 calc R . . . .
C51 C 0.03421(16) 0.7850(3) 0.53748(11) 0.0583(8) Uani 1 1 d . . . . .
H51 H -0.002095 0.829928 0.524083 0.070 Uiso 1 1 calc R . . . .
C50 C 0.09556(16) 0.8273(2) 0.54582(10) 0.0530(7) Uani 1 1 d . . . . .
C1 C 0.04100(15) 0.5949(3) 0.21330(11) 0.0535(7) Uani 1 1 d . . . . .
H1 H -0.004474 0.589862 0.199505 0.064 Uiso 1 1 calc R . . . .
C38 C 0.36820(17) 0.8740(2) 0.45230(11) 0.0565(7) Uani 1 1 d . . . . .
C25 C 0.45747(17) 0.6053(3) 0.78738(11) 0.0559(7) Uani 1 1 d . . . . .
H25 H 0.503040 0.605346 0.800841 0.067 Uiso 1 1 calc R . . . .
C33 C 0.47591(14) 0.4980(3) 0.43310(11) 0.0527(6) Uani 1 1 d . . . . .
H33 H 0.516670 0.531259 0.444299 0.063 Uiso 1 1 calc R . . . .
C43 C 0.05933(16) 0.3158(3) 0.59671(11) 0.0582(8) Uani 1 1 d . . . . .
H43 H 0.028431 0.264713 0.596551 0.070 Uiso 1 1 calc R . . . .
C26 C 0.42486(18) 0.6152(3) 0.82295(11) 0.0586(8) Uani 1 1 d . . . . .
H26 H 0.449263 0.622082 0.859886 0.070 Uiso 1 1 calc R . . . .
C52 C 0.02470(15) 0.6791(3) 0.54818(10) 0.0566(8) Uani 1 1 d . . . . .
H52 H -0.017046 0.653039 0.542150 0.068 Uiso 1 1 calc R . . . .
C56 C 0.17557(16) 0.2080(2) 0.78890(11) 0.0554(7) Uani 1 1 d . . . . .
H56A H 0.204673 0.269504 0.795806 0.066 Uiso 1 1 calc R . . . .
H56B H 0.202433 0.144506 0.801989 0.066 Uiso 1 1 calc R . . . .
C32 C 0.46972(15) 0.3895(3) 0.42281(12) 0.0567(7) Uani 1 1 d . . . . .
H32 H 0.507283 0.349870 0.427563 0.068 Uiso 1 1 calc R . . . .
C45 C 0.03895(14) 0.4201(3) 0.58014(11) 0.0541(7) Uani 1 1 d . . . . .
H45 H -0.005117 0.438416 0.568921 0.065 Uiso 1 1 calc R . . . .
C54 C 0.18323(17) 0.1751(2) 0.69757(12) 0.0569(7) Uani 1 1 d . . . . .
H54A H 0.204055 0.105773 0.708914 0.068 Uiso 1 1 calc R . . . .
H54B H 0.217454 0.229180 0.707529 0.068 Uiso 1 1 calc R . . . .
C55 C 0.13825(17) 0.1974(3) 0.72796(12) 0.0584(7) Uani 1 1 d . . . . .
H55A H 0.106708 0.139411 0.721054 0.070 Uiso 1 1 calc R . . . .
H55B H 0.114168 0.263298 0.714231 0.070 Uiso 1 1 calc R . . . .
C37 C 0.43403(18) 0.8541(2) 0.46361(12) 0.0596(8) Uani 1 1 d . . . . .
H37 H 0.463970 0.909724 0.477188 0.072 Uiso 1 1 calc R . . . .
C58 C 0.16788(16) 0.2394(3) 0.88125(12) 0.0561(7) Uani 1 1 d . . . . .
H58A H 0.193515 0.304814 0.886463 0.067 Uiso 1 1 calc R . . . .
H58B H 0.198156 0.180277 0.895697 0.067 Uiso 1 1 calc R . . . .
C53 C 0.14791(18) 0.1750(2) 0.63600(12) 0.0596(8) Uani 1 1 d . . . . .
H53A H 0.177192 0.146916 0.619603 0.072 Uiso 1 1 calc R . . . .
H53B H 0.110253 0.127557 0.626187 0.072 Uiso 1 1 calc R . . . .
C57 C 0.13114(18) 0.2217(3) 0.82078(13) 0.0614(8) Uani 1 1 d . . . . .
H57A H 0.102293 0.282463 0.806046 0.074 Uiso 1 1 calc R . . . .
H57B H 0.103971 0.158132 0.815643 0.074 Uiso 1 1 calc R . . . .
C59 C 0.12357(17) 0.2481(3) 0.91337(12) 0.0571(7) Uani 1 1 d . . . . .
H59A H 0.094414 0.309016 0.899929 0.069 Uiso 1 1 calc R . . . .
H59B H 0.096763 0.183921 0.907173 0.069 Uiso 1 1 calc R . . . .
C01Q C 0.1021(2) 0.9407(2) 0.52952(12) 0.0670(9) Uani 1 1 d . . . . .
H01A H 0.147881 0.961655 0.545180 0.080 Uiso 1 1 calc R . . . .
H01B H 0.077804 0.987983 0.544091 0.080 Uiso 1 1 calc R . . . .
C01R C 0.0771(2) 0.9549(3) 0.46824(13) 0.0671(9) Uani 1 1 d . . . . .
H01C H 0.031474 0.933209 0.452725 0.080 Uiso 1 1 calc R . . . .
H01D H 0.079213 1.030484 0.460145 0.080 Uiso 1 1 calc R . . . .
C61 C 0.4054(2) 0.2174(3) 0.39420(15) 0.0696(9) Uani 1 1 d . . . . .
H61A H 0.360188 0.194243 0.383446 0.083 Uiso 0.673(6) 1 calc R . P A 1
H61B H 0.431208 0.179088 0.427063 0.083 Uiso 0.673(6) 1 calc R . P A 1
H61C H 0.387676 0.181776 0.418111 0.083 Uiso 0.327(6) 1 calc R . P A 2
H61D H 0.449119 0.189439 0.402112 0.083 Uiso 0.327(6) 1 calc R . P A 2
C60 C 0.16084(19) 0.2617(3) 0.97380(13) 0.0683(9) Uani 1 1 d . . . . .
H60A H 0.185936 0.326872 0.980444 0.102 Uiso 1 1 calc GR . . . .
H60B H 0.189781 0.201644 0.987492 0.102 Uiso 1 1 calc GR . . . .
H60C H 0.130407 0.265015 0.991758 0.102 Uiso 1 1 calc GR . . . .
C01U C 0.3804(4) 0.2136(11) 0.2927(3) 0.059(2) Uani 0.673(6) 1 d . . P A 1
H01E H 0.364518 0.286479 0.292242 0.071 Uiso 0.673(6) 1 calc R . P A 1
H01F H 0.343341 0.165475 0.284866 0.071 Uiso 0.673(6) 1 calc R . P A 1
C01V C 0.3838(4) 0.2090(10) 0.1466(4) 0.069(2) Uani 0.673(6) 1 d . . P A 1
H01G H 0.404125 0.139264 0.148280 0.083 Uiso 0.673(6) 1 calc R . P A 1
H01H H 0.417734 0.263001 0.153298 0.083 Uiso 0.673(6) 1 calc R . P A 1
C01W C 0.1147(2) 0.8918(3) 0.44168(14) 0.0766(11) Uani 1 1 d . . . . .
H01I H 0.108828 0.815675 0.446376 0.092 Uiso 1 1 calc R . . . .
H01J H 0.160990 0.907946 0.459528 0.092 Uiso 1 1 calc R . . . .
C01X C 0.3586(5) 0.2247(13) 0.0404(6) 0.065(2) Uani 0.673(6) 1 d . . P A 1
H01K H 0.385956 0.286361 0.043273 0.098 Uiso 0.673(6) 1 calc GR . P A 1
H01L H 0.321825 0.227011 0.006455 0.098 Uiso 0.673(6) 1 calc GR . P A 1
H01M H 0.383445 0.160422 0.042080 0.098 Uiso 0.673(6) 1 calc GR . P A 1
C01Y C 0.0933(2) 0.9160(3) 0.38165(15) 0.0768(11) Uani 1 1 d . . . . .
H01N H 0.047045 0.899438 0.363964 0.092 Uiso 1 1 calc R . . . .
H01O H 0.098674 0.992351 0.377139 0.092 Uiso 1 1 calc R . . . .
C01Z C 0.3455(3) 0.9809(3) 0.46639(18) 0.0858(12) Uani 1 1 d . . . . .
H01P H 0.307962 1.006252 0.435749 0.103 Uiso 1 1 calc R . . . .
H01Q H 0.380325 1.033484 0.473840 0.103 Uiso 1 1 calc R . . . .
C020 C 0.3576(3) 0.2153(4) 0.1912(2) 0.0631(14) Uani 0.673(6) 1 d . . P A 1
H02A H 0.324456 0.160033 0.184873 0.076 Uiso 0.673(6) 1 calc R . P A 1
H02B H 0.336113 0.284269 0.188699 0.076 Uiso 0.673(6) 1 calc R . P A 1
C021 C 0.4076(3) 0.2024(4) 0.2480(2) 0.0651(14) Uani 0.673(6) 1 d . . P A 1
H02C H 0.441679 0.255732 0.253909 0.078 Uiso 0.673(6) 1 calc R . P A 1
H02D H 0.427690 0.132095 0.251056 0.078 Uiso 0.673(6) 1 calc R . P A 1
C022 C 0.3331(3) 0.2252(4) 0.0893(2) 0.0648(14) Uani 0.673(6) 1 d . . P A 1
H02E H 0.311281 0.293333 0.088468 0.078 Uiso 0.673(6) 1 calc R . P A 1
H02F H 0.300258 0.169255 0.082369 0.078 Uiso 0.673(6) 1 calc R . P A 1
C023 C 0.4303(2) 0.1890(4) 0.3492(2) 0.0664(14) Uani 0.673(6) 1 d . . P A 1
H02G H 0.470122 0.229044 0.354954 0.080 Uiso 0.673(6) 1 calc R . P A 1
H02H H 0.441015 0.113052 0.351436 0.080 Uiso 0.673(6) 1 calc R . P A 1
C029 C 0.3645(7) 0.9309(8) 0.5622(3) 0.221(6) Uani 1 1 d . . . . .
H02K H 0.404761 0.967288 0.565379 0.265 Uiso 0.5 1 calc R . P B -1
H02L H 0.369850 0.858945 0.550461 0.265 Uiso 0.5 1 calc R . P B -1
H02I H 0.401889 0.978141 0.578458 0.265 Uiso 0.5 1 calc R . P C -2
H02J H 0.380649 0.861222 0.556543 0.265 Uiso 0.5 1 calc R . P C -2
C02A C 0.3265(5) 0.9695(5) 0.5168(4) 0.175(4) Uani 1 1 d . . . . .
H02M H 0.314392 1.040889 0.524428 0.210 Uiso 1 1 calc R . . . .
H02N H 0.286884 0.926588 0.505391 0.210 Uiso 1 1 calc R . . . .
C7AA C 0.3791(9) 0.910(2) 0.6180(5) 0.205(11) Uani 0.5 1 d . . P D -1
H7AA H 0.375029 0.832227 0.619984 0.246 Uiso 0.5 1 calc R . P D -1
H7AB H 0.425481 0.924983 0.635749 0.246 Uiso 0.5 1 calc R . P D -1
C4AA C 0.4215(7) 0.9816(8) 0.7839(6) 0.080(3) Uani 0.5 1 d . . P D -2
H4AA H 0.456178 1.018934 0.777768 0.119 Uiso 0.5 1 calc GR . P D -2
H4AB H 0.436612 0.958024 0.820977 0.119 Uiso 0.5 1 calc GR . P D -2
H4AC H 0.384790 1.029060 0.776734 0.119 Uiso 0.5 1 calc GR . P D -2
C5AA C 0.4009(6) 0.8859(8) 0.7469(5) 0.088(3) Uani 0.5 1 d . . P D -2
H5AA H 0.378216 0.832443 0.759850 0.105 Uiso 0.5 1 calc R . P D -2
H5AB H 0.437561 0.852881 0.741003 0.105 Uiso 0.5 1 calc R . P D -2
C6AA C 0.3495(9) 0.8874(9) 0.6981(5) 0.118(6) Uani 0.5 1 d . . P D -1
H6AA H 0.339926 0.811303 0.691789 0.142 Uiso 0.5 1 calc R . P D -1
H6AB H 0.318188 0.921162 0.710720 0.142 Uiso 0.5 1 calc R . P D -1
C0AA C 0.3548(11) 0.9451(13) 0.6484(5) 0.198(11) Uani 0.5 1 d . . P D -1
H0AA H 0.310285 0.964883 0.625584 0.237 Uiso 0.5 1 calc R . P D -1
H0AB H 0.377610 1.011989 0.662265 0.237 Uiso 0.5 1 calc R . P D -1
C68 C 0.3639(18) 0.227(3) 0.0537(14) 0.112(14) Uani 0.327(6) 1 d . . P A 2
H68A H 0.329600 0.174372 0.043251 0.168 Uiso 0.327(6) 1 calc GR . P A 2
H68B H 0.390342 0.217804 0.032407 0.168 Uiso 0.327(6) 1 calc GR . P A 2
H68C H 0.345079 0.297796 0.047718 0.168 Uiso 0.327(6) 1 calc GR . P A 2
C67 C 0.3971(6) 0.2164(10) 0.1004(6) 0.072(3) Uani 0.327(6) 1 d . U P A 2
H67A H 0.428810 0.274462 0.111460 0.086 Uiso 0.327(6) 1 calc R . P A 2
H67B H 0.421193 0.149435 0.105124 0.086 Uiso 0.327(6) 1 calc R . P A 2
C66 C 0.3595(9) 0.2157(17) 0.1358(9) 0.070(4) Uani 0.327(6) 1 d . U P A 2
H66A H 0.328873 0.156092 0.125085 0.084 Uiso 0.327(6) 1 calc R . P A 2
H66B H 0.333859 0.281356 0.129366 0.084 Uiso 0.327(6) 1 calc R . P A 2
C65 C 0.3991(7) 0.2067(9) 0.1960(6) 0.073(3) Uani 0.327(6) 1 d . U P A 2
H65A H 0.428496 0.267883 0.207132 0.088 Uiso 0.327(6) 1 calc R . P A 2
H65B H 0.425905 0.142439 0.202425 0.088 Uiso 0.327(6) 1 calc R . P A 2
C64 C 0.3589(8) 0.2022(8) 0.2311(7) 0.077(3) Uani 0.327(6) 1 d . U P A 2
H64A H 0.333794 0.135985 0.223271 0.093 Uiso 0.327(6) 1 calc R . P A 2
H64B H 0.328012 0.261401 0.221221 0.093 Uiso 0.327(6) 1 calc R . P A 2
C63 C 0.3994(11) 0.208(3) 0.2934(11) 0.080(5) Uani 0.327(6) 1 d . U P A 2
H63A H 0.434076 0.154329 0.302966 0.096 Uiso 0.327(6) 1 calc R . P A 2
H63B H 0.419756 0.277880 0.302390 0.096 Uiso 0.327(6) 1 calc R . P A 2
C62 C 0.3565(7) 0.1874(8) 0.3273(6) 0.084(4) Uani 0.327(6) 1 d . U P A 2
H62A H 0.342298 0.113035 0.324143 0.101 Uiso 0.327(6) 1 calc R . P A 2
H62B H 0.318013 0.233221 0.314837 0.101 Uiso 0.327(6) 1 calc R . P A 2
C3AA C 0.0606(3) 0.8811(5) 0.2585(3) 0.1133(19) Uani 1 1 d . . . . .
H3AA H 0.028081 0.916471 0.269199 0.136 Uiso 1 1 calc R . . . .
H3AB H 0.050521 0.804957 0.254213 0.136 Uiso 1 1 calc R . . . .
C1AA C 0.1298(4) 0.8558(6) 0.3543(2) 0.148(3) Uani 1 1 d . . . . .
H1AA H 0.115580 0.781462 0.350888 0.177 Uiso 1 1 calc R . . . .
H1AB H 0.175955 0.857002 0.377538 0.177 Uiso 1 1 calc R . . . .
C2AA C 0.1227(4) 0.8970(8) 0.2976(2) 0.162(4) Uani 1 1 d . . . . .
H2AA H 0.132775 0.973150 0.299899 0.194 Uiso 1 1 calc R . . . .
H2AB H 0.154401 0.860331 0.286397 0.194 Uiso 1 1 calc R . . . .
C8AA C 0.0594(3) 0.9313(6) 0.2019(2) 0.137(3) Uani 1 1 d . . . . .
H8AA H 0.081458 0.999485 0.208774 0.205 Uiso 1 1 calc GR . . . .
H8AB H 0.014855 0.940922 0.177366 0.205 Uiso 1 1 calc GR . . . .
H8AC H 0.081313 0.883178 0.186072 0.205 Uiso 1 1 calc GR . . . .
C1BA C 0.3523(7) 0.9480(12) 0.6938(5) 0.114(4) Uani 0.5 1 d . . P D -2
H1BA H 0.310371 0.960535 0.696844 0.136 Uiso 0.5 1 calc R . P D -2
H1BB H 0.370916 1.016913 0.690319 0.136 Uiso 0.5 1 calc R . P D -2
C3BA C 0.4341(9) 0.9324(14) 0.7938(8) 0.117(5) Uani 0.5 1 d . . P D -1
H3BA H 0.416028 1.001647 0.796001 0.176 Uiso 0.5 1 calc GR . P D -1
H3BB H 0.479915 0.931651 0.816204 0.176 Uiso 0.5 1 calc GR . P D -1
H3BC H 0.411855 0.878172 0.806005 0.176 Uiso 0.5 1 calc GR . P D -1
C9AA C 0.3274(8) 0.9193(16) 0.6004(6) 0.147(6) Uani 0.5 1 d . . P D -2
H9AA H 0.316359 0.992311 0.606484 0.176 Uiso 0.5 1 calc R . P D -2
H9AB H 0.286228 0.885478 0.578408 0.176 Uiso 0.5 1 calc R . P D -2
C2BA C 0.4257(13) 0.911(2) 0.7378(9) 0.224(14) Uani 0.5 1 d . . P D -1
H2BA H 0.452159 0.849059 0.736983 0.269 Uiso 0.5 1 calc R . P D -1
H2BB H 0.441626 0.971987 0.723801 0.269 Uiso 0.5 1 calc R . P D -1
C0BA C 0.3430(13) 0.8768(10) 0.6435(6) 0.187(10) Uani 0.5 1 d . . P D -2
H0BA H 0.383903 0.839100 0.650238 0.224 Uiso 0.5 1 calc R . P D -2
H0BB H 0.310225 0.822895 0.641020 0.224 Uiso 0.5 1 calc R . P D -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
S001 C8 1.723(2) . ?
S001 C4 1.740(3) . ?
S002 C21 1.727(2) . ?
S002 C28 1.735(3) . ?
C14 C15 1.442(3) . ?
C14 C19 1.419(3) . ?
C14 C13 1.420(3) . ?
C15 C10 1.425(3) . ?
C15 C16 1.417(3) . ?
C7 C11 1.469(3) . ?
C7 C5 1.438(3) . ?
C7 C8 1.360(3) . ?
C11 C10 1.383(3) . ?
C11 C12 1.409(3) . ?
C10 C9 1.537(3) . ?
C18 C17 1.414(3) . ?
C18 C22 1.465(3) . ?
C18 C19 1.386(3) . ?
C5 C4 1.417(3) . ?
C5 C6 1.399(4) . ?
C12 H12 0.9300 . ?
C12 C13 1.378(3) . ?
C16 H16 0.9300 . ?
C16 C17 1.377(3) . ?
C17 H17 0.9300 . ?
C22 C23 1.438(3) . ?
C22 C21 1.354(3) . ?
C19 C20 1.536(3) . ?
C13 H13 0.9300 . ?
C41 C20 1.545(3) . ?
C41 C42 1.381(4) . ?
C41 C46 1.400(3) . ?
C23 C28 1.423(3) . ?
C23 C24 1.395(4) . ?
C20 C21 1.512(3) . ?
C20 C48 1.522(3) . ?
C9 C8 1.513(3) . ?
C9 C29 1.527(3) . ?
C9 C40 1.531(3) . ?
C48 C47 1.402(4) . ?
C48 C49 1.388(4) . ?
C29 C34 1.408(3) . ?
C29 C30 1.381(4) . ?
C40 C35 1.392(4) . ?
C40 C39 1.379(4) . ?
C42 H42 0.9300 . ?
C42 C44 1.389(4) . ?
C34 C35 1.469(4) . ?
C34 C33 1.382(4) . ?
C4 C3 1.404(3) . ?
C28 C27 1.409(3) . ?
C46 C47 1.466(4) . ?
C46 C45 1.391(4) . ?
C30 H30 0.9300 . ?
C30 C31 1.425(4) . ?
C47 C52 1.393(4) . ?
C3 H3 0.9300 . ?
C3 C2 1.370(4) . ?
C6 H6 0.9300 . ?
C6 C1 1.390(3) . ?
C35 C36 1.401(4) . ?
C49 H49 0.9300 . ?
C49 C50 1.404(4) . ?
C44 C43 1.401(4) . ?
C44 C53 1.509(4) . ?
C24 H24 0.9300 . ?
C24 C25 1.391(4) . ?
C39 H39 0.9300 . ?
C39 C38 1.394(4) . ?
C31 C32 1.395(5) . ?
C31 C61 1.503(4) . ?
C2 H2 0.9300 . ?
C2 C1 1.399(5) . ?
C27 H27 0.9300 . ?
C27 C26 1.365(5) . ?
C36 H36 0.9300 . ?
C36 C37 1.377(5) . ?
C51 H51 0.9300 . ?
C51 C50 1.388(5) . ?
C51 C52 1.381(5) . ?
C50 C01Q 1.499(4) . ?
C1 H1 0.9300 . ?
C38 C37 1.388(5) . ?
C38 C01Z 1.516(5) . ?
C25 H25 0.9300 . ?
C25 C26 1.393(5) . ?
C33 H33 0.9300 . ?
C33 C32 1.374(5) . ?
C43 H43 0.9300 . ?
C43 C45 1.390(5) . ?
C26 H26 0.9300 . ?
C52 H52 0.9300 . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C56 C55 1.523(4) . ?
C56 C57 1.528(4) . ?
C32 H32 0.9300 . ?
C45 H45 0.9300 . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C54 C55 1.523(4) . ?
C54 C53 1.527(4) . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C37 H37 0.9300 . ?
C58 H58A 0.9700 . ?
C58 H58B 0.9700 . ?
C58 C57 1.521(4) . ?
C58 C59 1.525(4) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C57 H57A 0.9700 . ?
C57 H57B 0.9700 . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C59 C60 1.515(4) . ?
C01Q H01A 0.9700 . ?
C01Q H01B 0.9700 . ?
C01Q C01R 1.523(4) . ?
C01R H01C 0.9700 . ?
C01R H01D 0.9700 . ?
C01R C01W 1.498(5) . ?
C61 H61A 0.9700 . ?
C61 H61B 0.9700 . ?
C61 H61C 0.9700 . ?
C61 H61D 0.9700 . ?
C61 C023 1.536(6) . ?
C61 C62 1.738(15) . ?
C60 H60A 0.9600 . ?
C60 H60B 0.9600 . ?
C60 H60C 0.9600 . ?
C01U H01E 0.9700 . ?
C01U H01F 0.9700 . ?
C01U C021 1.526(10) . ?
C01U C023 1.522(10) . ?
C01V H01G 0.9700 . ?
C01V H01H 0.9700 . ?
C01V C020 1.506(11) . ?
C01V C022 1.526(10) . ?
C01W H01I 0.9700 . ?
C01W H01J 0.9700 . ?
C01W C01Y 1.516(5) . ?
C01X H01K 0.9600 . ?
C01X H01L 0.9600 . ?
C01X H01M 0.9600 . ?
C01X C022 1.602(16) . ?
C01Y H01N 0.9700 . ?
C01Y H01O 0.9700 . ?
C01Y C1AA 1.476(6) . ?
C01Z H01P 0.9700 . ?
C01Z H01Q 0.9700 . ?
C01Z C02A 1.557(8) . ?
C020 H02A 0.9700 . ?
C020 H02B 0.9700 . ?
C020 C021 1.507(8) . ?
C021 H02C 0.9700 . ?
C021 H02D 0.9700 . ?
C022 H02E 0.9700 . ?
C022 H02F 0.9700 . ?
C023 H02G 0.9700 . ?
C023 H02H 0.9700 . ?
C029 H02K 0.9700 . ?
C029 H02L 0.9700 . ?
C029 H02I 0.9700 . ?
C029 H02J 0.9700 . ?
C029 C02A 1.276(13) . ?
C029 C7AA 1.421(14) . ?
C029 C9AA 1.533(14) . ?
C02A H02M 0.9700 . ?
C02A H02N 0.9700 . ?
C7AA H7AA 0.9700 . ?
C7AA H7AB 0.9700 . ?
C7AA C0AA 1.211(18) . ?
C4AA H4AA 0.9600 . ?
C4AA H4AB 0.9600 . ?
C4AA H4AC 0.9600 . ?
C4AA C5AA 1.503(15) . ?
C5AA H5AA 0.9700 . ?
C5AA H5AB 0.9700 . ?
C5AA C1BA 1.612(19) . ?
C6AA H6AA 0.9700 . ?
C6AA H6AB 0.9700 . ?
C6AA C0AA 1.547(14) . ?
C6AA C2BA 1.64(3) . ?
C0AA H0AA 0.9700 . ?
C0AA H0AB 0.9700 . ?
C68 H68A 0.9600 . ?
C68 H68B 0.9600 . ?
C68 H68C 0.9600 . ?
C68 C67 1.19(4) . ?
C67 H67A 0.9700 . ?
C67 H67B 0.9700 . ?
C67 C66 1.47(2) . ?
C66 H66A 0.9700 . ?
C66 H66B 0.9700 . ?
C66 C65 1.51(3) . ?
C65 H65A 0.9700 . ?
C65 H65B 0.9700 . ?
C65 C64 1.513(15) . ?
C64 H64A 0.9700 . ?
C64 H64B 0.9700 . ?
C64 C63 1.56(3) . ?
C63 H63A 0.9700 . ?
C63 H63B 0.9700 . ?
C63 C62 1.56(2) . ?
C62 H62A 0.9700 . ?
C62 H62B 0.9700 . ?
C3AA H3AA 0.9700 . ?
C3AA H3AB 0.9700 . ?
C3AA C2AA 1.386(9) . ?
C3AA C8AA 1.622(8) . ?
C1AA H1AA 0.9700 . ?
C1AA H1AB 0.9700 . ?
C1AA C2AA 1.547(8) . ?
C2AA H2AA 0.9700 . ?
C2AA H2AB 0.9700 . ?
C8AA H8AA 0.9600 . ?
C8AA H8AB 0.9600 . ?
C8AA H8AC 0.9600 . ?
C1BA H1BA 0.9700 . ?
C1BA H1BB 0.9700 . ?
C1BA C0BA 1.555(19) . ?
C3BA H3BA 0.9600 . ?
C3BA H3BB 0.9600 . ?
C3BA H3BC 0.9600 . ?
C3BA C2BA 1.46(3) . ?
C9AA H9AA 0.9700 . ?
C9AA H9AB 0.9700 . ?
C9AA C0BA 1.19(2) . ?
C2BA H2BA 0.9700 . ?
C2BA H2BB 0.9700 . ?
C0BA H0BA 0.9700 . ?
C0BA H0BB 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
C8 S001 C4 90.20(11) . . ?
C21 S002 C28 90.44(12) . . ?
C19 C14 C15 117.1(2) . . ?
C19 C14 C13 123.4(2) . . ?
C13 C14 C15 119.4(2) . . ?
C10 C15 C14 117.4(2) . . ?
C16 C15 C14 120.0(2) . . ?
C16 C15 C10 122.5(2) . . ?
C5 C7 C11 139.1(2) . . ?
C8 C7 C11 108.0(2) . . ?
C8 C7 C5 112.8(2) . . ?
C10 C11 C7 108.10(19) . . ?
C10 C11 C12 121.39(19) . . ?
C12 C11 C7 130.4(2) . . ?
C15 C10 C9 127.1(2) . . ?
C11 C10 C15 121.1(2) . . ?
C11 C10 C9 111.43(18) . . ?
C17 C18 C22 129.9(2) . . ?
C19 C18 C17 121.69(19) . . ?
C19 C18 C22 108.3(2) . . ?
C4 C5 C7 110.1(2) . . ?
C6 C5 C7 130.9(2) . . ?
C6 C5 C4 119.0(2) . . ?
C11 C12 H12 120.5 . . ?
C13 C12 C11 119.0(2) . . ?
C13 C12 H12 120.5 . . ?
C15 C16 H16 119.2 . . ?
C17 C16 C15 121.5(2) . . ?
C17 C16 H16 119.2 . . ?
C18 C17 H17 120.8 . . ?
C16 C17 C18 118.5(2) . . ?
C16 C17 H17 120.8 . . ?
C23 C22 C18 138.3(2) . . ?
C21 C22 C18 108.2(2) . . ?
C21 C22 C23 113.6(2) . . ?
C14 C19 C20 127.8(2) . . ?
C18 C19 C14 121.0(2) . . ?
C18 C19 C20 110.85(18) . . ?
C14 C13 H13 119.2 . . ?
C12 C13 C14 121.6(2) . . ?
C12 C13 H13 119.2 . . ?
C42 C41 C20 128.4(2) . . ?
C42 C41 C46 121.1(2) . . ?
C46 C41 C20 110.3(2) . . ?
C28 C23 C22 109.5(2) . . ?
C24 C23 C22 131.2(2) . . ?
C24 C23 C28 119.2(2) . . ?
C19 C20 C41 117.60(19) . . ?
C21 C20 C19 99.39(18) . . ?
C21 C20 C41 110.52(18) . . ?
C21 C20 C48 114.79(19) . . ?
C48 C20 C19 114.08(18) . . ?
C48 C20 C41 101.15(19) . . ?
C8 C9 C10 99.08(17) . . ?
C8 C9 C29 112.78(18) . . ?
C8 C9 C40 113.48(18) . . ?
C29 C9 C10 117.81(18) . . ?
C29 C9 C40 101.40(19) . . ?
C40 C9 C10 112.94(18) . . ?
C22 C21 S002 113.67(18) . . ?
C22 C21 C20 113.19(19) . . ?
C20 C21 S002 133.06(18) . . ?
C7 C8 S001 114.19(17) . . ?
C7 C8 C9 113.35(19) . . ?
C9 C8 S001 132.45(17) . . ?
C47 C48 C20 110.9(2) . . ?
C49 C48 C20 128.0(2) . . ?
C49 C48 C47 121.1(2) . . ?
C34 C29 C9 110.0(2) . . ?
C30 C29 C9 128.5(2) . . ?
C30 C29 C34 121.5(2) . . ?
C35 C40 C9 111.1(2) . . ?
C39 C40 C9 127.9(2) . . ?
C39 C40 C35 120.9(2) . . ?
C41 C42 H42 119.8 . . ?
C41 C42 C44 120.4(2) . . ?
C44 C42 H42 119.8 . . ?
C29 C34 C35 109.1(2) . . ?
C33 C34 C29 120.4(3) . . ?
C33 C34 C35 130.5(2) . . ?
C5 C4 S001 112.71(18) . . ?
C3 C4 S001 126.0(2) . . ?
C3 C4 C5 121.3(3) . . ?
C23 C28 S002 112.79(18) . . ?
C27 C28 S002 126.8(2) . . ?
C27 C28 C23 120.4(3) . . ?
C41 C46 C47 108.8(2) . . ?
C45 C46 C41 119.0(3) . . ?
C45 C46 C47 132.1(3) . . ?
C29 C30 H30 120.9 . . ?
C29 C30 C31 118.1(3) . . ?
C31 C30 H30 120.9 . . ?
C48 C47 C46 108.8(2) . . ?
C52 C47 C48 120.0(3) . . ?
C52 C47 C46 131.1(3) . . ?
C4 C3 H3 120.9 . . ?
C2 C3 C4 118.2(2) . . ?
C2 C3 H3 120.9 . . ?
C5 C6 H6 120.3 . . ?
C1 C6 C5 119.4(2) . . ?
C1 C6 H6 120.3 . . ?
C40 C35 C34 108.3(2) . . ?
C40 C35 C36 119.3(3) . . ?
C36 C35 C34 132.3(3) . . ?
C48 C49 H49 120.5 . . ?
C48 C49 C50 119.0(3) . . ?
C50 C49 H49 120.5 . . ?
C42 C44 C43 118.3(3) . . ?
C42 C44 C53 120.3(3) . . ?
C43 C44 C53 121.3(3) . . ?
C23 C24 H24 120.3 . . ?
C25 C24 C23 119.5(3) . . ?
C25 C24 H24 120.3 . . ?
C40 C39 H39 119.8 . . ?
C40 C39 C38 120.4(3) . . ?
C38 C39 H39 119.8 . . ?
C30 C31 C61 120.4(3) . . ?
C32 C31 C30 118.7(3) . . ?
C32 C31 C61 120.9(3) . . ?
C3 C2 H2 119.2 . . ?
C3 C2 C1 121.7(2) . . ?
C1 C2 H2 119.2 . . ?
C28 C27 H27 120.7 . . ?
C26 C27 C28 118.6(3) . . ?
C26 C27 H27 120.7 . . ?
C35 C36 H36 120.6 . . ?
C37 C36 C35 118.8(3) . . ?
C37 C36 H36 120.6 . . ?
C50 C51 H51 118.5 . . ?
C52 C51 H51 118.5 . . ?
C52 C51 C50 122.9(3) . . ?
C49 C50 C01Q 120.8(3) . . ?
C51 C50 C49 118.8(3) . . ?
C51 C50 C01Q 120.4(3) . . ?
C6 C1 C2 120.5(3) . . ?
C6 C1 H1 119.8 . . ?
C2 C1 H1 119.8 . . ?
C39 C38 C01Z 120.5(3) . . ?
C37 C38 C39 118.2(3) . . ?
C37 C38 C01Z 121.2(3) . . ?
C24 C25 H25 119.8 . . ?
C24 C25 C26 120.4(3) . . ?
C26 C25 H25 119.8 . . ?
C34 C33 H33 120.8 . . ?
C32 C33 C34 118.3(3) . . ?
C32 C33 H33 120.8 . . ?
C44 C43 H43 119.2 . . ?
C45 C43 C44 121.6(3) . . ?
C45 C43 H43 119.2 . . ?
C27 C26 C25 121.8(2) . . ?
C27 C26 H26 119.1 . . ?
C25 C26 H26 119.1 . . ?
C47 C52 H52 120.9 . . ?
C51 C52 C47 118.2(3) . . ?
C51 C52 H52 120.9 . . ?
H56A C56 H56B 107.7 . . ?
C55 C56 H56A 108.8 . . ?
C55 C56 H56B 108.8 . . ?
C55 C56 C57 113.6(3) . . ?
C57 C56 H56A 108.8 . . ?
C57 C56 H56B 108.8 . . ?
C31 C32 H32 118.5 . . ?
C33 C32 C31 123.0(3) . . ?
C33 C32 H32 118.5 . . ?
C46 C45 H45 120.3 . . ?
C43 C45 C46 119.5(3) . . ?
C43 C45 H45 120.3 . . ?
H54A C54 H54B 107.7 . . ?
C55 C54 H54A 108.8 . . ?
C55 C54 H54B 108.8 . . ?
C55 C54 C53 113.6(3) . . ?
C53 C54 H54A 108.8 . . ?
C53 C54 H54B 108.8 . . ?
C56 C55 H55A 109.1 . . ?
C56 C55 H55B 109.1 . . ?
C54 C55 C56 112.6(3) . . ?
C54 C55 H55A 109.1 . . ?
C54 C55 H55B 109.1 . . ?
H55A C55 H55B 107.8 . . ?
C36 C37 C38 122.5(3) . . ?
C36 C37 H37 118.8 . . ?
C38 C37 H37 118.8 . . ?
H58A C58 H58B 107.7 . . ?
C57 C58 H58A 108.8 . . ?
C57 C58 H58B 108.8 . . ?
C57 C58 C59 114.0(3) . . ?
C59 C58 H58A 108.8 . . ?
C59 C58 H58B 108.8 . . ?
C44 C53 C54 112.4(2) . . ?
C44 C53 H53A 109.1 . . ?
C44 C53 H53B 109.1 . . ?
C54 C53 H53A 109.1 . . ?
C54 C53 H53B 109.1 . . ?
H53A C53 H53B 107.9 . . ?
C56 C57 H57A 108.7 . . ?
C56 C57 H57B 108.7 . . ?
C58 C57 C56 114.1(3) . . ?
C58 C57 H57A 108.7 . . ?
C58 C57 H57B 108.7 . . ?
H57A C57 H57B 107.6 . . ?
C58 C59 H59A 108.9 . . ?
C58 C59 H59B 108.9 . . ?
H59A C59 H59B 107.7 . . ?
C60 C59 C58 113.5(3) . . ?
C60 C59 H59A 108.9 . . ?
C60 C59 H59B 108.9 . . ?
C50 C01Q H01A 109.1 . . ?
C50 C01Q H01B 109.1 . . ?
C50 C01Q C01R 112.6(3) . . ?
H01A C01Q H01B 107.8 . . ?
C01R C01Q H01A 109.1 . . ?
C01R C01Q H01B 109.1 . . ?
C01Q C01R H01C 108.8 . . ?
C01Q C01R H01D 108.8 . . ?
H01C C01R H01D 107.7 . . ?
C01W C01R C01Q 113.8(3) . . ?
C01W C01R H01C 108.8 . . ?
C01W C01R H01D 108.8 . . ?
C31 C61 H61A 109.3 . . ?
C31 C61 H61B 109.3 . . ?
C31 C61 H61C 109.1 . . ?
C31 C61 H61D 109.1 . . ?
C31 C61 C023 111.7(3) . . ?
C31 C61 C62 112.6(4) . . ?
H61A C61 H61B 107.9 . . ?
H61C C61 H61D 107.8 . . ?
C023 C61 H61A 109.3 . . ?
C023 C61 H61B 109.3 . . ?
C62 C61 H61C 109.1 . . ?
C62 C61 H61D 109.1 . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
H01E C01U H01F 107.7 . . ?
C021 C01U H01E 108.8 . . ?
C021 C01U H01F 108.8 . . ?
C023 C01U H01E 108.8 . . ?
C023 C01U H01F 108.8 . . ?
C023 C01U C021 113.7(6) . . ?
H01G C01V H01H 107.5 . . ?
C020 C01V H01G 108.5 . . ?
C020 C01V H01H 108.5 . . ?
C020 C01V C022 115.3(6) . . ?
C022 C01V H01G 108.5 . . ?
C022 C01V H01H 108.5 . . ?
C01R C01W H01I 109.1 . . ?
C01R C01W H01J 109.1 . . ?
C01R C01W C01Y 112.7(3) . . ?
H01I C01W H01J 107.8 . . ?
C01Y C01W H01I 109.1 . . ?
C01Y C01W H01J 109.1 . . ?
H01K C01X H01L 109.5 . . ?
H01K C01X H01M 109.5 . . ?
H01L C01X H01M 109.5 . . ?
C022 C01X H01K 109.5 . . ?
C022 C01X H01L 109.5 . . ?
C022 C01X H01M 109.5 . . ?
C01W C01Y H01N 108.7 . . ?
C01W C01Y H01O 108.7 . . ?
H01N C01Y H01O 107.6 . . ?
C1AA C01Y C01W 114.1(3) . . ?
C1AA C01Y H01N 108.7 . . ?
C1AA C01Y H01O 108.7 . . ?
C38 C01Z H01P 109.5 . . ?
C38 C01Z H01Q 109.5 . . ?
C38 C01Z C02A 110.8(3) . . ?
H01P C01Z H01Q 108.1 . . ?
C02A C01Z H01P 109.5 . . ?
C02A C01Z H01Q 109.5 . . ?
C01V C020 H02A 108.4 . . ?
C01V C020 H02B 108.4 . . ?
C01V C020 C021 115.7(6) . . ?
H02A C020 H02B 107.4 . . ?
C021 C020 H02A 108.4 . . ?
C021 C020 H02B 108.4 . . ?
C01U C021 H02C 108.6 . . ?
C01U C021 H02D 108.6 . . ?
C020 C021 C01U 114.8(6) . . ?
C020 C021 H02C 108.6 . . ?
C020 C021 H02D 108.6 . . ?
H02C C021 H02D 107.5 . . ?
C01V C022 C01X 117.5(6) . . ?
C01V C022 H02E 107.9 . . ?
C01V C022 H02F 107.9 . . ?
C01X C022 H02E 107.9 . . ?
C01X C022 H02F 107.9 . . ?
H02E C022 H02F 107.2 . . ?
C61 C023 H02G 109.0 . . ?
C61 C023 H02H 109.0 . . ?
C01U C023 C61 112.8(5) . . ?
C01U C023 H02G 109.0 . . ?
C01U C023 H02H 109.0 . . ?
H02G C023 H02H 107.8 . . ?
H02K C029 H02L 104.0 . . ?
H02I C029 H02J 108.2 . . ?
C02A C029 H02K 99.1 . . ?
C02A C029 H02L 99.1 . . ?
C02A C029 H02I 109.7 . . ?
C02A C029 H02J 109.7 . . ?
C02A C029 C7AA 150.3(12) . . ?
C02A C029 C9AA 109.8(12) . . ?
C7AA C029 H02K 99.1 . . ?
C7AA C029 H02L 99.1 . . ?
C9AA C029 H02I 109.7 . . ?
C9AA C029 H02J 109.7 . . ?
C01Z C02A H02M 106.4 . . ?
C01Z C02A H02N 106.4 . . ?
C029 C02A C01Z 123.9(8) . . ?
C029 C02A H02M 106.4 . . ?
C029 C02A H02N 106.4 . . ?
H02M C02A H02N 106.4 . . ?
C029 C7AA H7AA 104.7 . . ?
C029 C7AA H7AB 104.7 . . ?
H7AA C7AA H7AB 105.7 . . ?
C0AA C7AA C029 130.5(19) . . ?
C0AA C7AA H7AA 104.7 . . ?
C0AA C7AA H7AB 104.7 . . ?
H4AA C4AA H4AB 109.5 . . ?
H4AA C4AA H4AC 109.5 . . ?
H4AB C4AA H4AC 109.5 . . ?
C5AA C4AA H4AA 109.5 . . ?
C5AA C4AA H4AB 109.5 . . ?
C5AA C4AA H4AC 109.5 . . ?
C4AA C5AA H5AA 112.3 . . ?
C4AA C5AA H5AB 112.3 . . ?
C4AA C5AA C1BA 97.6(9) . . ?
H5AA C5AA H5AB 109.8 . . ?
C1BA C5AA H5AA 112.3 . . ?
C1BA C5AA H5AB 112.3 . . ?
H6AA C6AA H6AB 110.3 . . ?
C0AA C6AA H6AA 112.8 . . ?
C0AA C6AA H6AB 112.8 . . ?
C0AA C6AA C2BA 94.6(12) . . ?
C2BA C6AA H6AA 112.8 . . ?
C2BA C6AA H6AB 112.8 . . ?
C7AA C0AA C6AA 127(2) . . ?
C7AA C0AA H0AA 105.7 . . ?
C7AA C0AA H0AB 105.7 . . ?
C6AA C0AA H0AA 105.7 . . ?
C6AA C0AA H0AB 105.7 . . ?
H0AA C0AA H0AB 106.1 . . ?
H68A C68 H68B 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C67 C68 H68A 109.5 . . ?
C67 C68 H68B 109.5 . . ?
C67 C68 H68C 109.5 . . ?
C68 C67 H67A 108.9 . . ?
C68 C67 H67B 108.9 . . ?
C68 C67 C66 113(2) . . ?
H67A C67 H67B 107.7 . . ?
C66 C67 H67A 108.9 . . ?
C66 C67 H67B 108.9 . . ?
C67 C66 H66A 108.3 . . ?
C67 C66 H66B 108.3 . . ?
C67 C66 C65 116.0(14) . . ?
H66A C66 H66B 107.4 . . ?
C65 C66 H66A 108.3 . . ?
C65 C66 H66B 108.3 . . ?
C66 C65 H65A 108.6 . . ?
C66 C65 H65B 108.6 . . ?
C66 C65 C64 114.8(14) . . ?
H65A C65 H65B 107.5 . . ?
C64 C65 H65A 108.6 . . ?
C64 C65 H65B 108.6 . . ?
C65 C64 H64A 108.5 . . ?
C65 C64 H64B 108.5 . . ?
C65 C64 C63 115.0(15) . . ?
H64A C64 H64B 107.5 . . ?
C63 C64 H64A 108.5 . . ?
C63 C64 H64B 108.5 . . ?
C64 C63 H63A 109.1 . . ?
C64 C63 H63B 109.1 . . ?
H63A C63 H63B 107.9 . . ?
C62 C63 C64 112.4(17) . . ?
C62 C63 H63A 109.1 . . ?
C62 C63 H63B 109.1 . . ?
C61 C62 H62A 110.4 . . ?
C61 C62 H62B 110.4 . . ?
C63 C62 C61 106.4(14) . . ?
C63 C62 H62A 110.4 . . ?
C63 C62 H62B 110.4 . . ?
H62A C62 H62B 108.6 . . ?
H3AA C3AA H3AB 108.4 . . ?
C2AA C3AA H3AA 110.1 . . ?
C2AA C3AA H3AB 110.1 . . ?
C2AA C3AA C8AA 107.9(6) . . ?
C8AA C3AA H3AA 110.1 . . ?
C8AA C3AA H3AB 110.1 . . ?
C01Y C1AA H1AA 108.3 . . ?
C01Y C1AA H1AB 108.3 . . ?
C01Y C1AA C2AA 116.1(4) . . ?
H1AA C1AA H1AB 107.4 . . ?
C2AA C1AA H1AA 108.3 . . ?
C2AA C1AA H1AB 108.3 . . ?
C3AA C2AA C1AA 113.2(7) . . ?
C3AA C2AA H2AA 108.9 . . ?
C3AA C2AA H2AB 108.9 . . ?
C1AA C2AA H2AA 108.9 . . ?
C1AA C2AA H2AB 108.9 . . ?
H2AA C2AA H2AB 107.7 . . ?
C3AA C8AA H8AA 109.5 . . ?
C3AA C8AA H8AB 109.5 . . ?
C3AA C8AA H8AC 109.5 . . ?
H8AA C8AA H8AB 109.5 . . ?
H8AA C8AA H8AC 109.5 . . ?
H8AB C8AA H8AC 109.5 . . ?
C5AA C1BA H1BA 110.1 . . ?
C5AA C1BA H1BB 110.1 . . ?
H1BA C1BA H1BB 108.4 . . ?
C0BA C1BA C5AA 108.1(12) . . ?
C0BA C1BA H1BA 110.1 . . ?
C0BA C1BA H1BB 110.1 . . ?
H3BA C3BA H3BB 109.5 . . ?
H3BA C3BA H3BC 109.5 . . ?
H3BB C3BA H3BC 109.5 . . ?
C2BA C3BA H3BA 109.5 . . ?
C2BA C3BA H3BB 109.5 . . ?
C2BA C3BA H3BC 109.5 . . ?
C029 C9AA H9AA 104.7 . . ?
C029 C9AA H9AB 104.7 . . ?
H9AA C9AA H9AB 105.7 . . ?
C0BA C9AA C029 130(2) . . ?
C0BA C9AA H9AA 104.7 . . ?
C0BA C9AA H9AB 104.7 . . ?
C6AA C2BA H2BA 108.9 . . ?
C6AA C2BA H2BB 108.9 . . ?
C3BA C2BA C6AA 113.5(18) . . ?
C3BA C2BA H2BA 108.9 . . ?
C3BA C2BA H2BB 108.9 . . ?
H2BA C2BA H2BB 107.7 . . ?
C1BA C0BA H0BA 107.7 . . ?
C1BA C0BA H0BB 107.7 . . ?
C9AA C0BA C1BA 118.3(15) . . ?
C9AA C0BA H0BA 107.7 . . ?
C9AA C0BA H0BB 107.7 . . ?
H0BA C0BA H0BB 107.1 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.825
_oxdiff_exptl_absorpt_empirical_full_min 0.469
