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

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

data_4a
_database_code_depnum_ccdc_archive 'CCDC 1952344'
loop_
_audit_author_name
_audit_author_address
'Hans Georg Stammler'
;University of Bielefeld
Germany
;
_audit_update_record             
;
2019-09-09 deposited with the CCDC.	2021-05-06 downloaded from the CCDC.
;
#measured as jala73
_audit_creation_date             2016-07-19
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C16 H10 F6 O6 S2'
_chemical_formula_sum            'C16 H10 F6 O6 S2'
_chemical_formula_weight         476.36
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C16 H10 F6 O6 S2'
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'
O O 0.0492 0.0322 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.5762(4)
_cell_length_b                   10.0978(5)
_cell_length_c                   10.1439(3)
_cell_angle_alpha                87.983(3)
_cell_angle_beta                 78.962(3)
_cell_angle_gamma                69.485(4)
_cell_volume                     901.16(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    10422
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.3640
_cell_measurement_theta_min      4.3980
_exptl_absorpt_coefficient_mu    3.595
_exptl_absorpt_correction_T_max  0.877
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             480
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.0496
-5 -5 -3 0.0425
5 3 3 0.0799
0 0 1 0.0557
-5 1 -3 0.0664
-2 -5 0 0.0374
0 1 0 0.0476
-1 0 0 0.0496
0 -2 -5 0.0524

_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.099
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
0.9987 -0.0021 0.0009 0.0320 0.1623 0.0566
-4.9960 -4.9892 -3.0040 0.3742 -0.7875 0.5042
4.9944 2.9894 3.0037 -0.3460 0.7920 -0.1796
-0.0006 0.0001 0.9996 -0.1545 -0.0043 0.0080
-4.9912 1.0101 -3.0030 0.2896 -0.8012 -0.4696
-2.0015 -4.9953 -0.0026 0.0065 -0.3132 0.6982
0.0008 0.9999 0.0002 -0.0141 -0.0023 -0.1623
-0.9987 0.0021 -0.0009 -0.0320 -0.1623 -0.0566
0.0013 -2.0000 -4.9983 0.8008 0.0259 0.2844

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13616
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.349
_diffrn_reflns_theta_min         4.444
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9981
_diffrn_measured_fraction_theta_max 0.9899
_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  65.00   1.00    1.00    --   42.33 -37.00   0.00   94
  2  ω      2.00  78.00   1.00    1.00    --   42.33 -99.00 -30.00   76
  3  ω     56.00  98.00   1.00    1.00    --   42.33-178.00 -30.00   42
  4  ω     39.00 119.00   1.00    2.10    --  109.86-125.00  30.00   80
  5  ω     30.00 104.00   1.00    2.10    --  109.86 -94.00  60.00   74
  6  ω     31.00 106.00   1.00    2.10    --  109.86 -94.00 150.00   75
  7  ω    117.00 160.00   1.00    2.10    --  109.86  43.00  90.09   43
  8  ω    136.00 163.00   1.00    2.10    --  109.86  77.00  60.00   27
  9  ω    125.00 176.00   1.00    2.10    --  109.86  61.00  30.00   51
 10  ω    120.00 177.00   1.00    2.10    --  109.86  71.00-117.40   57
 11  ω    141.00 168.00   1.00    2.10    --  109.86  61.00-167.11   27
 12  ω    118.00 145.00   1.00    2.10    --  109.86  61.00-150.00   27
 13  ω     86.00 117.00   1.00    2.10    --  109.86  45.00 -60.00   31
 14  ω     82.00 112.00   1.00    2.10    --  109.86  61.00 -30.00   30
 15  ω     84.00 156.00   1.00    2.10    --  109.86  53.00  -8.41   72
 16  ω     87.00 112.00   1.00    2.10    --  109.86  43.00  90.09   25
 17  ω     87.00 115.00   1.00    2.10    --  109.86  45.00  60.00   28
 18  ω     82.00 108.00   1.00    2.10    --  109.86  61.00  30.00   26
 19  ω     86.00 178.00   1.00    2.10    --  109.86  61.00   0.00   92
 20  ω     86.00 118.00   1.00    2.10    --  109.86  45.00 150.00   32
 21  ω     83.00 177.00   1.00    2.10    --  109.86  61.00 150.00   94
 22  ω     78.00 105.00   1.00    2.10    --  109.86  77.00  60.00   27
 23  ω     82.00 115.00   1.00    2.10    --  109.86  61.00  90.00   33
 24  ω     83.00 109.00   1.00    2.10    --  109.86  61.00 120.00   26
 25  ω     84.00 112.00   1.00    2.10    --  109.86  59.00 164.34   28
 26  ω     78.00 166.00   1.00    2.10    --  109.86  77.00  90.00   88
 27  ω     82.00 178.00   1.00    2.10    --  109.86  61.00 -60.00   96
 28  ω     82.00 109.00   1.00    2.10    --  109.86  61.00-180.00   27
 29  ω     82.00 108.00   1.00    2.10    --  109.86  61.00-167.11   26
 30  ω     83.00 109.00   1.00    2.10    --  109.86  61.00-120.00   26
 31  ω     83.00 116.00   1.00    2.10    --  109.86  61.00-150.00   33
 32  ω     82.00 108.00   1.00    2.10    --  109.86  61.00 -90.00   26
 33  ω     78.00 171.00   1.00    2.10    --  109.86  77.00-150.00   93
 34  ω     79.00 106.00   1.00    2.10    --  109.86  77.00 -90.00   27
 35  ω     78.00 104.00   1.00    2.10    --  109.86  77.00 -60.00   26
 36  ω     80.00 107.00   1.00    2.10    --  109.86  71.00-117.40   27
 37  ω     78.00 105.00   1.00    2.10    --  109.86  77.00   0.00   27
 38  ω     82.00 109.00   1.00    2.10    --  109.86  63.00  52.41   27
 39  ω     82.00 109.00   1.00    2.10    --  109.86  61.00  60.00   27
 40  ω     57.00 120.00   1.00    1.00    --   42.33 178.00-120.00   63
 41  ω    -53.00 -24.00   1.00    1.00    --  -42.33 -37.00  60.00   29
 42  ω    -41.00 -11.00   1.00    1.00    --  -42.33 -77.00 120.00   30
 43  ω    -72.00 -11.00   1.00    1.00    --  -42.33 -77.00  60.00   61
 44  ω    -62.00 -21.00   1.00    1.00    --  -42.33 -37.00 -30.00   41
 45  ω     36.00 139.00   1.00    2.10    --  109.86 -77.00-180.00  103
 46  ω    -62.00 -11.00   1.00    1.00    --  -42.33 -77.00 -30.00   51
 47  ω    -69.00 -18.00   1.00    1.00    --  -42.33 -57.00-120.00   51
 48  ω    -85.00 -11.00   1.00    1.00    --  -42.33 -77.00-150.00   74
 49  ω   -116.00 -89.00   1.00    1.00    --  -42.33 -77.00  60.00   27
 50  ω   -113.00 -88.00   1.00    1.00    --  -42.33 -37.00  60.00   25
 51  ω   -112.00 -81.00   1.00    1.00    --  -42.33 -77.00 120.00   31
 52  ω   -110.00 -63.00   1.00    1.00    --  -42.33 -37.00 150.00   47
 53  ω   -113.00 -68.00   1.00    1.00    --  -42.33 -37.00 -30.00   45
 54  ω   -112.00 -85.00   1.00    1.00    --  -42.33 -77.00 -30.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0321146000
_diffrn_orient_matrix_UB_12      -0.0140970000
_diffrn_orient_matrix_UB_13      -0.1545595000
_diffrn_orient_matrix_UB_21      0.1625379000
_diffrn_orient_matrix_UB_22      -0.0024171000
_diffrn_orient_matrix_UB_23      -0.0041683000
_diffrn_orient_matrix_UB_31      0.0563512000
_diffrn_orient_matrix_UB_32      -0.1623640000
_diffrn_orient_matrix_UB_33      0.0080875000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3333
_reflns_number_total             3536
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3536
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0312
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0449P)²+0.5195P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0860
_refine_special_details          
;
 ?
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
S1 S 0.10913(4) 0.38486(4) 0.19862(4) 0.02185(11) Uani 1 1 d . . . . .
S2 S 0.69403(5) 0.00427(4) 0.28831(4) 0.02694(12) Uani 1 1 d . . . . .
F1 F 0.15761(17) 0.17481(16) 0.03471(14) 0.0600(4) Uani 1 1 d . . . . .
F2 F 0.04902(16) 0.15649(14) 0.23670(16) 0.0603(4) Uani 1 1 d . . . . .
F3 F 0.28777(15) 0.12135(13) 0.19151(16) 0.0546(3) Uani 1 1 d . . . . .
F4 F 0.88166(13) -0.24634(11) 0.31323(13) 0.0449(3) Uani 1 1 d . . . . .
F5 F 0.72620(17) -0.15395(15) 0.49544(14) 0.0613(4) Uani 1 1 d . . . . .
F6 F 0.91413(14) -0.08399(13) 0.42193(16) 0.0562(4) Uani 1 1 d . . . . .
O1 O 0.25294(12) 0.39655(13) 0.10074(11) 0.0248(2) Uani 1 1 d . . . . .
O2 O -0.02557(13) 0.45927(15) 0.15062(13) 0.0344(3) Uani 1 1 d . . . . .
O3 O 0.11874(14) 0.40137(13) 0.33433(11) 0.0291(3) Uani 1 1 d . . . . .
O4 O 0.60598(13) 0.12592(12) 0.39757(12) 0.0254(2) Uani 1 1 d . . . . .
O5 O 0.79432(17) 0.04379(14) 0.18720(13) 0.0398(3) Uani 1 1 d . . . . .
O6 O 0.58755(16) -0.05228(14) 0.25903(17) 0.0443(4) Uani 1 1 d . . . . .
C1 C 0.29233(18) 0.51820(18) 0.12057(15) 0.0241(3) Uani 1 1 d . . . . .
C2 C 0.41694(17) 0.49706(17) 0.18135(15) 0.0213(3) Uani 1 1 d . . . . .
C3 C 0.49792(19) 0.35672(18) 0.23191(19) 0.0292(4) Uani 1 1 d . . . . .
H3A H 0.5577 0.2938 0.1556 0.035 Uiso 1 1 calc R . . . .
H3B H 0.4232 0.3178 0.2780 0.035 Uiso 1 1 calc R . . . .
C4 C 0.60003(16) 0.35858(16) 0.32491(15) 0.0209(3) Uani 1 1 d . . . . .
C5 C 0.65499(17) 0.24397(17) 0.40491(16) 0.0221(3) Uani 1 1 d . . . . .
C6 C 0.74385(18) 0.24079(18) 0.49689(16) 0.0254(3) Uani 1 1 d . . . . .
H6 H 0.7761 0.1623 0.5491 0.030 Uiso 1 1 calc R . . . .
C7 C 0.78427(18) 0.35885(18) 0.50973(16) 0.0258(3) Uani 1 1 d . . . . .
H7 H 0.8450 0.3598 0.5709 0.031 Uiso 1 1 calc R . . . .
C8 C 0.73438(17) 0.47427(17) 0.43191(15) 0.0233(3) Uani 1 1 d . . . . .
H8 H 0.7620 0.5525 0.4413 0.028 Uiso 1 1 calc R . . . .
C9 C 0.64273(16) 0.47599(17) 0.33889(15) 0.0210(3) Uani 1 1 d . . . . .
C10 C 0.59404(19) 0.60069(18) 0.25384(18) 0.0289(4) Uani 1 1 d . . . . .
H10A H 0.5708 0.6856 0.3082 0.035 Uiso 1 1 calc R . . . .
H10B H 0.6788 0.5959 0.1820 0.035 Uiso 1 1 calc R . . . .
C11 C 0.46033(17) 0.61450(17) 0.19306(15) 0.0224(3) Uani 1 1 d . . . . .
C12 C 0.3769(2) 0.74533(19) 0.14773(18) 0.0306(4) Uani 1 1 d . . . . .
H12 H 0.4059 0.8230 0.1559 0.037 Uiso 1 1 calc R . . . .
C13 C 0.2522(2) 0.7611(2) 0.0910(2) 0.0438(5) Uani 1 1 d . . . . .
H13 H 0.1968 0.8493 0.0630 0.053 Uiso 1 1 calc R . . . .
C14 C 0.2090(2) 0.6455(2) 0.0757(2) 0.0386(4) Uani 1 1 d . . . . .
H14 H 0.1262 0.6543 0.0363 0.046 Uiso 1 1 calc R . . . .
C15 C 0.1549(2) 0.1966(2) 0.1621(2) 0.0360(4) Uani 1 1 d . . . . .
C16 C 0.8114(2) -0.1282(2) 0.3873(2) 0.0347(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O1 1.5742(11) . ?
S1 O2 1.4146(12) . ?
S1 O3 1.4167(12) . ?
S1 C15 1.8295(19) . ?
S2 O4 1.5685(12) . ?
S2 O5 1.4128(14) . ?
S2 O6 1.4106(13) . ?
S2 C16 1.8290(19) . ?
F1 C15 1.313(2) . ?
F2 C15 1.318(2) . ?
F3 C15 1.318(2) . ?
F4 C16 1.322(2) . ?
F5 C16 1.312(2) . ?
F6 C16 1.320(2) . ?
O1 C1 1.4364(19) . ?
O4 C5 1.4347(18) . ?
C1 C2 1.394(2) . ?
C1 C14 1.369(3) . ?
C2 C3 1.484(2) . ?
C2 C11 1.403(2) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.488(2) . ?
C4 C5 1.395(2) . ?
C4 C9 1.402(2) . ?
C5 C6 1.371(2) . ?
C6 H6 0.9300 . ?
C6 C7 1.393(2) . ?
C7 H7 0.9300 . ?
C7 C8 1.378(2) . ?
C8 H8 0.9300 . ?
C8 C9 1.402(2) . ?
C9 C10 1.488(2) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.487(2) . ?
C11 C12 1.398(2) . ?
C12 H12 0.9300 . ?
C12 C13 1.381(3) . ?
C13 H13 0.9300 . ?
C13 C14 1.391(3) . ?
C14 H14 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
O1 S1 C15 95.35(8) . . ?
O2 S1 O1 111.23(7) . . ?
O2 S1 O3 120.92(8) . . ?
O2 S1 C15 107.21(9) . . ?
O3 S1 O1 110.77(6) . . ?
O3 S1 C15 108.15(9) . . ?
O4 S2 C16 100.67(8) . . ?
O5 S2 O4 111.72(7) . . ?
O5 S2 C16 106.90(9) . . ?
O6 S2 O4 106.94(8) . . ?
O6 S2 O5 122.65(9) . . ?
O6 S2 C16 105.59(9) . . ?
C1 O1 S1 116.60(10) . . ?
C5 O4 S2 120.39(10) . . ?
C2 C1 O1 117.13(14) . . ?
C14 C1 O1 118.49(14) . . ?
C14 C1 C2 124.35(16) . . ?
C1 C2 C3 121.06(14) . . ?
C1 C2 C11 116.81(15) . . ?
C11 C2 C3 122.13(14) . . ?
C2 C3 H3A 108.6 . . ?
C2 C3 H3B 108.6 . . ?
C2 C3 C4 114.74(14) . . ?
H3A C3 H3B 107.6 . . ?
C4 C3 H3A 108.6 . . ?
C4 C3 H3B 108.6 . . ?
C5 C4 C3 121.17(14) . . ?
C5 C4 C9 116.84(14) . . ?
C9 C4 C3 121.97(14) . . ?
C4 C5 O4 117.74(13) . . ?
C6 C5 O4 117.76(14) . . ?
C6 C5 C4 124.34(15) . . ?
C5 C6 H6 121.1 . . ?
C5 C6 C7 117.88(15) . . ?
C7 C6 H6 121.1 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 C6 120.06(15) . . ?
C8 C7 H7 120.0 . . ?
C7 C8 H8 119.4 . . ?
C7 C8 C9 121.26(15) . . ?
C9 C8 H8 119.4 . . ?
C4 C9 C10 120.42(14) . . ?
C8 C9 C4 119.60(15) . . ?
C8 C9 C10 119.96(14) . . ?
C9 C10 H10A 108.4 . . ?
C9 C10 H10B 108.4 . . ?
H10A C10 H10B 107.5 . . ?
C11 C10 C9 115.49(14) . . ?
C11 C10 H10A 108.4 . . ?
C11 C10 H10B 108.4 . . ?
C2 C11 C10 120.40(14) . . ?
C12 C11 C2 119.73(15) . . ?
C12 C11 C10 119.87(15) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 C11 121.04(16) . . ?
C13 C12 H12 119.5 . . ?
C12 C13 H13 119.9 . . ?
C12 C13 C14 120.25(18) . . ?
C14 C13 H13 119.9 . . ?
C1 C14 C13 117.79(16) . . ?
C1 C14 H14 121.1 . . ?
C13 C14 H14 121.1 . . ?
F1 C15 S1 110.37(15) . . ?
F1 C15 F2 109.34(16) . . ?
F1 C15 F3 109.30(17) . . ?
F2 C15 S1 108.08(13) . . ?
F3 C15 S1 110.71(12) . . ?
F3 C15 F2 109.01(18) . . ?
F4 C16 S2 108.64(13) . . ?
F5 C16 S2 110.25(13) . . ?
F5 C16 F4 108.96(16) . . ?
F5 C16 F6 109.75(18) . . ?
F6 C16 S2 110.37(13) . . ?
F6 C16 F4 108.84(15) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 O1 C1 C2 104.93(14) . . . . ?
S1 O1 C1 C14 -76.91(18) . . . . ?
S2 O4 C5 C4 86.98(15) . . . . ?
S2 O4 C5 C6 -97.55(15) . . . . ?
O1 S1 C15 F1 -61.80(14) . . . . ?
O1 S1 C15 F2 178.67(14) . . . . ?
O1 S1 C15 F3 59.34(15) . . . . ?
O1 C1 C2 C3 -4.3(2) . . . . ?
O1 C1 C2 C11 176.28(13) . . . . ?
O1 C1 C14 C13 -177.59(17) . . . . ?
O2 S1 O1 C1 86.23(12) . . . . ?
O2 S1 C15 F1 52.39(15) . . . . ?
O2 S1 C15 F2 -67.14(16) . . . . ?
O2 S1 C15 F3 173.53(14) . . . . ?
O3 S1 O1 C1 -51.25(13) . . . . ?
O3 S1 C15 F1 -175.72(12) . . . . ?
O3 S1 C15 F2 64.75(16) . . . . ?
O3 S1 C15 F3 -54.58(16) . . . . ?
O4 S2 C16 F4 172.85(12) . . . . ?
O4 S2 C16 F5 53.51(15) . . . . ?
O4 S2 C16 F6 -67.90(15) . . . . ?
O4 C5 C6 C7 -176.34(13) . . . . ?
O5 S2 O4 C5 -14.06(14) . . . . ?
O5 S2 C16 F4 -70.36(14) . . . . ?
O5 S2 C16 F5 170.31(13) . . . . ?
O5 S2 C16 F6 48.90(16) . . . . ?
O6 S2 O4 C5 -150.81(12) . . . . ?
O6 S2 C16 F4 61.73(15) . . . . ?
O6 S2 C16 F5 -57.61(16) . . . . ?
O6 S2 C16 F6 -179.02(14) . . . . ?
C1 C2 C3 C4 -164.56(15) . . . . ?
C1 C2 C11 C10 -178.65(14) . . . . ?
C1 C2 C11 C12 1.6(2) . . . . ?
C2 C1 C14 C13 0.4(3) . . . . ?
C2 C3 C4 C5 164.55(14) . . . . ?
C2 C3 C4 C9 -13.9(2) . . . . ?
C2 C11 C12 C13 -0.2(3) . . . . ?
C3 C2 C11 C10 1.9(2) . . . . ?
C3 C2 C11 C12 -177.87(16) . . . . ?
C3 C4 C5 O4 -1.9(2) . . . . ?
C3 C4 C5 C6 -177.03(15) . . . . ?
C3 C4 C9 C8 177.48(15) . . . . ?
C3 C4 C9 C10 -3.8(2) . . . . ?
C4 C5 C6 C7 -1.2(2) . . . . ?
C4 C9 C10 C11 20.5(2) . . . . ?
C5 C4 C9 C8 -1.1(2) . . . . ?
C5 C4 C9 C10 177.70(14) . . . . ?
C5 C6 C7 C8 0.4(2) . . . . ?
C6 C7 C8 C9 0.0(2) . . . . ?
C7 C8 C9 C4 0.4(2) . . . . ?
C7 C8 C9 C10 -178.41(15) . . . . ?
C8 C9 C10 C11 -160.76(14) . . . . ?
C9 C4 C5 O4 176.67(13) . . . . ?
C9 C4 C5 C6 1.5(2) . . . . ?
C9 C10 C11 C2 -19.6(2) . . . . ?
C9 C10 C11 C12 160.20(15) . . . . ?
C10 C11 C12 C13 -179.93(18) . . . . ?
C11 C2 C3 C4 14.9(2) . . . . ?
C11 C12 C13 C14 -1.2(3) . . . . ?
C12 C13 C14 C1 1.1(3) . . . . ?
C14 C1 C2 C3 177.70(18) . . . . ?
C14 C1 C2 C11 -1.8(2) . . . . ?
C15 S1 O1 C1 -162.96(12) . . . . ?
C16 S2 O4 C5 99.11(12) . . . . ?

_olex2_date_sample_data_collection 2016-07-19
_olex2_date_sample_submission    1468792800
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.176
_oxdiff_exptl_absorpt_empirical_full_min 0.913
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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.
;
_shelxl_version_number           2013-2
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1952345'
loop_
_audit_author_name
_audit_author_address
'Hans Georg Stammler'
;University of Bielefeld
Germany
;
_audit_update_record             
;
2019-09-09 deposited with the CCDC.	2021-05-06 downloaded from the CCDC.
;
# measured as jala74
_audit_creation_date             2016-07-29
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C16 H8 F6 O6 S2'
_chemical_formula_sum            'C16 H8 F6 O6 S2'
_chemical_formula_weight         474.34
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C16 H8 F6 O6 S2'
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'
O O 0.0492 0.0322 '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'

_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                   5.4457(5)
_cell_length_b                   9.7022(10)
_cell_length_c                   17.3622(8)
_cell_angle_alpha                84.758(6)
_cell_angle_beta                 87.356(7)
_cell_angle_gamma                74.878(9)
_cell_volume                     881.63(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3814
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.9880
_cell_measurement_theta_min      4.7090
_exptl_absorpt_coefficient_mu    3.674
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.757
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.787
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             476
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.0115
0 -1 0 0.0115
0 0 1 0.0295
0 0 -1 0.0295
-2 -2 -5 0.0954
2 2 5 0.1012

_exptl_crystal_size_max          0.298
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.023
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
0.0157 1.0031 -0.0048 -0.1633 -0.0151 -0.0127
-0.0157 -1.0031 0.0048 0.1633 0.0151 0.0127
0.0000 0.0043 1.0026 0.0156 -0.0200 -0.0856
-0.0000 -0.0043 -1.0026 -0.0156 0.0200 0.0856
-2.0275 -1.9186 -4.9431 0.0593 0.6601 0.2759
2.0275 1.9186 4.9431 -0.0593 -0.6601 -0.2759

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_av_unetI/netI     0.0584
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11552
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.331
_diffrn_reflns_theta_min         2.556
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9821
_diffrn_measured_fraction_theta_max 0.9769
_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  25.00   1.00   10.64    --  -38.50  37.00 -90.00   67
  2  ω    -27.00  33.00   1.00   10.64    --  -38.50  77.00 -30.00   60
  3  ω    -67.00 -29.00   1.00   10.64    --  -38.50  77.00 -30.00   38
  4  ω     18.00  50.00   1.00   10.64    --   41.95  57.00 -90.00   32
  5  ω     59.00  98.00   1.00   10.64    --   41.95  22.00  31.00   39
  6  ω     79.00 123.00   1.00   10.64    --   41.95-178.00  90.00   44
  7  ω     66.00  99.00   1.00   10.64    --   41.95  77.00   0.00   33
  8  ω     58.00 125.00   1.00   10.64    --   41.95 178.00 -90.00   67
  9  ω     68.00 105.00   1.00   10.64    --   41.95  57.00 -90.00   37
 10  ω     23.00  64.00   1.00   10.64    --   41.95  37.00 120.00   41
 11  ω      6.00  32.00   1.00   10.64    --   41.95  90.00  54.27   26
 12  ω     18.00 111.00   1.00   10.64    --   41.95  77.00-180.00   93
 13  ω     12.00  87.00   1.00   10.64    --   41.95  77.00 120.00   75
 14  ω    -23.00  61.00   1.00   10.64    --   41.95 -37.00  30.00   84
 15  ω     12.00  64.00   1.00   10.64    --   41.95  77.00 -60.00   52
 16  ω     16.00  59.00   1.00   10.64    --   41.95  77.00   0.00   43
 17  ω     13.00  57.00   1.00   10.64    --   41.95  22.00  31.00   44
 18  ω     85.00 111.00   1.00   33.00    --  111.00  61.00  30.00   26
 19  ω     42.00  85.00   1.00   33.00    --  111.00-125.00-150.00   43
 20  ω     85.00 114.00   1.00   33.00    --  111.00  59.00 -88.76   29
 21  ω     81.00 156.00   1.00   33.00    --  111.00  77.00  60.00   75
 22  ω    111.00 176.00   1.00   33.00    --  111.00  77.00  90.00   65
 23  ω     81.00 108.00   1.00   33.00    --  111.00  77.00 120.00   27
 24  ω     81.00 107.00   1.00   33.00    --  111.00  77.00  90.00   26
 25  ω     89.00 150.00   1.00   33.00    --  111.00  45.00   0.00   61
 26  ω     81.00 107.00   1.00   33.00    --  111.00  77.00 -60.00   26
 27  ω     81.00 178.00   1.00   33.00    --  111.00  77.00 -90.00   97
 28  ω     36.00  76.00   1.00   33.00    --  111.00 -94.00 -60.00   40
 29  ω     81.00 109.00   1.00   33.00    --  111.00 -94.00 -60.00   28
 30  ω     82.00 109.00   1.00   33.00    --  111.00  77.00 -30.00   27
 31  ω     82.00 109.00   1.00   33.00    --  111.00  73.00-112.18   27
 32  ω    153.00 178.00   1.00   33.00    --  111.00  52.00 177.87   25
 33  ω     81.00 162.00   1.00   33.00    --  111.00  77.00-150.00   81
 34  ω    116.00 164.00   1.00   33.00    --  111.00  61.00 -30.00   48
 35  ω     85.00 114.00   1.00   33.00    --  111.00  61.00   0.00   29
 36  ω    147.00 178.00   1.00   33.00    --  111.00  61.00 120.00   31
 37  ω     87.00 114.00   1.00   33.00    --  111.00  61.00 120.00   27
 38  ω     85.00 111.00   1.00   33.00    --  111.00  61.00  90.00   26
 39  ω     83.00 130.00   1.00   33.00    --  111.00  67.00  56.17   47
 40  ω     77.00 107.00   1.00   33.00    --  111.00 -94.00   0.00   30
 41  ω     41.00  66.00   1.00   33.00    --  111.00 -94.00   0.00   25
 42  ω     85.00 112.00   1.00   33.00    --  111.00  61.00 -30.00   27
 43  ω     83.00 112.00   1.00   33.00    --  111.00  77.00  30.00   29
 44  ω     33.00 106.00   1.00   33.00    --  111.00 -94.00-150.00   73
 45  ω     86.00 111.00   1.00   33.00    --  111.00  61.00-180.00   25
 46  ω     85.00 177.00   1.00   33.00    --  111.00  61.00 150.00   92
 47  ω     81.00 174.00   1.00   33.00    --  111.00  77.00   0.00   93
 48  ω     33.00  58.00   1.00   33.00    --  111.00 -94.00  60.00   25
 49  ω     82.00 109.00   1.00   33.00    --  111.00 -94.00  60.00   27
 50  ω     90.00 121.00   1.00   33.00    --  111.00  45.00 -90.00   31
 51  ω     31.00 109.00   1.00   33.00    --  111.00 -94.00 -90.00   78
 52  ω     89.00 115.00   1.00   33.00    --  111.00  45.00 120.00   26
 53  ω     85.00 123.00   1.00   33.00    --  111.00  61.00-150.00   38
 54  ω     46.00 108.00   1.00   33.00    --  111.00 -94.00 120.00   62
 55  ω     89.00 116.00   1.00   33.00    --  111.00  45.00-150.00   27
 56  ω     86.00 156.00   1.00   33.00    --  111.00  61.00 -60.00   70
 57  ω     85.00 173.00   1.00   33.00    --  111.00  61.00-120.00   88
 58  ω    131.00 154.00   1.00   33.00    --  111.00  61.00  30.00   23
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0864421000
_diffrn_orient_matrix_UB_12      -0.1640386000
_diffrn_orient_matrix_UB_13      0.0162232000
_diffrn_orient_matrix_UB_21      -0.2666604000
_diffrn_orient_matrix_UB_22      -0.0110048000
_diffrn_orient_matrix_UB_23      -0.0198931000
_diffrn_orient_matrix_UB_31      0.0856810000
_diffrn_orient_matrix_UB_32      -0.0144380000
_diffrn_orient_matrix_UB_33      -0.0853508000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2672
_reflns_number_total             3434
_reflns_odcompleteness_completeness 98.36
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         3434
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0614
_refine_ls_restrained_S_all      1.016
_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)+(0.1110P)²+0.2466P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1619
_refine_ls_wR_factor_ref         0.1782
_refine_special_details          
;
 Disorder of S(2), O(5), O(6), C(16), F(4), F(5), F(6) over two sites (59:41)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
S1 S 0.49705(15) 0.25195(8) 0.12891(5) 0.0299(2) Uani 1 1 d . . . . .
S2A S -0.0978(3) 0.26263(14) 0.41359(8) 0.0324(5) Uani 0.587(3) 1 d . . P A 1
S2B S 0.0307(3) 0.32396(19) 0.43512(10) 0.0259(6) Uani 0.413(3) 1 d . . P A 2
F1 F 0.8191(4) 0.2692(2) 0.01445(12) 0.0413(5) Uani 1 1 d . . . . .
F2 F 0.6956(4) 0.0744(2) 0.02715(13) 0.0421(5) Uani 1 1 d . . . . .
F3 F 0.9671(4) 0.1074(3) 0.10576(14) 0.0486(6) Uani 1 1 d . . . . .
F4A F 0.3364(9) 0.3213(5) 0.4212(3) 0.0440(11) Uani 0.587(3) 1 d . . P A 1
F5A F 0.3313(14) 0.1640(8) 0.3414(4) 0.064(2) Uani 0.587(3) 1 d . . P A 1
F6A F 0.3324(12) 0.1069(6) 0.4651(3) 0.0555(14) Uani 0.587(3) 1 d . . P A 1
F4B F 0.226(2) 0.1229(10) 0.3431(6) 0.059(2) Uani 0.413(3) 1 d . . P A 2
F5B F -0.1004(12) 0.1029(9) 0.4002(6) 0.065(3) Uani 0.413(3) 1 d . . P A 2
F6B F 0.2408(18) 0.0557(8) 0.4644(5) 0.054(2) Uani 0.413(3) 1 d . . P A 2
O1 O 0.6279(4) 0.3424(2) 0.17575(13) 0.0286(5) Uani 1 1 d . . . . .
O2 O 0.3044(4) 0.3397(3) 0.08077(15) 0.0375(6) Uani 1 1 d . . . . .
O3 O 0.4565(6) 0.1370(3) 0.17975(16) 0.0454(7) Uani 1 1 d . . . . .
O4 O -0.1415(5) 0.3809(3) 0.34805(17) 0.0467(7) Uani 1 1 d . . . . .
O5A O -0.1703(17) 0.3238(9) 0.4861(5) 0.0388(9) Uani 0.587(3) 1 d . . P A 1
O6A O -0.1862(12) 0.1402(6) 0.3983(3) 0.0388(9) Uani 0.587(3) 1 d . . P A 1
O5B O -0.130(3) 0.3400(14) 0.4978(7) 0.0388(9) Uani 0.413(3) 1 d . . P A 2
O6B O 0.2625(17) 0.3644(9) 0.4357(5) 0.0388(9) Uani 0.413(3) 1 d . . P A 2
C1 C 0.5638(6) 0.4959(3) 0.16324(18) 0.0273(6) Uani 1 1 d . . . . .
C2 C 0.3536(6) 0.5727(3) 0.20715(17) 0.0260(6) Uani 1 1 d . . . . .
C3 C 0.1949(6) 0.5075(3) 0.25529(18) 0.0267(6) Uani 1 1 d . . . . .
H3 H 0.2238 0.4084 0.2593 0.032 Uiso 1 1 calc R U . . .
C4 C -0.0066(6) 0.5907(3) 0.29732(17) 0.0269(6) Uani 1 1 d . . . . .
C5 C -0.1775(6) 0.5327(4) 0.34614(18) 0.0296(7) Uani 1 1 d . . . . .
C6 C -0.3769(6) 0.6121(4) 0.38517(19) 0.0342(8) Uani 1 1 d . . . . .
H6 H -0.4848 0.5684 0.4156 0.041 Uiso 1 1 calc R U . . .
C7 C -0.4188(6) 0.7628(4) 0.3789(2) 0.0373(8) Uani 1 1 d . . . . .
H7 H -0.5541 0.8187 0.4060 0.045 Uiso 1 1 calc R U . . .
C8 C -0.2623(7) 0.8266(4) 0.3335(2) 0.0388(8) Uani 1 1 d . . . . .
H8 H -0.2918 0.9257 0.3302 0.047 Uiso 1 1 calc R U . . .
C9 C -0.0538(6) 0.7438(4) 0.2908(2) 0.0296(7) Uani 1 1 d . . . . .
C10 C 0.1059(6) 0.8068(3) 0.2424(2) 0.0311(7) Uani 1 1 d . . . . .
H10 H 0.0764 0.9060 0.2382 0.037 Uiso 1 1 calc R U . . .
C11 C 0.3085(6) 0.7258(3) 0.20003(19) 0.0280(6) Uani 1 1 d . . . . .
C12 C 0.4732(7) 0.7903(4) 0.1512(2) 0.0332(7) Uani 1 1 d . . . . .
H12 H 0.4455 0.8894 0.1470 0.040 Uiso 1 1 calc R U . . .
C13 C 0.6693(6) 0.7095(4) 0.1109(2) 0.0337(7) Uani 1 1 d . . . . .
H13 H 0.7722 0.7539 0.0786 0.040 Uiso 1 1 calc R U . . .
C14 C 0.7189(6) 0.5574(4) 0.11745(19) 0.0315(7) Uani 1 1 d . . . . .
H14 H 0.8555 0.5017 0.0907 0.038 Uiso 1 1 calc R U . . .
C15 C 0.7636(6) 0.1700(4) 0.0650(2) 0.0329(7) Uani 1 1 d . . . . .
C16A C 0.2499(13) 0.2116(7) 0.4098(4) 0.0387(11) Uani 0.587(3) 1 d . . P A 1
C16B C 0.0979(18) 0.1404(9) 0.4078(5) 0.0387(11) Uani 0.413(3) 1 d . . 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
S1 O1 1.565(2) . ?
S1 O2 1.417(3) . ?
S1 O3 1.415(3) . ?
S1 C15 1.839(3) . ?
S2A O4 1.520(3) . ?
S2A O5A 1.436(9) . ?
S2A O6A 1.443(7) . ?
S2A C16A 1.828(7) . ?
S2B O4 1.783(3) . ?
S2B O5B 1.358(14) . ?
S2B O6B 1.417(10) . ?
S2B C16B 1.824(9) . ?
F1 C15 1.327(4) . ?
F2 C15 1.320(4) . ?
F3 C15 1.320(4) . ?
F4A C16A 1.305(9) . ?
F5A C16A 1.329(9) . ?
F6A C16A 1.334(8) . ?
F4B C16B 1.296(14) . ?
F5B C16B 1.242(13) . ?
F6B C16B 1.355(11) . ?
O1 C1 1.436(4) . ?
O4 C5 1.432(4) . ?
C1 C2 1.423(4) . ?
C1 C14 1.347(5) . ?
C2 C3 1.403(5) . ?
C2 C11 1.435(4) . ?
C3 H3 0.9300 . ?
C3 C4 1.400(4) . ?
C4 C5 1.419(5) . ?
C4 C9 1.435(5) . ?
C5 C6 1.350(5) . ?
C6 H6 0.9300 . ?
C6 C7 1.414(5) . ?
C7 H7 0.9300 . ?
C7 C8 1.362(6) . ?
C8 H8 0.9300 . ?
C8 C9 1.428(5) . ?
C9 C10 1.397(5) . ?
C10 H10 0.9300 . ?
C10 C11 1.398(5) . ?
C11 C12 1.428(5) . ?
C12 H12 0.9300 . ?
C12 C13 1.356(5) . ?
C13 H13 0.9300 . ?
C13 C14 1.424(5) . ?
C14 H14 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
O1 S1 C15 100.25(14) . . ?
O2 S1 O1 112.03(14) . . ?
O2 S1 C15 106.94(16) . . ?
O3 S1 O1 107.54(15) . . ?
O3 S1 O2 122.59(18) . . ?
O3 S1 C15 104.94(17) . . ?
O4 S2A C16A 98.3(2) . . ?
O5A S2A O4 109.7(4) . . ?
O5A S2A O6A 118.1(4) . . ?
O5A S2A C16A 106.1(4) . . ?
O6A S2A O4 114.0(3) . . ?
O6A S2A C16A 108.4(3) . . ?
O4 S2B C16B 88.3(3) . . ?
O5B S2B O4 110.7(5) . . ?
O5B S2B O6B 120.2(5) . . ?
O5B S2B C16B 109.8(6) . . ?
O6B S2B O4 114.3(4) . . ?
O6B S2B C16B 108.9(5) . . ?
C1 O1 S1 120.82(19) . . ?
C5 O4 S2A 132.8(3) . . ?
C5 O4 S2B 100.6(2) . . ?
C2 C1 O1 116.7(3) . . ?
C14 C1 O1 118.6(3) . . ?
C14 C1 C2 124.4(3) . . ?
C1 C2 C11 116.0(3) . . ?
C3 C2 C1 123.9(3) . . ?
C3 C2 C11 120.1(3) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 C2 120.5(3) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 C5 123.7(3) . . ?
C3 C4 C9 120.1(3) . . ?
C5 C4 C9 116.2(3) . . ?
C4 C5 O4 116.1(3) . . ?
C6 C5 O4 119.5(3) . . ?
C6 C5 C4 124.2(3) . . ?
C5 C6 H6 120.6 . . ?
C5 C6 C7 118.9(3) . . ?
C7 C6 H6 120.6 . . ?
C6 C7 H7 119.8 . . ?
C8 C7 C6 120.5(3) . . ?
C8 C7 H7 119.8 . . ?
C7 C8 H8 119.4 . . ?
C7 C8 C9 121.1(3) . . ?
C9 C8 H8 119.4 . . ?
C8 C9 C4 119.1(3) . . ?
C10 C9 C4 118.6(3) . . ?
C10 C9 C8 122.2(3) . . ?
C9 C10 H10 118.9 . . ?
C9 C10 C11 122.2(3) . . ?
C11 C10 H10 118.9 . . ?
C10 C11 C2 118.5(3) . . ?
C10 C11 C12 122.2(3) . . ?
C12 C11 C2 119.3(3) . . ?
C11 C12 H12 119.4 . . ?
C13 C12 C11 121.2(3) . . ?
C13 C12 H12 119.4 . . ?
C12 C13 H13 119.7 . . ?
C12 C13 C14 120.5(3) . . ?
C14 C13 H13 119.7 . . ?
C1 C14 C13 118.6(3) . . ?
C1 C14 H14 120.7 . . ?
C13 C14 H14 120.7 . . ?
F1 C15 S1 110.2(2) . . ?
F2 C15 S1 108.5(2) . . ?
F2 C15 F1 109.1(3) . . ?
F2 C15 F3 109.8(3) . . ?
F3 C15 S1 110.4(2) . . ?
F3 C15 F1 108.8(3) . . ?
F4A C16A S2A 110.1(4) . . ?
F4A C16A F5A 110.2(7) . . ?
F4A C16A F6A 109.5(6) . . ?
F5A C16A S2A 109.5(5) . . ?
F5A C16A F6A 109.0(6) . . ?
F6A C16A S2A 108.6(5) . . ?
F4B C16B S2B 112.6(7) . . ?
F4B C16B F6B 108.1(9) . . ?
F5B C16B S2B 111.8(7) . . ?
F5B C16B F4B 107.0(10) . . ?
F5B C16B F6B 110.5(9) . . ?
F6B C16B S2B 106.9(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 O1 C1 C2 87.3(3) . . . . ?
S1 O1 C1 C14 -99.1(3) . . . . ?
S2A O4 C5 C4 124.3(3) . . . . ?
S2A O4 C5 C6 -60.4(4) . . . . ?
S2B O4 C5 C4 99.3(3) . . . . ?
S2B O4 C5 C6 -85.3(3) . . . . ?
O1 S1 C15 F1 -68.4(2) . . . . ?
O1 S1 C15 F2 172.2(2) . . . . ?
O1 S1 C15 F3 51.8(3) . . . . ?
O1 C1 C2 C3 -6.2(4) . . . . ?
O1 C1 C2 C11 173.7(2) . . . . ?
O1 C1 C14 C13 -174.1(3) . . . . ?
O2 S1 O1 C1 -4.8(3) . . . . ?
O2 S1 C15 F1 48.6(3) . . . . ?
O2 S1 C15 F2 -70.8(3) . . . . ?
O2 S1 C15 F3 168.8(2) . . . . ?
O3 S1 O1 C1 -142.3(2) . . . . ?
O3 S1 C15 F1 -179.8(2) . . . . ?
O3 S1 C15 F2 60.8(3) . . . . ?
O3 S1 C15 F3 -59.6(3) . . . . ?
O4 S2A C16A F4A 59.3(5) . . . . ?
O4 S2A C16A F5A -61.9(5) . . . . ?
O4 S2A C16A F6A 179.1(5) . . . . ?
O4 S2B C16B F4B 61.0(8) . . . . ?
O4 S2B C16B F5B -59.4(8) . . . . ?
O4 S2B C16B F6B 179.5(7) . . . . ?
O4 C5 C6 C7 -176.2(3) . . . . ?
O5A S2A O4 S2B 58.9(3) . . . . ?
O5A S2A O4 C5 17.5(5) . . . . ?
O5A S2A C16A F4A -54.0(6) . . . . ?
O5A S2A C16A F5A -175.3(6) . . . . ?
O5A S2A C16A F6A 65.8(6) . . . . ?
O6A S2A O4 S2B -166.1(3) . . . . ?
O6A S2A O4 C5 152.5(4) . . . . ?
O6A S2A C16A F4A 178.2(4) . . . . ?
O6A S2A C16A F5A 56.9(6) . . . . ?
O6A S2A C16A F6A -62.0(6) . . . . ?
O5B S2B O4 S2A -69.6(5) . . . . ?
O5B S2B O4 C5 80.8(5) . . . . ?
O5B S2B C16B F4B 172.5(9) . . . . ?
O5B S2B C16B F5B 52.0(9) . . . . ?
O5B S2B C16B F6B -69.0(9) . . . . ?
O6B S2B O4 S2A 150.9(4) . . . . ?
O6B S2B O4 C5 -58.7(4) . . . . ?
O6B S2B C16B F4B -54.1(9) . . . . ?
O6B S2B C16B F5B -174.5(8) . . . . ?
O6B S2B C16B F6B 64.4(8) . . . . ?
C1 C2 C3 C4 179.3(3) . . . . ?
C1 C2 C11 C10 -179.4(3) . . . . ?
C1 C2 C11 C12 -0.4(4) . . . . ?
C2 C1 C14 C13 -1.1(5) . . . . ?
C2 C3 C4 C5 178.9(3) . . . . ?
C2 C3 C4 C9 0.6(4) . . . . ?
C2 C11 C12 C13 0.8(5) . . . . ?
C3 C2 C11 C10 0.5(4) . . . . ?
C3 C2 C11 C12 179.5(3) . . . . ?
C3 C4 C5 O4 -2.8(4) . . . . ?
C3 C4 C5 C6 -178.0(3) . . . . ?
C3 C4 C9 C8 179.2(3) . . . . ?
C3 C4 C9 C10 -0.4(4) . . . . ?
C4 C5 C6 C7 -1.2(5) . . . . ?
C4 C9 C10 C11 0.3(5) . . . . ?
C5 C4 C9 C8 0.8(4) . . . . ?
C5 C4 C9 C10 -178.9(3) . . . . ?
C5 C6 C7 C8 0.8(5) . . . . ?
C6 C7 C8 C9 0.4(5) . . . . ?
C7 C8 C9 C4 -1.2(5) . . . . ?
C7 C8 C9 C10 178.5(3) . . . . ?
C8 C9 C10 C11 -179.3(3) . . . . ?
C9 C4 C5 O4 175.5(3) . . . . ?
C9 C4 C5 C6 0.4(4) . . . . ?
C9 C10 C11 C2 -0.4(5) . . . . ?
C9 C10 C11 C12 -179.3(3) . . . . ?
C10 C11 C12 C13 179.7(3) . . . . ?
C11 C2 C3 C4 -0.7(4) . . . . ?
C11 C12 C13 C14 -1.3(5) . . . . ?
C12 C13 C14 C1 1.4(5) . . . . ?
C14 C1 C2 C3 -179.3(3) . . . . ?
C14 C1 C2 C11 0.7(4) . . . . ?
C15 S1 O1 C1 108.4(2) . . . . ?
C16A S2A O4 S2B -51.6(2) . . . . ?
C16A S2A O4 C5 -93.0(4) . . . . ?
C16B S2B O4 S2A 40.9(3) . . . . ?
C16B S2B O4 C5 -168.6(4) . . . . ?

_olex2_date_sample_data_collection 2016-07-27
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.526
_oxdiff_exptl_absorpt_empirical_full_min 0.570
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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.
;
_shelxl_version_number           2014-3
####################################################################### 
# 
# 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_Anti-2
_database_code_depnum_ccdc_archive 'CCDC 1952348'
loop_
_audit_author_name
_audit_author_address
'Hans Georg Stammler'
;University of Bielefeld
Germany
;
_audit_update_record             
;
2019-09-09 deposited with the CCDC.	2021-05-06 downloaded from the CCDC.
;
# measured as jach11
_audit_creation_date             2019-08-19
_audit_creation_method           
;
Olex2 1.3-dev
(compiled 2019.03.18 svn.r3573 for OlexSys, GUI svn.r5894)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
  
;
_chemical_formula_moiety         '2(C18 H10), 0.5(C7 H8)'
_chemical_formula_sum            'C39.50 H24'
_chemical_formula_weight         498.59
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'

_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                   10.1399(8)
_cell_length_b                   11.8036(11)
_cell_length_c                   12.2024(11)
_cell_angle_alpha                104.246(4)
_cell_angle_beta                 90.620(5)
_cell_angle_gamma                111.016(5)
_cell_volume                     1313.5(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    34511
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      2.910
_shelx_estimated_absorpt_T_max   0.999
_shelx_estimated_absorpt_T_min   0.979
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  0.9986
_exptl_absorpt_correction_T_min  0.9789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             522
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_exptl_special_details           
;
  
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.061
_diffrn_reflns_av_unetI/netI     0.0706
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18989
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_min         3.039
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4680
_reflns_number_total             7266
_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       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect, Bruker AXS, 2004'
_computing_data_reduction        
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.328
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         7266
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1116
_refine_ls_R_factor_gt           0.0624
_refine_ls_restrained_S_all      1.022
_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)+(0.0613P)²+0.6144P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1564
_refine_special_details          
'The solvent toluene molecule is disordered at a center of inversion.'
_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. Others
 Fixed Sof: C37(0.5) H37(0.5) C38(0.5) H38(0.5) C39(0.5) H39(0.5) C40(0.5)
 H40(0.5) C41(0.5) H41(0.5) C42(0.5) C43(0.5) H43A(0.5) H43B(0.5) H43C(0.5)
3.a Ternary CH refined with riding coordinates:
 C3(H3), C10(H10), C21(H21), C28(H28)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14), C24(H24), C25(H25),
 C26(H26), C30(H30), C31(H31), C32(H32), C37(H37), C38(H38), C39(H39), C40(H40),
  C41(H41)
3.c Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C)
3.d :
 C16(H16), C18(H18), C34(H34), C36(H36)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.72831(18) 0.05414(17) 0.31338(15) 0.0221(4) Uani 1 1 d . . . . .
C2 C 0.60520(18) 0.01676(17) 0.36783(15) 0.0207(4) Uani 1 1 d . . . . .
C3 C 0.54709(18) 0.11017(16) 0.43737(15) 0.0199(4) Uani 1 1 d . . . . .
H3 H 0.585725 0.189883 0.413235 0.024 Uiso 1 1 calc R U . . .
C4 C 0.38696(18) 0.05625(17) 0.41094(15) 0.0200(4) Uani 1 1 d . . . . .
C5 C 0.30955(19) 0.12934(17) 0.39427(15) 0.0218(4) Uani 1 1 d . . . . .
C6 C 0.16043(19) 0.07444(18) 0.37478(16) 0.0250(4) Uani 1 1 d . . . . .
H6 H 0.107468 0.123429 0.363434 0.030 Uiso 1 1 calc R U . . .
C7 C 0.09069(19) -0.05094(18) 0.37211(16) 0.0267(4) Uani 1 1 d . . . . .
H7 H -0.010154 -0.087453 0.359962 0.032 Uiso 1 1 calc R U . . .
C8 C 0.16778(19) -0.12383(18) 0.38716(15) 0.0238(4) Uani 1 1 d . . . . .
H8 H 0.119503 -0.210199 0.383948 0.029 Uiso 1 1 calc R U . . .
C9 C 0.31514(18) -0.07034(17) 0.40684(15) 0.0208(4) Uani 1 1 d . . . . .
C10 C 0.40578(18) -0.14239(16) 0.42840(15) 0.0208(4) Uani 1 1 d . . . . .
H10 H 0.348489 -0.234647 0.399749 0.025 Uiso 1 1 calc R U . . .
C11 C 0.53363(18) -0.11015(17) 0.36233(15) 0.0207(4) Uani 1 1 d . . . . .
C12 C 0.58339(19) -0.19993(17) 0.30220(15) 0.0233(4) Uani 1 1 d . . . . .
H12 H 0.535766 -0.286114 0.299962 0.028 Uiso 1 1 calc R U . . .
C13 C 0.70354(19) -0.16337(18) 0.24500(16) 0.0247(4) Uani 1 1 d . . . . .
H13 H 0.736081 -0.225148 0.202176 0.030 Uiso 1 1 calc R U . . .
C14 C 0.77534(19) -0.03799(18) 0.25031(16) 0.0249(4) Uani 1 1 d . . . . .
H14 H 0.857017 -0.013888 0.211082 0.030 Uiso 1 1 calc R U . . .
C15 C 0.80707(19) 0.18648(19) 0.32492(16) 0.0257(4) Uani 1 1 d . . . . .
C16 C 0.8679(2) 0.2957(2) 0.33750(19) 0.0370(5) Uani 1 1 d . . . . .
H16 H 0.916775 0.383500 0.347615 0.044 Uiso 1 1 calc R U . . .
C17 C 0.38446(19) 0.25998(18) 0.39582(15) 0.0230(4) Uani 1 1 d . . . . .
C18 C 0.4506(2) 0.3643(2) 0.39380(18) 0.0314(5) Uani 1 1 d . . . . .
H18 H 0.503965 0.448384 0.392179 0.038 Uiso 1 1 calc R U . . .
C19 C -0.25625(19) 0.49305(17) 0.16812(15) 0.0222(4) Uani 1 1 d . . . . .
C20 C -0.15581(18) 0.46762(16) 0.09825(15) 0.0207(4) Uani 1 1 d . . . . .
C21 C 0.00245(18) 0.52042(16) 0.13607(15) 0.0206(4) Uani 1 1 d . . . . .
H21 H 0.017182 0.551824 0.220934 0.025 Uiso 1 1 calc R U . . .
C22 C 0.05518(18) 0.41316(16) 0.10079(15) 0.0199(4) Uani 1 1 d . . . . .
C23 C 0.14517(18) 0.38972(17) 0.17294(16) 0.0225(4) Uani 1 1 d . . . . .
C24 C 0.18743(19) 0.28718(18) 0.13364(16) 0.0249(4) Uani 1 1 d . . . . .
H24 H 0.247982 0.270851 0.182461 0.030 Uiso 1 1 calc R U . . .
C25 C 0.1417(2) 0.20998(18) 0.02470(16) 0.0264(4) Uani 1 1 d . . . . .
H25 H 0.170788 0.140772 -0.001317 0.032 Uiso 1 1 calc R U . . .
C26 C 0.05223(19) 0.23353(17) -0.04776(16) 0.0237(4) Uani 1 1 d . . . . .
H26 H 0.020449 0.180034 -0.122717 0.028 Uiso 1 1 calc R U . . .
C27 C 0.01011(18) 0.33475(17) -0.01017(15) 0.0216(4) Uani 1 1 d . . . . .
C28 C -0.08757(18) 0.36452(17) -0.08382(15) 0.0210(4) Uani 1 1 d . . . . .
H28 H -0.135667 0.288069 -0.148466 0.025 Uiso 1 1 calc R U . . .
C29 C -0.20082(18) 0.39062(17) -0.01277(15) 0.0214(4) Uani 1 1 d . . . . .
C30 C -0.34428(19) 0.34050(18) -0.05422(16) 0.0256(4) Uani 1 1 d . . . . .
H30 H -0.374516 0.287120 -0.129349 0.031 Uiso 1 1 calc R U . . .
C31 C -0.4432(2) 0.36845(19) 0.01409(17) 0.0282(4) Uani 1 1 d . . . . .
H31 H -0.540581 0.335986 -0.015051 0.034 Uiso 1 1 calc R U . . .
C32 C -0.4001(2) 0.44339(19) 0.12434(17) 0.0274(4) Uani 1 1 d . . . . .
H32 H -0.468330 0.461489 0.170945 0.033 Uiso 1 1 calc R U . . .
C33 C -0.21433(19) 0.56760(17) 0.28520(16) 0.0243(4) Uani 1 1 d . . . . .
C34 C -0.1836(2) 0.62650(19) 0.38150(18) 0.0325(5) Uani 1 1 d . . . . .
H34 H -0.158837 0.673861 0.458929 0.039 Uiso 1 1 calc R U . . .
C35 C 0.19253(19) 0.46775(17) 0.28851(16) 0.0227(4) Uani 1 1 d . . . . .
C36 C 0.2282(2) 0.52582(18) 0.38509(17) 0.0303(4) Uani 1 1 d . . . . .
H36 H 0.256762 0.572367 0.462503 0.036 Uiso 1 1 calc R U . . .
C37 C 0.4252(10) -0.0872(12) -0.0783(13) 0.021(2) Uani 0.5 1 d . . P A -1
H37 H 0.412902 -0.150984 -0.146885 0.026 Uiso 0.5 1 calc R U P A -1
C38 C 0.3091(5) -0.0843(4) -0.0214(4) 0.0375(10) Uani 0.5 1 d . . P A -1
H38 H 0.216320 -0.142563 -0.052579 0.045 Uiso 0.5 1 calc R U P A -1
C39 C 0.329(2) 0.0043(16) 0.0815(15) 0.048(4) Uani 0.5 1 d . . P A -1
H39 H 0.250016 0.003868 0.122200 0.058 Uiso 0.5 1 calc R U P A -1
C40 C 0.4611(5) 0.0926(4) 0.1265(4) 0.0387(10) Uani 0.5 1 d . . P A -1
H40 H 0.473735 0.154209 0.196713 0.046 Uiso 0.5 1 calc R U P A -1
C41 C 0.5754(19) 0.0892(17) 0.0661(16) 0.052(5) Uani 0.5 1 d . . P A -1
H41 H 0.667355 0.149324 0.097156 0.062 Uiso 0.5 1 calc R U P A -1
C42 C 0.5621(4) 0.0040(4) -0.0353(3) 0.0283(8) Uani 0.5 1 d . . P A -1
C43 C 0.6902(16) 0.0059(14) -0.0977(12) 0.032(2) Uani 0.5 1 d . . P A -1
H43A H 0.682398 -0.080699 -0.132794 0.047 Uiso 0.5 1 calc R U P A -1
H43B H 0.776560 0.049859 -0.043989 0.047 Uiso 0.5 1 calc R U P A -1
H43C H 0.694845 0.049823 -0.156944 0.047 Uiso 0.5 1 calc R U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.401(3) . ?
C1 C14 1.404(3) . ?
C1 C15 1.446(3) . ?
C2 C3 1.516(2) . ?
C2 C11 1.395(3) . ?
C3 H3 1.0000 . ?
C3 C4 1.514(2) . ?
C3 C10 1.613(2) 2_656 ?
C4 C5 1.404(2) . ?
C4 C9 1.396(3) . ?
C5 C6 1.406(2) . ?
C5 C17 1.449(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.384(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.393(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.389(2) . ?
C9 C10 1.517(2) . ?
C10 H10 1.0000 . ?
C10 C11 1.515(3) . ?
C11 C12 1.387(2) . ?
C12 H12 0.9500 . ?
C12 C13 1.395(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.380(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.182(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.179(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.402(3) . ?
C19 C32 1.404(3) . ?
C19 C33 1.448(3) . ?
C20 C21 1.517(2) . ?
C20 C29 1.397(2) . ?
C21 H21 1.0000 . ?
C21 C22 1.515(2) . ?
C21 C28 1.610(3) 2_565 ?
C22 C23 1.403(2) . ?
C22 C27 1.402(2) . ?
C23 C24 1.403(3) . ?
C23 C35 1.448(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.378(3) . ?
C25 H25 0.9500 . ?
C25 C26 1.402(3) . ?
C26 H26 0.9500 . ?
C26 C27 1.386(2) . ?
C27 C28 1.516(2) . ?
C28 H28 1.0000 . ?
C28 C29 1.520(2) . ?
C29 C30 1.393(2) . ?
C30 H30 0.9500 . ?
C30 C31 1.389(3) . ?
C31 H31 0.9500 . ?
C31 C32 1.381(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.181(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.185(3) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C37 C38 1.380(13) . ?
C37 C42 1.413(12) . ?
C38 H38 0.9500 . ?
C38 C39 1.380(18) . ?
C39 H39 0.9500 . ?
C39 C40 1.369(17) . ?
C40 H40 0.9500 . ?
C40 C41 1.387(18) . ?
C41 H41 0.9500 . ?
C41 C42 1.360(18) . ?
C42 C43 1.509(17) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C14 119.16(17) . . ?
C2 C1 C15 119.93(16) . . ?
C14 C1 C15 120.89(17) . . ?
C1 C2 C3 122.49(16) . . ?
C11 C2 C1 120.07(16) . . ?
C11 C2 C3 117.40(16) . . ?
C2 C3 H3 108.4 . . ?
C2 C3 C10 111.62(14) . 2_656 ?
C4 C3 C2 108.33(14) . . ?
C4 C3 H3 108.4 . . ?
C4 C3 C10 111.59(14) . 2_656 ?
C10 C3 H3 108.4 2_656 . ?
C5 C4 C3 122.59(16) . . ?
C9 C4 C3 117.74(15) . . ?
C9 C4 C5 119.64(15) . . ?
C4 C5 C6 119.58(17) . . ?
C4 C5 C17 119.58(15) . . ?
C6 C5 C17 120.83(16) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 C5 120.07(16) . . ?
C7 C6 H6 120.0 . . ?
C6 C7 H7 119.9 . . ?
C6 C7 C8 120.28(17) . . ?
C8 C7 H7 119.9 . . ?
C7 C8 H8 120.0 . . ?
C9 C8 C7 120.08(18) . . ?
C9 C8 H8 120.0 . . ?
C4 C9 C10 116.58(15) . . ?
C8 C9 C4 120.33(16) . . ?
C8 C9 C10 123.06(16) . . ?
C3 C10 H10 108.6 2_656 . ?
C9 C10 C3 110.76(13) . 2_656 ?
C9 C10 H10 108.6 . . ?
C11 C10 C3 111.48(13) . 2_656 ?
C11 C10 C9 108.69(15) . . ?
C11 C10 H10 108.6 . . ?
C2 C11 C10 116.95(15) . . ?
C12 C11 C2 120.17(17) . . ?
C12 C11 C10 122.82(16) . . ?
C11 C12 H12 120.1 . . ?
C11 C12 C13 119.86(18) . . ?
C13 C12 H12 120.1 . . ?
C12 C13 H13 119.8 . . ?
C14 C13 C12 120.36(16) . . ?
C14 C13 H13 119.8 . . ?
C1 C14 H14 119.8 . . ?
C13 C14 C1 120.32(17) . . ?
C13 C14 H14 119.8 . . ?
C16 C15 C1 177.3(2) . . ?
C15 C16 H16 180.0 . . ?
C18 C17 C5 176.42(19) . . ?
C17 C18 H18 180.0 . . ?
C20 C19 C32 119.41(17) . . ?
C20 C19 C33 121.03(16) . . ?
C32 C19 C33 119.55(17) . . ?
C19 C20 C21 123.47(16) . . ?
C29 C20 C19 119.53(16) . . ?
C29 C20 C21 117.00(15) . . ?
C20 C21 H21 108.5 . . ?
C20 C21 C28 111.94(14) . 2_565 ?
C22 C21 C20 107.57(14) . . ?
C22 C21 H21 108.5 . . ?
C22 C21 C28 111.62(14) . 2_565 ?
C28 C21 H21 108.5 2_565 . ?
C23 C22 C21 123.42(16) . . ?
C27 C22 C21 117.05(15) . . ?
C27 C22 C23 119.54(16) . . ?
C22 C23 C24 119.60(17) . . ?
C22 C23 C35 121.10(16) . . ?
C24 C23 C35 119.28(16) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 C23 120.46(17) . . ?
C25 C24 H24 119.8 . . ?
C24 C25 H25 120.0 . . ?
C24 C25 C26 120.05(17) . . ?
C26 C25 H25 120.0 . . ?
C25 C26 H26 120.0 . . ?
C27 C26 C25 120.08(17) . . ?
C27 C26 H26 120.0 . . ?
C22 C27 C28 117.06(15) . . ?
C26 C27 C22 120.26(17) . . ?
C26 C27 C28 122.67(16) . . ?
C21 C28 H28 108.1 2_565 . ?
C27 C28 C21 112.29(14) . 2_565 ?
C27 C28 H28 108.1 . . ?
C27 C28 C29 108.00(14) . . ?
C29 C28 C21 112.06(14) . 2_565 ?
C29 C28 H28 108.1 . . ?
C20 C29 C28 117.19(15) . . ?
C30 C29 C20 120.27(17) . . ?
C30 C29 C28 122.54(16) . . ?
C29 C30 H30 119.9 . . ?
C31 C30 C29 120.13(17) . . ?
C31 C30 H30 119.9 . . ?
C30 C31 H31 120.0 . . ?
C32 C31 C30 120.08(17) . . ?
C32 C31 H31 120.0 . . ?
C19 C32 H32 119.7 . . ?
C31 C32 C19 120.55(18) . . ?
C31 C32 H32 119.7 . . ?
C34 C33 C19 178.2(2) . . ?
C33 C34 H34 180.0 . . ?
C36 C35 C23 176.4(2) . . ?
C35 C36 H36 180.0 . . ?
C38 C37 H37 119.8 . . ?
C38 C37 C42 120.4(10) . . ?
C42 C37 H37 119.8 . . ?
C37 C38 H38 120.4 . . ?
C37 C38 C39 119.2(10) . . ?
C39 C38 H38 120.4 . . ?
C38 C39 H39 119.1 . . ?
C40 C39 C38 121.8(15) . . ?
C40 C39 H39 119.1 . . ?
C39 C40 H40 121.1 . . ?
C39 C40 C41 117.7(11) . . ?
C41 C40 H40 121.1 . . ?
C40 C41 H41 118.4 . . ?
C42 C41 C40 123.2(14) . . ?
C42 C41 H41 118.4 . . ?
C37 C42 C43 121.7(8) . . ?
C41 C42 C37 117.6(12) . . ?
C41 C42 C43 120.8(10) . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 138.41(17) . . . . ?
C1 C2 C3 C10 -98.34(19) . . . 2_656 ?
C1 C2 C11 C10 176.92(16) . . . . ?
C1 C2 C11 C12 -0.5(3) . . . . ?
C2 C1 C14 C13 -2.0(3) . . . . ?
C2 C3 C4 C5 -137.46(17) . . . . ?
C2 C3 C4 C9 44.6(2) . . . . ?
C2 C11 C12 C13 -1.4(3) . . . . ?
C3 C2 C11 C10 -1.1(2) . . . . ?
C3 C2 C11 C12 -178.54(16) . . . . ?
C3 C4 C5 C6 -177.30(16) . . . . ?
C3 C4 C5 C17 3.5(2) . . . . ?
C3 C4 C9 C8 177.61(16) . . . . ?
C3 C4 C9 C10 -0.6(2) . . . . ?
C3 C10 C11 C2 -76.96(19) 2_656 . . . ?
C3 C10 C11 C12 100.41(19) 2_656 . . . ?
C4 C5 C6 C7 0.0(3) . . . . ?
C4 C9 C10 C3 78.37(19) . . . 2_656 ?
C4 C9 C10 C11 -44.4(2) . . . . ?
C5 C4 C9 C8 -0.4(3) . . . . ?
C5 C4 C9 C10 -178.61(16) . . . . ?
C5 C6 C7 C8 -0.9(3) . . . . ?
C6 C7 C8 C9 1.1(3) . . . . ?
C7 C8 C9 C4 -0.4(3) . . . . ?
C7 C8 C9 C10 177.63(17) . . . . ?
C8 C9 C10 C3 -99.76(19) . . . 2_656 ?
C8 C9 C10 C11 137.44(17) . . . . ?
C9 C4 C5 C6 0.6(3) . . . . ?
C9 C4 C5 C17 -178.52(16) . . . . ?
C9 C10 C11 C2 45.4(2) . . . . ?
C9 C10 C11 C12 -137.23(17) . . . . ?
C10 C3 C4 C5 99.27(19) 2_656 . . . ?
C10 C3 C4 C9 -78.70(19) 2_656 . . . ?
C10 C11 C12 C13 -178.71(16) . . . . ?
C11 C2 C3 C4 -43.6(2) . . . . ?
C11 C2 C3 C10 79.63(18) . . . 2_656 ?
C11 C12 C13 C14 1.7(3) . . . . ?
C12 C13 C14 C1 0.0(3) . . . . ?
C14 C1 C2 C3 -179.87(16) . . . . ?
C14 C1 C2 C11 2.2(3) . . . . ?
C15 C1 C2 C3 1.6(3) . . . . ?
C15 C1 C2 C11 -176.29(16) . . . . ?
C15 C1 C14 C13 176.50(17) . . . . ?
C17 C5 C6 C7 179.15(17) . . . . ?
C19 C20 C21 C22 133.82(18) . . . . ?
C19 C20 C21 C28 -103.2(2) . . . 2_565 ?
C19 C20 C29 C28 -178.96(16) . . . . ?
C19 C20 C29 C30 0.7(3) . . . . ?
C20 C19 C32 C31 1.0(3) . . . . ?
C20 C21 C22 C23 -133.99(18) . . . . ?
C20 C21 C22 C27 46.0(2) . . . . ?
C20 C29 C30 C31 1.0(3) . . . . ?
C21 C20 C29 C28 1.5(2) . . . . ?
C21 C20 C29 C30 -178.85(16) . . . . ?
C21 C22 C23 C24 179.21(17) . . . . ?
C21 C22 C23 C35 0.8(3) . . . . ?
C21 C22 C27 C26 -178.96(16) . . . . ?
C21 C22 C27 C28 -0.3(2) . . . . ?
C21 C28 C29 C20 -79.83(19) 2_565 . . . ?
C21 C28 C29 C30 100.5(2) 2_565 . . . ?
C22 C23 C24 C25 0.3(3) . . . . ?
C22 C27 C28 C21 79.1(2) . . . 2_565 ?
C22 C27 C28 C29 -45.0(2) . . . . ?
C23 C22 C27 C26 1.1(3) . . . . ?
C23 C22 C27 C28 179.71(16) . . . . ?
C23 C24 C25 C26 0.0(3) . . . . ?
C24 C25 C26 C27 0.3(3) . . . . ?
C25 C26 C27 C22 -0.8(3) . . . . ?
C25 C26 C27 C28 -179.37(17) . . . . ?
C26 C27 C28 C21 -102.28(19) . . . 2_565 ?
C26 C27 C28 C29 133.66(18) . . . . ?
C27 C22 C23 C24 -0.8(3) . . . . ?
C27 C22 C23 C35 -179.26(17) . . . . ?
C27 C28 C29 C20 44.4(2) . . . . ?
C27 C28 C29 C30 -135.27(18) . . . . ?
C28 C21 C22 C23 102.84(19) 2_565 . . . ?
C28 C21 C22 C27 -77.14(19) 2_565 . . . ?
C28 C29 C30 C31 -179.38(18) . . . . ?
C29 C20 C21 C22 -46.7(2) . . . . ?
C29 C20 C21 C28 76.30(19) . . . 2_565 ?
C29 C30 C31 C32 -1.7(3) . . . . ?
C30 C31 C32 C19 0.6(3) . . . . ?
C32 C19 C20 C21 177.82(17) . . . . ?
C32 C19 C20 C29 -1.7(3) . . . . ?
C33 C19 C20 C21 -3.4(3) . . . . ?
C33 C19 C20 C29 177.12(17) . . . . ?
C33 C19 C32 C31 -177.79(18) . . . . ?
C35 C23 C24 C25 178.78(18) . . . . ?
C37 C38 C39 C40 3(2) . . . . ?
C38 C37 C42 C41 3(2) . . . . ?
C38 C37 C42 C43 -177.9(11) . . . . ?
C38 C39 C40 C41 -1(2) . . . . ?
C39 C40 C41 C42 1(2) . . . . ?
C40 C41 C42 C37 -2(2) . . . . ?
C40 C41 C42 C43 179.3(12) . . . . ?
C42 C37 C38 C39 -3.7(17) . . . . ?

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

data_Syn-2
_database_code_depnum_ccdc_archive 'CCDC 1952347'
loop_
_audit_author_name
_audit_author_address
'Hans Georg Stammler'
;University of Bielefeld
Germany
;
_audit_update_record             
;
2019-09-09 deposited with the CCDC.	2021-05-06 downloaded from the CCDC.
;
# measured as niermeier25_lt
_audit_creation_date             2016-11-17
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H20'
_chemical_formula_sum            'C36 H20'
_chemical_formula_weight         452.52
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C36 H20'
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'

_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                   10.03642(5)
_cell_length_b                   20.42255(9)
_cell_length_c                   12.53918(8)
_cell_angle_alpha                90
_cell_angle_beta                 111.7520(7)
_cell_angle_gamma                90
_cell_volume                     2387.14(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    52436
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.2910
_cell_measurement_theta_min      3.7850
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.903
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             944.0
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.0838
0 -1 0 0.0838
0 -5 2 0.0956
0 5 -2 0.0956
-1 2 5 0.1029
1 -2 -5 0.1029
5 -5 -1 0.0749
5 5 1 0.0870
-5 -5 -1 0.0870
-5 4 0 0.0330

_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.125
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
0.0000 1.0000 -0.0000 0.0152 0.0582 0.0455
-0.0000 -1.0000 0.0000 -0.0152 -0.0582 -0.0455
-0.0000 -5.0000 2.0000 -0.0481 -0.1336 -0.4383
0.0000 5.0000 -2.0000 0.0481 0.1336 0.4383
-1.0000 2.0000 5.0000 0.2428 0.4394 -0.3931
1.0000 -2.0000 -5.0000 -0.2428 -0.4394 0.3931
5.0000 -5.0000 -1.0000 -0.8051 -0.0160 -0.3362
5.0000 5.0000 1.0000 -0.6256 0.7237 -0.0919
-5.0000 -5.0000 -1.0000 0.6256 -0.7237 0.0919
-5.0000 4.0000 -0.0000 0.7761 -0.1210 0.3961

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_unetI/netI     0.0066
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            81574
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.323
_diffrn_reflns_theta_min         4.330
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6228
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.9998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -115.00 -20.00   1.00    1.58    --  -42.58 -38.00 150.00   95
  2  ω    -69.00  28.00   1.00    1.58    --  -42.58  57.00 -90.00   97
  3  ω   -116.00 -11.00   1.00    1.58    --  -42.58 -77.00  90.00  105
  4  ω   -116.00 -11.00   1.00    1.58    --  -42.58 -77.00-120.00  105
  5  ω   -116.00 -11.00   1.00    1.58    --  -42.58 -77.00 150.00  105
  6  ω   -113.00 -16.00   1.00    1.58    --  -42.58 -57.00 -30.00   97
  7  ω   -116.00 -11.00   1.00    1.58    --  -42.58 -77.00 -60.00  105
  8  ω   -113.00 -16.00   1.00    1.58    --  -42.58 -57.00 120.00   97
  9  ω   -116.00 -11.00   1.00    1.58    --  -42.58 -77.00  30.00  105
 10  ω    -28.00  69.00   1.00    1.58    --   42.58 -57.00  90.00   97
 11  ω      1.00  82.00   1.00    1.58    --   42.58 -99.00   0.00   81
 12  ω     80.00 178.00   1.00    6.30    --  111.00  77.00 -90.00   98
 13  ω     81.00 178.00   1.00    6.30    --  111.00  70.00  51.16   97
 14  ω     37.00 142.00   1.00    6.30    --  111.00 -77.00 -30.00  105
 15  ω     80.00 178.00   1.00    6.30    --  111.00  77.00  30.00   98
 16  ω     80.00 178.00   1.00    6.30    --  111.00  77.00   0.00   98
 17  ω     81.00 178.00   1.00    6.30    --  111.00  70.00 134.26   97
 18  ω     39.00 121.00   1.00    6.30    --  111.00-125.00 -90.00   82
 19  ω     83.00 178.00   1.00    6.30    --  111.00  61.00 120.00   95
 20  ω     81.00 178.00   1.00    6.30    --  111.00  70.00 -96.91   97
 21  ω     80.00 178.00   1.00    6.30    --  111.00  77.00 -30.00   98
 22  ω     83.00 178.00   1.00    6.30    --  111.00  61.00-150.00   95
 23  ω     80.00 178.00   1.00    6.30    --  111.00  77.00  60.00   98
 24  ω     39.00 121.00   1.00    6.30    --  111.00-125.00  90.00   82
 25  ω     81.00 178.00   1.00    6.30    --  111.00  71.00 -39.00   97
 26  ω     30.00 109.00   1.00    6.30    --  111.00 -94.00 -60.00   79
 27  ω     80.00 178.00   1.00    6.30    --  111.00  75.00 -54.29   98
 28  ω     37.00 142.00   1.00    6.30    --  111.00 -77.00 150.00  105
 29  ω     83.00 178.00   1.00    6.30    --  111.00  61.00   0.00   95
 30  ω     30.00 109.00   1.00    6.30    --  111.00 -94.00 120.00   79
 31  ω     83.00 178.00   1.00    6.30    --  111.00  61.00-180.00   95
 32  ω     80.00 178.00   1.00    6.30    --  111.00  77.00-150.00   98
 33  ω     80.00 178.00   1.00    6.30    --  111.00  77.00 150.00   98
 34  ω     83.00 178.00   1.00    6.30    --  111.00  61.00  90.00   95
 35  ω     82.00 178.00   1.00    6.30    --  111.00  66.00  94.04   96
 36  ω     83.00 178.00   1.00    6.30    --  111.00  61.00 -60.00   95
 37  ω     80.00 178.00   1.00    6.30    --  111.00  77.00-180.00   98
 38  ω     80.00 178.00   1.00    6.30    --  111.00  77.00  90.00   98
 39  ω     87.00 178.00   1.00    6.30    --  111.00  45.00 -90.00   91
 40  ω     83.00 178.00   1.00    6.30    --  111.00  61.00  30.00   95
 41  ω     87.00 178.00   1.00    6.30    --  111.00  45.00 150.00   91
 42  ω     83.00 178.00   1.00    6.30    --  111.00  61.00-120.00   95
 43  ω     83.00 178.00   1.00    6.30    --  111.00  61.00 150.00   95
 44  ω     80.00 178.00   1.00    6.30    --  111.00  77.00-120.00   98
 45  ω     80.00 178.00   1.00    6.30    --  111.00  75.00 175.34   98
 46  ω     86.00 178.00   1.00    6.30    --  111.00  51.00 173.98   92
 47  ω     83.00 178.00   1.00    6.30    --  111.00  64.00 -58.82   95
 48  ω   -116.00 -11.00   1.00    1.58    --  -42.58 -77.00-180.00  105
 49  ω   -113.00 -16.00   1.00    1.58    --  -42.58 -57.00 -90.00   97
 50  ω   -113.00 -16.00   1.00    1.58    --  -42.58 -57.00-150.00   97
 51  ω   -115.00 -20.00   1.00    1.58    --  -42.58 -38.00-120.00   95
 52  ω   -113.00 -16.00   1.00    1.58    --  -42.58 -57.00  60.00   97
 53  ω   -113.00 -16.00   1.00    1.58    --  -42.58 -57.00 150.00   97
 54  ω   -115.00 -20.00   1.00    1.58    --  -42.58 -38.00  30.00   95
 55  ω   -115.00 -20.00   1.00    1.58    --  -42.58 -38.00-150.00   95
 56  ω   -115.00 -20.00   1.00    1.58    --  -42.58 -38.00 -90.00   95
 57  ω   -115.00 -20.00   1.00    1.58    --  -42.58 -38.00  60.00   95
 58  ω     57.00 129.00   1.00    1.58    --   42.58 178.00-120.00   72
 59  ω      6.00 121.00   1.00    1.58    --   42.58  19.00  90.00  115
 60  ω     13.00  56.00   1.00    1.58    --   42.58  71.00 -39.00   43
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1430728000
_diffrn_orient_matrix_UB_12      0.0151758000
_diffrn_orient_matrix_UB_13      0.0138725000
_diffrn_orient_matrix_UB_21      0.0707751000
_diffrn_orient_matrix_UB_22      0.0582162000
_diffrn_orient_matrix_UB_23      0.0787524000
_diffrn_orient_matrix_UB_31      -0.0428130000
_diffrn_orient_matrix_UB_32      0.0455036000
_diffrn_orient_matrix_UB_33      -0.1053745000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4582
_reflns_number_total             4718
_reflns_odcompleteness_completeness 99.98
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.251
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4718
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0370
_refine_ls_restrained_S_all      1.043
_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+0.7788P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.0994
_refine_special_details          ?
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
C1 C -0.16523(10) 0.02662(5) 0.36616(8) 0.0177(2) Uani 1 1 d . . . . .
C2 C -0.06871(10) 0.07737(5) 0.37150(8) 0.0163(2) Uani 1 1 d . . . . .
C3 C -0.00228(10) 0.08748(5) 0.28172(8) 0.0158(2) Uani 1 1 d . . . . .
H3 H -0.014305 0.047154 0.236751 0.019 Uiso 1 1 calc R . . . .
C4 C 0.15622(10) 0.09973(5) 0.34388(8) 0.0163(2) Uani 1 1 d . . . . .
C5 C 0.26190(10) 0.07001(5) 0.31200(9) 0.0186(2) Uani 1 1 d . . . . .
C6 C 0.40694(11) 0.08294(5) 0.37575(10) 0.0239(2) Uani 1 1 d . . . . .
H6 H 0.477651 0.063279 0.355342 0.029 Uiso 1 1 calc R . . . .
C7 C 0.44505(11) 0.12476(5) 0.46870(10) 0.0267(2) Uani 1 1 d . . . . .
H7 H 0.541513 0.132670 0.511191 0.032 Uiso 1 1 calc R . . . .
C8 C 0.34039(11) 0.15525(5) 0.49949(9) 0.0228(2) Uani 1 1 d . . . . .
H8 H 0.367001 0.183635 0.561904 0.027 Uiso 1 1 calc R . . . .
C9 C 0.19629(10) 0.14318(5) 0.43683(8) 0.0176(2) Uani 1 1 d . . . . .
C10 C 0.07626(10) 0.17422(5) 0.46575(8) 0.0174(2) Uani 1 1 d . . . . .
H10 H 0.117528 0.191922 0.543840 0.021 Uiso 1 1 calc R . . . .
C11 C -0.02860(10) 0.12076(5) 0.46424(8) 0.0168(2) Uani 1 1 d . . . . .
C12 C -0.08347(11) 0.11418(5) 0.55031(8) 0.0194(2) Uani 1 1 d . . . . .
H12 H -0.055486 0.143132 0.611953 0.023 Uiso 1 1 calc R . . . .
C13 C -0.18042(11) 0.06424(5) 0.54434(9) 0.0213(2) Uani 1 1 d . . . . .
H13 H -0.217910 0.060080 0.601616 0.026 Uiso 1 1 calc R . . . .
C14 C -0.22095(10) 0.02082(5) 0.45324(9) 0.0201(2) Uani 1 1 d . . . . .
H14 H -0.285665 -0.012492 0.449614 0.024 Uiso 1 1 calc R . . . .
C15 C -0.20738(10) -0.02044(5) 0.27427(9) 0.0211(2) Uani 1 1 d . . . . .
C16 C -0.24432(12) -0.06082(6) 0.20081(11) 0.0318(3) Uani 1 1 d . . . . .
H16 H -0.273216 -0.092414 0.143335 0.038 Uiso 1 1 calc R . . . .
C17 C 0.22463(11) 0.02675(5) 0.21487(9) 0.0218(2) Uani 1 1 d . . . . .
C18 C 0.19725(13) -0.00833(6) 0.13384(11) 0.0319(3) Uani 1 1 d . . . . .
H18 H 0.175830 -0.035767 0.070478 0.038 Uiso 1 1 calc R . . . .
C19 C -0.34233(10) 0.16051(5) 0.16223(8) 0.0180(2) Uani 1 1 d . . . . .
C20 C -0.19797(10) 0.17661(5) 0.22223(8) 0.0165(2) Uani 1 1 d . . . . .
C21 C -0.07586(10) 0.14702(5) 0.19511(8) 0.0157(2) Uani 1 1 d . . . . .
H21 H -0.114504 0.129780 0.116607 0.019 Uiso 1 1 calc R . . . .
C22 C 0.03055(10) 0.20105(5) 0.20069(8) 0.0161(2) Uani 1 1 d . . . . .
C23 C 0.09464(10) 0.20857(5) 0.11924(8) 0.0173(2) Uani 1 1 d . . . . .
C24 C 0.19157(10) 0.26021(5) 0.13122(9) 0.0193(2) Uani 1 1 d . . . . .
H24 H 0.234195 0.265440 0.077344 0.023 Uiso 1 1 calc R . . . .
C25 C 0.22416(11) 0.30330(5) 0.22223(9) 0.0207(2) Uani 1 1 d . . . . .
H25 H 0.288111 0.337454 0.229115 0.025 Uiso 1 1 calc R . . . .
C26 C 0.16171(11) 0.29576(5) 0.30352(9) 0.0199(2) Uani 1 1 d . . . . .
H26 H 0.184107 0.324672 0.364994 0.024 Uiso 1 1 calc R . . . .
C27 C 0.06579(10) 0.24496(5) 0.29269(8) 0.0172(2) Uani 1 1 d . . . . .
C28 C -0.00291(10) 0.23318(5) 0.37968(8) 0.0170(2) Uani 1 1 d . . . . .
H28 H 0.006592 0.273168 0.425117 0.020 Uiso 1 1 calc R . . . .
C29 C -0.16102(10) 0.22016(5) 0.31493(8) 0.0170(2) Uani 1 1 d . . . . .
C30 C -0.26796(11) 0.24904(5) 0.34444(9) 0.0202(2) Uani 1 1 d . . . . .
H30 H -0.243495 0.279232 0.404161 0.024 Uiso 1 1 calc R . . . .
C31 C -0.41125(11) 0.23314(5) 0.28536(9) 0.0232(2) Uani 1 1 d . . . . .
H31 H -0.482054 0.252238 0.306350 0.028 Uiso 1 1 calc R . . . .
C32 C -0.44868(11) 0.18896(5) 0.19538(9) 0.0218(2) Uani 1 1 d . . . . .
H32 H -0.544534 0.178020 0.156670 0.026 Uiso 1 1 calc R . . . .
C33 C -0.38333(10) 0.11432(5) 0.06909(9) 0.0198(2) Uani 1 1 d . . . . .
C34 C -0.41933(11) 0.07605(6) -0.00832(10) 0.0259(2) Uani 1 1 d . . . . .
H34 H -0.447382 0.046227 -0.068663 0.031 Uiso 1 1 calc R . . . .
C35 C 0.06440(11) 0.16419(5) 0.02433(9) 0.0199(2) Uani 1 1 d . . . . .
C36 C 0.04355(12) 0.12775(6) -0.05441(9) 0.0270(2) Uani 1 1 d . . . . .
H36 H 0.027274 0.099304 -0.115882 0.032 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
C1 C2 1.4033(14) . ?
C1 C14 1.4042(14) . ?
C1 C15 1.4383(14) . ?
C2 C3 1.5201(13) . ?
C2 C11 1.3973(13) . ?
C3 H3 0.9800 . ?
C3 C4 1.5105(13) . ?
C3 C21 1.6152(13) . ?
C4 C5 1.4027(13) . ?
C4 C9 1.4001(13) . ?
C5 C6 1.4019(14) . ?
C5 C17 1.4373(14) . ?
C6 H6 0.9300 . ?
C6 C7 1.3798(15) . ?
C7 H7 0.9300 . ?
C7 C8 1.3931(15) . ?
C8 H8 0.9300 . ?
C8 C9 1.3884(14) . ?
C9 C10 1.5194(13) . ?
C10 H10 0.9800 . ?
C10 C11 1.5117(13) . ?
C10 C28 1.6157(13) . ?
C11 C12 1.3880(14) . ?
C12 H12 0.9300 . ?
C12 C13 1.3924(15) . ?
C13 H13 0.9300 . ?
C13 C14 1.3828(15) . ?
C14 H14 0.9300 . ?
C15 C16 1.1886(16) . ?
C16 H16 0.9300 . ?
C17 C18 1.1892(16) . ?
C18 H18 0.9300 . ?
C19 C20 1.4019(14) . ?
C19 C32 1.4066(14) . ?
C19 C33 1.4377(14) . ?
C20 C21 1.5138(12) . ?
C20 C29 1.4002(13) . ?
C21 H21 0.9800 . ?
C21 C22 1.5192(13) . ?
C22 C23 1.4026(13) . ?
C22 C27 1.3992(13) . ?
C23 C24 1.4047(14) . ?
C23 C35 1.4360(14) . ?
C24 H24 0.9300 . ?
C24 C25 1.3809(14) . ?
C25 H25 0.9300 . ?
C25 C26 1.3889(14) . ?
C26 H26 0.9300 . ?
C26 C27 1.3873(14) . ?
C27 C28 1.5103(13) . ?
C28 H28 0.9800 . ?
C28 C29 1.5142(13) . ?
C29 C30 1.3897(14) . ?
C30 H30 0.9300 . ?
C30 C31 1.3902(15) . ?
C31 H31 0.9300 . ?
C31 C32 1.3835(15) . ?
C32 H32 0.9300 . ?
C33 C34 1.1932(16) . ?
C34 H34 0.9300 . ?
C35 C36 1.1914(15) . ?
C36 H36 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
C2 C1 C14 119.47(9) . . ?
C2 C1 C15 121.65(9) . . ?
C14 C1 C15 118.88(9) . . ?
C1 C2 C3 123.33(9) . . ?
C11 C2 C1 119.27(9) . . ?
C11 C2 C3 117.39(8) . . ?
C2 C3 H3 108.5 . . ?
C2 C3 C21 112.55(7) . . ?
C4 C3 C2 107.91(8) . . ?
C4 C3 H3 108.5 . . ?
C4 C3 C21 110.73(7) . . ?
C21 C3 H3 108.5 . . ?
C5 C4 C3 122.98(9) . . ?
C9 C4 C3 117.20(8) . . ?
C9 C4 C5 119.82(9) . . ?
C4 C5 C17 121.37(9) . . ?
C6 C5 C4 119.41(9) . . ?
C6 C5 C17 119.22(9) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 C5 120.17(9) . . ?
C7 C6 H6 119.9 . . ?
C6 C7 H7 119.7 . . ?
C6 C7 C8 120.62(10) . . ?
C8 C7 H7 119.7 . . ?
C7 C8 H8 120.1 . . ?
C9 C8 C7 119.87(10) . . ?
C9 C8 H8 120.1 . . ?
C4 C9 C10 117.04(8) . . ?
C8 C9 C4 120.08(9) . . ?
C8 C9 C10 122.86(9) . . ?
C9 C10 H10 108.3 . . ?
C9 C10 C28 112.87(8) . . ?
C11 C10 C9 107.80(8) . . ?
C11 C10 H10 108.3 . . ?
C11 C10 C28 111.23(8) . . ?
C28 C10 H10 108.3 . . ?
C2 C11 C10 116.93(8) . . ?
C12 C11 C2 120.72(9) . . ?
C12 C11 C10 122.35(9) . . ?
C11 C12 H12 120.0 . . ?
C11 C12 C13 119.98(9) . . ?
C13 C12 H12 120.0 . . ?
C12 C13 H13 120.0 . . ?
C14 C13 C12 120.00(9) . . ?
C14 C13 H13 120.0 . . ?
C1 C14 H14 119.7 . . ?
C13 C14 C1 120.55(9) . . ?
C13 C14 H14 119.7 . . ?
C16 C15 C1 177.44(12) . . ?
C15 C16 H16 180.0 . . ?
C18 C17 C5 178.01(11) . . ?
C17 C18 H18 180.0 . . ?
C20 C19 C32 119.41(9) . . ?
C20 C19 C33 121.17(9) . . ?
C32 C19 C33 119.40(9) . . ?
C19 C20 C21 123.20(9) . . ?
C29 C20 C19 119.84(9) . . ?
C29 C20 C21 116.91(8) . . ?
C3 C21 H21 108.5 . . ?
C20 C21 C3 110.85(7) . . ?
C20 C21 H21 108.5 . . ?
C20 C21 C22 108.27(8) . . ?
C22 C21 C3 112.17(7) . . ?
C22 C21 H21 108.5 . . ?
C23 C22 C21 123.38(9) . . ?
C27 C22 C21 117.52(8) . . ?
C27 C22 C23 119.10(9) . . ?
C22 C23 C24 119.38(9) . . ?
C22 C23 C35 121.42(9) . . ?
C24 C23 C35 119.20(9) . . ?
C23 C24 H24 119.7 . . ?
C25 C24 C23 120.62(9) . . ?
C25 C24 H24 119.7 . . ?
C24 C25 H25 119.9 . . ?
C24 C25 C26 120.18(9) . . ?
C26 C25 H25 119.9 . . ?
C25 C26 H26 120.1 . . ?
C27 C26 C25 119.77(9) . . ?
C27 C26 H26 120.1 . . ?
C22 C27 C28 116.73(8) . . ?
C26 C27 C22 120.94(9) . . ?
C26 C27 C28 122.31(9) . . ?
C10 C28 H28 108.4 . . ?
C27 C28 C10 110.98(8) . . ?
C27 C28 H28 108.4 . . ?
C27 C28 C29 107.99(8) . . ?
C29 C28 C10 112.68(7) . . ?
C29 C28 H28 108.4 . . ?
C20 C29 C28 117.34(8) . . ?
C30 C29 C20 119.84(9) . . ?
C30 C29 C28 122.82(9) . . ?
C29 C30 H30 119.8 . . ?
C29 C30 C31 120.50(9) . . ?
C31 C30 H30 119.8 . . ?
C30 C31 H31 120.0 . . ?
C32 C31 C30 120.10(9) . . ?
C32 C31 H31 120.0 . . ?
C19 C32 H32 119.9 . . ?
C31 C32 C19 120.26(9) . . ?
C31 C32 H32 119.9 . . ?
C34 C33 C19 179.07(10) . . ?
C33 C34 H34 180.0 . . ?
C36 C35 C23 177.92(11) . . ?
C35 C36 H36 180.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -134.20(9) . . . . ?
C1 C2 C3 C21 103.32(10) . . . . ?
C1 C2 C11 C10 179.67(8) . . . . ?
C1 C2 C11 C12 -0.20(14) . . . . ?
C2 C1 C14 C13 -0.63(14) . . . . ?
C2 C3 C4 C5 135.61(9) . . . . ?
C2 C3 C4 C9 -44.71(11) . . . . ?
C2 C3 C21 C20 -2.25(11) . . . . ?
C2 C3 C21 C22 118.93(9) . . . . ?
C2 C11 C12 C13 -0.49(14) . . . . ?
C3 C2 C11 C10 0.62(12) . . . . ?
C3 C2 C11 C12 -179.26(8) . . . . ?
C3 C4 C5 C6 -178.66(9) . . . . ?
C3 C4 C5 C17 1.64(14) . . . . ?
C3 C4 C9 C8 178.31(9) . . . . ?
C3 C4 C9 C10 -0.39(12) . . . . ?
C3 C21 C22 C23 100.84(10) . . . . ?
C3 C21 C22 C27 -78.82(10) . . . . ?
C4 C3 C21 C20 -123.12(8) . . . . ?
C4 C3 C21 C22 -1.94(10) . . . . ?
C4 C5 C6 C7 -0.26(15) . . . . ?
C4 C9 C10 C11 45.82(11) . . . . ?
C4 C9 C10 C28 -77.42(10) . . . . ?
C5 C4 C9 C8 -2.00(14) . . . . ?
C5 C4 C9 C10 179.30(8) . . . . ?
C5 C6 C7 C8 -0.83(17) . . . . ?
C6 C7 C8 C9 0.50(17) . . . . ?
C7 C8 C9 C4 0.92(15) . . . . ?
C7 C8 C9 C10 179.54(9) . . . . ?
C8 C9 C10 C11 -132.84(10) . . . . ?
C8 C9 C10 C28 103.92(11) . . . . ?
C9 C4 C5 C6 1.67(14) . . . . ?
C9 C4 C5 C17 -178.02(9) . . . . ?
C9 C10 C11 C2 -45.76(11) . . . . ?
C9 C10 C11 C12 134.11(9) . . . . ?
C9 C10 C28 C27 -2.04(11) . . . . ?
C9 C10 C28 C29 119.22(9) . . . . ?
C10 C11 C12 C13 179.64(9) . . . . ?
C10 C28 C29 C20 -77.13(10) . . . . ?
C10 C28 C29 C30 102.41(10) . . . . ?
C11 C2 C3 C4 44.81(11) . . . . ?
C11 C2 C3 C21 -77.66(10) . . . . ?
C11 C10 C28 C27 -123.35(9) . . . . ?
C11 C10 C28 C29 -2.10(11) . . . . ?
C11 C12 C13 C14 0.62(15) . . . . ?
C12 C13 C14 C1 -0.06(14) . . . . ?
C14 C1 C2 C3 179.75(8) . . . . ?
C14 C1 C2 C11 0.75(14) . . . . ?
C15 C1 C2 C3 0.62(14) . . . . ?
C15 C1 C2 C11 -178.38(9) . . . . ?
C15 C1 C14 C13 178.53(9) . . . . ?
C17 C5 C6 C7 179.44(10) . . . . ?
C19 C20 C21 C3 -98.35(10) . . . . ?
C19 C20 C21 C22 138.21(9) . . . . ?
C19 C20 C29 C28 177.25(8) . . . . ?
C19 C20 C29 C30 -2.30(14) . . . . ?
C20 C19 C32 C31 0.92(15) . . . . ?
C20 C21 C22 C23 -136.52(9) . . . . ?
C20 C21 C22 C27 43.82(11) . . . . ?
C20 C29 C30 C31 2.45(14) . . . . ?
C21 C3 C4 C5 -100.80(10) . . . . ?
C21 C3 C4 C9 78.87(10) . . . . ?
C21 C20 C29 C28 -0.43(12) . . . . ?
C21 C20 C29 C30 -179.98(8) . . . . ?
C21 C22 C23 C24 179.78(8) . . . . ?
C21 C22 C23 C35 -0.83(14) . . . . ?
C21 C22 C27 C26 -179.75(9) . . . . ?
C21 C22 C27 C28 1.57(12) . . . . ?
C22 C23 C24 C25 0.12(14) . . . . ?
C22 C27 C28 C10 77.78(10) . . . . ?
C22 C27 C28 C29 -46.19(11) . . . . ?
C23 C22 C27 C26 0.57(14) . . . . ?
C23 C22 C27 C28 -178.11(8) . . . . ?
C23 C24 C25 C26 0.33(15) . . . . ?
C24 C25 C26 C27 -0.33(15) . . . . ?
C25 C26 C27 C22 -0.12(15) . . . . ?
C25 C26 C27 C28 178.48(9) . . . . ?
C26 C27 C28 C10 -100.88(10) . . . . ?
C26 C27 C28 C29 135.15(10) . . . . ?
C27 C22 C23 C24 -0.56(14) . . . . ?
C27 C22 C23 C35 178.83(9) . . . . ?
C27 C28 C29 C20 45.81(11) . . . . ?
C27 C28 C29 C30 -134.65(9) . . . . ?
C28 C10 C11 C2 78.47(10) . . . . ?
C28 C10 C11 C12 -101.65(10) . . . . ?
C28 C29 C30 C31 -177.08(9) . . . . ?
C29 C20 C21 C3 79.24(10) . . . . ?
C29 C20 C21 C22 -44.20(11) . . . . ?
C29 C30 C31 C32 -0.89(15) . . . . ?
C30 C31 C32 C19 -0.80(15) . . . . ?
C32 C19 C20 C21 178.15(9) . . . . ?
C32 C19 C20 C29 0.63(14) . . . . ?
C33 C19 C20 C21 -0.42(14) . . . . ?
C33 C19 C20 C29 -177.94(9) . . . . ?
C33 C19 C32 C31 179.52(9) . . . . ?
C35 C23 C24 C25 -179.28(9) . . . . ?

_olex2_date_sample_data_collection 2016-11-16
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C3(H3), C10(H10), C21(H21), C28(H28)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14), C24(H24), C25(H25),
 C26(H26), C30(H30), C31(H31), C32(H32)
2.c :
 C16(H16), C18(H18), C34(H34), C36(H36)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.435
_oxdiff_exptl_absorpt_empirical_full_min 0.769
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_SHELXL_version_number     2016/4
_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.
;
####################################################################### 
# 
# 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_10
_database_code_depnum_ccdc_archive 'CCDC 1952352'
loop_
_audit_author_name
_audit_author_address
'Hans Georg Stammler'
;University of Bielefeld
Germany
;
_audit_update_record             
;
2019-09-09 deposited with the CCDC.	2021-05-06 downloaded from the CCDC.
;
# measured as niermeier94
_audit_creation_date             2019-04-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C84 H68 B4 N4, 3.5(C6 H6)'
_chemical_formula_sum            'C105 H89 B4 N4'
_chemical_formula_weight         1450.04
_chemical_melting_point          ?
_chemical_oxdiff_formula         C105H77B4N4
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'
B B 0.0090 0.0039 '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                   14.4537(8)
_cell_length_b                   14.7536(6)
_cell_length_c                   20.5177(7)
_cell_angle_alpha                100.327(3)
_cell_angle_beta                 98.165(4)
_cell_angle_gamma                99.886(4)
_cell_volume                     4172.5(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6708
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      74.2750
_cell_measurement_theta_min      3.1050
_shelx_estimated_absorpt_T_max   0.979
_shelx_estimated_absorpt_T_min   0.800
_exptl_absorpt_coefficient_mu    0.496
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.49a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1534
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.0407
0 1 0 0.0292
-1 0 0 0.0290
1 0 0 0.0135
0 0 1 0.1987
0 0 -1 0.2376

_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.043
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
0.0016 -0.9984 -0.0000 0.0698 -0.0465 -0.0683
-0.0016 0.9984 0.0000 -0.0698 0.0465 0.0683
-1.0000 -0.0009 -0.0010 -0.0567 -0.0883 -0.0330
1.0000 0.0009 0.0010 0.0567 0.0883 0.0330
-0.0022 0.0005 0.9990 0.0255 -0.0250 0.0687
0.0022 -0.0005 -0.9990 -0.0255 0.0250 -0.0687

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0986
_diffrn_reflns_av_unetI/netI     0.1398
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28058
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.079
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         3.109
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00 -23.00   1.00    9.50    --  -38.50 -37.00 -60.00   87
  2  ω   -110.00 -18.00   1.00    9.50    --  -38.50 -37.00-150.00   92
  3  ω    -80.00  -4.00   1.00    9.50    --  -38.50 125.00   0.00   76
  4  ω    -49.00 -14.00   1.00    9.50    --  -38.50 125.00  90.00   35
  5  ω     45.00  89.00   1.00    9.50    --   42.89-125.00 -90.00   44
  6  ω     76.00 105.00   1.00   38.00    --  106.24 -94.00  30.00   29
  7  ω     45.00  71.00   1.00   38.00    --  106.24 -94.00  30.00   26
  8  ω    132.00 178.00   1.00   38.00    --  106.24  77.00-150.00   46
  9  ω     49.00 129.00   1.00   38.00    --  106.24 -77.00  90.00   80
 10  ω     84.00 175.00   1.00   38.00    --  106.24  45.00-180.00   91
 11  ω     33.00 125.00   1.00   38.00    --  106.24 -30.00-120.00   92
 12  ω     43.00 130.00   1.00   38.00    --  106.24 -61.00 -60.00   87
 13  ω     71.00 178.00   1.00   38.00    --  106.24  15.00 -60.00  107
 14  ω     31.00 100.00   1.00   38.00    --  106.24 -94.00 -90.00   69
 15  ω     88.00 117.00   1.00   38.00    --  106.24-125.00   0.00   29
 16  ω     92.00 117.00   1.00   38.00    --  106.24-125.00-180.00   25
 17  ω     85.00 110.00   1.00   38.00    --  106.24 -94.00-180.00   25
 18  ω     37.00  88.00   1.00   38.00    --  106.24 -36.00  57.00   51
 19  ω     76.00 115.00   1.00   38.00    --  106.24  77.00-150.00   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0567453000
_diffrn_orient_matrix_UB_12      -0.0697984000
_diffrn_orient_matrix_UB_13      0.0257126000
_diffrn_orient_matrix_UB_21      0.0882766000
_diffrn_orient_matrix_UB_22      0.0467316000
_diffrn_orient_matrix_UB_23      -0.0248877000
_diffrn_orient_matrix_UB_31      0.0328208000
_diffrn_orient_matrix_UB_32      0.0684925000
_diffrn_orient_matrix_UB_33      0.0688156000
_diffrn_oxdiff_digest_frames     
;
01d2c4b88346423e6e12db857fb812e69a01134b99a
;
_diffrn_oxdiff_digest_hkl        
;
01ad57ced4edd85ec017f6d19d5e468342ee69
;
_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              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9295
_reflns_number_total             14901
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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 1.171.40.49a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.49a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.49a (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         0.316
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1097
_refine_ls_number_reflns         14901
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1035
_refine_ls_R_factor_gt           0.0598
_refine_ls_restrained_S_all      0.931
_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)+(0.0285P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1475
_refine_special_details          
'Hydrogen atoms bondes to nitrogen were refined isotropically, those ones bonded to carbon were taken into account using a riding model. One solvent benzene molecule was disordered in ratio 53:47, both parts were constrained to an idealized hexagon.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Sof(C95A)=Sof(H95A)=Sof(C94A)=Sof(H94A)=Sof(C93A)=Sof(H93A)=Sof(C92A)=
 Sof(H92A)=Sof(C91A)=Sof(H91A)=Sof(C96A)=Sof(H96A)=1-FVAR(1)
 Sof(C95B)=Sof(H95B)=Sof(C94B)=Sof(H94B)=Sof(C93B)=Sof(H93B)=Sof(C92B)=
 Sof(H92B)=Sof(C91B)=Sof(H91B)=Sof(C96B)=Sof(H96B)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C3(H3), C10(H10), C45(H45), C52(H52)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14), C18(H18), C19(H19),
 C20(H20), C21(H21), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28),
  C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
 C40(H40), C41(H41), C42(H42), C48(H48), C49(H49), C50(H50), C54(H54), C55(H55),
  C56(H56), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C66(H66),
 C67(H67), C68(H68), C69(H69), C70(H70), C74(H74), C75(H75), C76(H76), C77(H77),
  C78(H78), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84), C85(H85),
 C86(H86), C87(H87), C88(H88), C89(H89), C90(H90), C95A(H95A), C94A(H94A),
 C93A(H93A), C92A(H92A), C91A(H91A), C96A(H96A), C95B(H95B), C94B(H94B),
 C93B(H93B), C92B(H92B), C91B(H91B), C96B(H96B), C97(H97), C98(H98), C99(H99),
 C100(H100), C101(H101), C102(H102), C103(H103), C104(H104), C105(H105)
3.c Fitted hexagon refined as free rotating group:
 C95A(C94A,C93A,C92A,C91A,C96A), C95B(C94B,C93B,C92B,C91B,C96B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.50335(17) 0.28571(15) 0.70212(12) 0.0266(5) Uani 1 1 d . . . . .
H1A H 0.515(2) 0.345(2) 0.6813(17) 0.032(8) Uiso 1 1 d . . . . .
H1B H 0.450(3) 0.290(2) 0.7285(19) 0.042(9) Uiso 1 1 d . . . . .
H1C H 0.479(3) 0.232(3) 0.664(2) 0.054(11) Uiso 1 1 d . . . . .
N2 N 0.34823(16) 0.59583(15) 1.02193(11) 0.0228(4) Uani 1 1 d . . . . .
H2A H 0.410(3) 0.599(2) 1.0422(17) 0.030(8) Uiso 1 1 d . . . . .
H2B H 0.335(3) 0.663(3) 1.031(2) 0.056(11) Uiso 1 1 d . . . . .
H2C H 0.303(3) 0.561(3) 1.044(2) 0.054(11) Uiso 1 1 d . . . . .
N3 N 0.40275(16) 0.53781(14) 0.57002(12) 0.0213(4) Uani 1 1 d . . . . .
H3A H 0.336(3) 0.529(2) 0.5464(19) 0.041(9) Uiso 1 1 d . . . . .
H3B H 0.407(3) 0.586(3) 0.609(2) 0.044(10) Uiso 1 1 d . . . . .
H3C H 0.442(3) 0.558(3) 0.540(2) 0.055(11) Uiso 1 1 d . . . . .
N4 N 0.27484(16) 0.62288(15) 0.76711(11) 0.0219(4) Uani 1 1 d . . . . .
H4A H 0.314(3) 0.649(2) 0.8083(19) 0.035(9) Uiso 1 1 d . . . . .
H4B H 0.293(3) 0.561(3) 0.7522(18) 0.039(9) Uiso 1 1 d . . . . .
H4C H 0.209(3) 0.607(3) 0.777(2) 0.054(11) Uiso 1 1 d . . . . .
C1 C 0.74740(17) 0.53830(16) 0.87164(12) 0.0187(5) Uani 1 1 d . . . . .
C2 C 0.73959(16) 0.63183(15) 0.87492(12) 0.0159(5) Uani 1 1 d . . . . .
C3 C 0.64921(16) 0.66382(14) 0.84861(12) 0.0157(5) Uani 1 1 d . . . . .
H3 H 0.592906 0.613201 0.847444 0.019 Uiso 1 1 calc R . . . .
C4 C 0.64153(16) 0.75161(15) 0.89692(12) 0.0164(5) Uani 1 1 d . . . . .
C5 C 0.55876(17) 0.76566(15) 0.92149(11) 0.0169(5) Uani 1 1 d . . . . .
C6 C 0.55752(18) 0.85300(16) 0.96215(13) 0.0222(5) Uani 1 1 d . . . . .
H6 H 0.500993 0.863361 0.978312 0.027 Uiso 1 1 calc R . . . .
C7 C 0.63861(19) 0.92386(16) 0.97864(13) 0.0246(5) Uani 1 1 d . . . . .
H7 H 0.637206 0.983034 1.005464 0.029 Uiso 1 1 calc R . . . .
C8 C 0.72190(18) 0.90862(16) 0.95607(13) 0.0229(5) Uani 1 1 d . . . . .
H8 H 0.777663 0.956970 0.968533 0.027 Uiso 1 1 calc R . . . .
C9 C 0.72436(17) 0.82328(15) 0.91544(12) 0.0180(5) Uani 1 1 d . . . . .
C10 C 0.81448(17) 0.79983(15) 0.89406(12) 0.0192(5) Uani 1 1 d . . . . .
H10 H 0.869951 0.845020 0.924350 0.023 Uiso 1 1 calc R . . . .
C11 C 0.82075(17) 0.70275(16) 0.90419(12) 0.0190(5) Uani 1 1 d . . . . .
C12 C 0.90180(18) 0.68132(17) 0.93811(13) 0.0228(5) Uani 1 1 d . . . . .
H12 H 0.954531 0.730387 0.959889 0.027 Uiso 1 1 calc R . . . .
C13 C 0.90618(18) 0.58882(19) 0.94035(14) 0.0277(6) Uani 1 1 d . . . . .
H13 H 0.960282 0.574563 0.965482 0.033 Uiso 1 1 calc R . . . .
C14 C 0.83124(18) 0.51757(17) 0.90574(13) 0.0226(5) Uani 1 1 d . . . . .
H14 H 0.835831 0.453889 0.904726 0.027 Uiso 1 1 calc R . . . .
C15 C 0.67857(17) 0.45833(16) 0.83135(13) 0.0205(5) Uani 1 1 d . . . . .
C16 C 0.63921(18) 0.38299(16) 0.79602(13) 0.0213(5) Uani 1 1 d . . . . .
C17 C 0.5787(2) 0.20295(16) 0.79435(13) 0.0248(5) Uani 1 1 d . . . . .
C18 C 0.4942(2) 0.13542(18) 0.78018(16) 0.0321(6) Uani 1 1 d . . . . .
H18 H 0.448041 0.133859 0.741857 0.039 Uiso 1 1 calc R . . . .
C19 C 0.4752(3) 0.07024(19) 0.82040(18) 0.0421(8) Uani 1 1 d . . . . .
H19 H 0.416559 0.025793 0.809935 0.050 Uiso 1 1 calc R . . . .
C20 C 0.5423(3) 0.0706(2) 0.87556(18) 0.0490(9) Uani 1 1 d . . . . .
H20 H 0.529979 0.026240 0.903156 0.059 Uiso 1 1 calc R . . . .
C21 C 0.6269(3) 0.1353(2) 0.89049(16) 0.0436(8) Uani 1 1 d . . . . .
H21 H 0.672967 0.135437 0.928463 0.052 Uiso 1 1 calc R . . . .
C22 C 0.6456(2) 0.20112(19) 0.85002(15) 0.0330(6) Uani 1 1 d . . . . .
H22 H 0.704602 0.245059 0.860677 0.040 Uiso 1 1 calc R . . . .
C23 C 0.6746(2) 0.25548(17) 0.69926(13) 0.0268(6) Uani 1 1 d . . . . .
C24 C 0.7583(2) 0.3168(2) 0.69573(16) 0.0348(6) Uani 1 1 d . . . . .
H24 H 0.774277 0.377255 0.724679 0.042 Uiso 1 1 calc R . . . .
C25 C 0.8187(3) 0.2930(2) 0.65194(19) 0.0472(8) Uani 1 1 d . . . . .
H25 H 0.874910 0.336678 0.651276 0.057 Uiso 1 1 calc R . . . .
C26 C 0.7971(3) 0.2052(3) 0.60886(18) 0.0497(9) Uani 1 1 d . . . . .
H26 H 0.838244 0.188491 0.578530 0.060 Uiso 1 1 calc R . . . .
C27 C 0.7155(3) 0.1429(2) 0.61059(16) 0.0445(8) Uani 1 1 d . . . . .
H27 H 0.700029 0.082920 0.580983 0.053 Uiso 1 1 calc R . . . .
C28 C 0.6552(2) 0.1669(2) 0.65548(15) 0.0344(7) Uani 1 1 d . . . . .
H28 H 0.599862 0.122273 0.656453 0.041 Uiso 1 1 calc R . . . .
C29 C 0.47787(17) 0.69045(15) 0.91406(12) 0.0176(5) Uani 1 1 d . . . . .
C30 C 0.41292(17) 0.62937(16) 0.91941(12) 0.0184(5) Uani 1 1 d . . . . .
C31 C 0.35514(17) 0.45260(16) 0.92987(12) 0.0185(5) Uani 1 1 d . . . . .
C32 C 0.29995(18) 0.38155(16) 0.95431(12) 0.0206(5) Uani 1 1 d . . . . .
H32 H 0.252575 0.397321 0.979516 0.025 Uiso 1 1 calc R . . . .
C33 C 0.31317(19) 0.28927(17) 0.94243(13) 0.0257(6) Uani 1 1 d . . . . .
H33 H 0.275397 0.243213 0.959844 0.031 Uiso 1 1 calc R . . . .
C34 C 0.3812(2) 0.26415(17) 0.90531(14) 0.0271(6) Uani 1 1 d . . . . .
H34 H 0.389395 0.200843 0.896459 0.033 Uiso 1 1 calc R . . . .
C35 C 0.43742(18) 0.33255(18) 0.88111(13) 0.0250(5) Uani 1 1 d . . . . .
H35 H 0.484348 0.316066 0.855708 0.030 Uiso 1 1 calc R . . . .
C36 C 0.42478(17) 0.42565(17) 0.89423(13) 0.0217(5) Uani 1 1 d . . . . .
H36 H 0.464795 0.471870 0.878388 0.026 Uiso 1 1 calc R . . . .
C37 C 0.22844(17) 0.56499(16) 0.90715(12) 0.0194(5) Uani 1 1 d . . . . .
C38 C 0.16245(17) 0.48716(18) 0.86711(13) 0.0229(5) Uani 1 1 d . . . . .
H38 H 0.177048 0.426298 0.863783 0.028 Uiso 1 1 calc R . . . .
C39 C 0.07559(19) 0.4969(2) 0.83192(15) 0.0315(6) Uani 1 1 d . . . . .
H39 H 0.032117 0.443008 0.805153 0.038 Uiso 1 1 calc R . . . .
C40 C 0.0529(2) 0.5850(2) 0.83608(16) 0.0372(7) Uani 1 1 d . . . . .
H40 H -0.005569 0.591716 0.811687 0.045 Uiso 1 1 calc R . . . .
C41 C 0.1159(2) 0.6631(2) 0.87593(17) 0.0358(7) Uani 1 1 d . . . . .
H41 H 0.100351 0.723625 0.879498 0.043 Uiso 1 1 calc R . . . .
C42 C 0.20264(19) 0.65271(18) 0.91094(14) 0.0260(6) Uani 1 1 d . . . . .
H42 H 0.245274 0.706862 0.938111 0.031 Uiso 1 1 calc R . . . .
C43 C 0.71398(16) 0.57499(15) 0.69422(12) 0.0163(5) Uani 1 1 d . . . . .
C44 C 0.72655(16) 0.65598(15) 0.74485(12) 0.0153(5) Uani 1 1 d . . . . .
C45 C 0.64560(15) 0.68689(14) 0.77456(11) 0.0147(4) Uani 1 1 d . . . . .
H45 H 0.584479 0.650017 0.745564 0.018 Uiso 1 1 calc R . . . .
C46 C 0.65202(16) 0.79000(15) 0.77149(11) 0.0151(4) Uani 1 1 d . . . . .
C47 C 0.57308(16) 0.82631(15) 0.74808(11) 0.0158(5) Uani 1 1 d . . . . .
C48 C 0.58761(18) 0.91990(16) 0.73995(12) 0.0204(5) Uani 1 1 d . . . . .
H48 H 0.534573 0.944737 0.723559 0.024 Uiso 1 1 calc R . . . .
C49 C 0.67778(18) 0.97652(16) 0.75539(13) 0.0222(5) Uani 1 1 d . . . . .
H49 H 0.686515 1.039269 0.748685 0.027 Uiso 1 1 calc R . . . .
C50 C 0.75625(18) 0.94136(16) 0.78093(13) 0.0205(5) Uani 1 1 d . . . . .
H50 H 0.818125 0.980455 0.792817 0.025 Uiso 1 1 calc R . . . .
C51 C 0.74267(17) 0.84934(15) 0.78861(12) 0.0172(5) Uani 1 1 d . . . . .
C52 C 0.82286(16) 0.80630(15) 0.81723(12) 0.0183(5) Uani 1 1 d . . . . .
H52 H 0.884808 0.848906 0.817587 0.022 Uiso 1 1 calc R . . . .
C53 C 0.81751(16) 0.71361(15) 0.76887(12) 0.0175(5) Uani 1 1 d . . . . .
C54 C 0.89521(17) 0.68942(16) 0.74293(13) 0.0219(5) Uani 1 1 d . . . . .
H54 H 0.956751 0.728384 0.758740 0.026 Uiso 1 1 calc R . . . .
C55 C 0.88327(18) 0.60740(18) 0.69328(14) 0.0257(6) Uani 1 1 d . . . . .
H55 H 0.937085 0.590364 0.676288 0.031 Uiso 1 1 calc R . . . .
C56 C 0.79402(18) 0.55138(17) 0.66899(13) 0.0218(5) Uani 1 1 d . . . . .
H56 H 0.786598 0.496421 0.634959 0.026 Uiso 1 1 calc R . . . .
C57 C 0.61927(18) 0.52258(15) 0.66600(12) 0.0191(5) Uani 1 1 d . . . . .
C58 C 0.53664(17) 0.48769(15) 0.64024(12) 0.0187(5) Uani 1 1 d . . . . .
C59 C 0.44614(17) 0.37069(15) 0.53012(12) 0.0178(5) Uani 1 1 d . . . . .
C60 C 0.38526(18) 0.34926(17) 0.46819(13) 0.0226(5) Uani 1 1 d . . . . .
H60 H 0.336545 0.384182 0.461515 0.027 Uiso 1 1 calc R . . . .
C61 C 0.3930(2) 0.27850(17) 0.41559(13) 0.0269(6) Uani 1 1 d . . . . .
H61 H 0.350437 0.266026 0.373795 0.032 Uiso 1 1 calc R . . . .
C62 C 0.4636(2) 0.22607(17) 0.42459(13) 0.0275(6) Uani 1 1 d . . . . .
H62 H 0.468124 0.176405 0.389393 0.033 Uiso 1 1 calc R . . . .
C63 C 0.5270(2) 0.24650(17) 0.48475(13) 0.0256(5) Uani 1 1 d . . . . .
H63 H 0.576102 0.211836 0.490714 0.031 Uiso 1 1 calc R . . . .
C64 C 0.51884(18) 0.31787(15) 0.53662(12) 0.0197(5) Uani 1 1 d . . . . .
H64 H 0.563309 0.331655 0.577622 0.024 Uiso 1 1 calc R . . . .
C65 C 0.35185(17) 0.40494(15) 0.63298(12) 0.0181(5) Uani 1 1 d . . . . .
C66 C 0.26554(19) 0.34697(17) 0.59702(14) 0.0245(5) Uani 1 1 d . . . . .
H66 H 0.257375 0.330545 0.549330 0.029 Uiso 1 1 calc R . . . .
C67 C 0.1917(2) 0.31269(19) 0.62827(15) 0.0309(6) Uani 1 1 d . . . . .
H67 H 0.134422 0.273973 0.601950 0.037 Uiso 1 1 calc R . . . .
C68 C 0.2014(2) 0.33489(18) 0.69772(15) 0.0294(6) Uani 1 1 d . . . . .
H68 H 0.150987 0.312011 0.719350 0.035 Uiso 1 1 calc R . . . .
C69 C 0.2860(2) 0.39117(18) 0.73534(13) 0.0270(6) Uani 1 1 d . . . . .
H69 H 0.294177 0.405469 0.783080 0.032 Uiso 1 1 calc R . . . .
C70 C 0.35933(18) 0.42699(16) 0.70312(13) 0.0213(5) Uani 1 1 d . . . . .
H70 H 0.415581 0.467276 0.729612 0.026 Uiso 1 1 calc R . . . .
C71 C 0.47771(17) 0.77158(16) 0.73310(12) 0.0177(5) Uani 1 1 d . . . . .
C72 C 0.39377(17) 0.73371(16) 0.72213(12) 0.0191(5) Uani 1 1 d . . . . .
C73 C 0.23081(16) 0.64153(16) 0.64185(12) 0.0187(5) Uani 1 1 d . . . . .
C74 C 0.16568(19) 0.55609(18) 0.62720(14) 0.0275(6) Uani 1 1 d . . . . .
H74 H 0.150241 0.527475 0.663279 0.033 Uiso 1 1 calc R . . . .
C75 C 0.1222(2) 0.5109(2) 0.56135(16) 0.0359(7) Uani 1 1 d . . . . .
H75 H 0.078303 0.452509 0.553206 0.043 Uiso 1 1 calc R . . . .
C76 C 0.1433(2) 0.5515(2) 0.50829(15) 0.0337(6) Uani 1 1 d . . . . .
H76 H 0.114317 0.521280 0.463374 0.040 Uiso 1 1 calc R . . . .
C77 C 0.2073(2) 0.63716(19) 0.52115(14) 0.0298(6) Uani 1 1 d . . . . .
H77 H 0.221856 0.665741 0.484867 0.036 Uiso 1 1 calc R . . . .
C78 C 0.24994(19) 0.68083(17) 0.58627(13) 0.0238(5) Uani 1 1 d . . . . .
H78 H 0.293577 0.739267 0.593899 0.029 Uiso 1 1 calc R . . . .
C79 C 0.23438(16) 0.78262(15) 0.74745(12) 0.0180(5) Uani 1 1 d . . . . .
C80 C 0.14749(18) 0.79717(17) 0.71595(14) 0.0229(5) Uani 1 1 d . . . . .
H80 H 0.114915 0.754641 0.675593 0.027 Uiso 1 1 calc R . . . .
C81 C 0.10705(19) 0.87205(18) 0.74180(15) 0.0290(6) Uani 1 1 d . . . . .
H81 H 0.048539 0.880841 0.718700 0.035 Uiso 1 1 calc R . . . .
C82 C 0.1524(2) 0.93328(19) 0.80108(16) 0.0325(6) Uani 1 1 d . . . . .
H82 H 0.124744 0.983959 0.819228 0.039 Uiso 1 1 calc R . . . .
C83 C 0.2380(2) 0.9209(2) 0.83403(16) 0.0357(7) Uani 1 1 d . . . . .
H83 H 0.269350 0.963064 0.874855 0.043 Uiso 1 1 calc R . . . .
C84 C 0.2784(2) 0.84658(19) 0.80742(14) 0.0290(6) Uani 1 1 d . . . . .
H84 H 0.337421 0.838984 0.830541 0.035 Uiso 1 1 calc R . . . .
B1 B 0.6017(2) 0.28117(18) 0.74921(15) 0.0222(6) Uani 1 1 d . . . . .
B2 B 0.33467(19) 0.55695(18) 0.94048(13) 0.0174(5) Uani 1 1 d . . . . .
B3 B 0.43497(19) 0.44661(17) 0.59453(13) 0.0172(5) Uani 1 1 d . . . . .
B4 B 0.28305(19) 0.69664(18) 0.71681(14) 0.0186(5) Uani 1 1 d . . . . .
C85 C 0.9016(3) 0.1840(3) 0.7914(3) 0.0611(12) Uani 1 1 d . . . . .
H85 H 0.835379 0.184364 0.782644 0.073 Uiso 1 1 calc R . . . .
C86 C 0.9418(3) 0.1306(3) 0.7458(2) 0.0575(11) Uani 1 1 d . . . . .
H86 H 0.902891 0.093184 0.705452 0.069 Uiso 1 1 calc R . . . .
C87 C 1.0383(3) 0.1307(3) 0.7580(2) 0.0510(9) Uani 1 1 d . . . . .
H87 H 1.065832 0.093608 0.726315 0.061 Uiso 1 1 calc R . . . .
C88 C 1.0945(2) 0.1852(2) 0.81683(19) 0.0463(9) Uani 1 1 d . . . . .
H88 H 1.161072 0.186075 0.825194 0.056 Uiso 1 1 calc R . . . .
C89 C 1.0550(3) 0.2381(2) 0.8631(2) 0.0475(9) Uani 1 1 d . . . . .
H89 H 1.093769 0.274878 0.903683 0.057 Uiso 1 1 calc R . . . .
C90 C 0.9588(3) 0.2375(2) 0.8504(2) 0.0572(11) Uani 1 1 d . . . . .
H90 H 0.931293 0.274201 0.882422 0.069 Uiso 1 1 calc R . . . .
C95A C 0.8713(9) 0.7874(12) 0.5908(7) 0.055(4) Uani 0.52(3) 1 d . . P A 2
H95A H 0.823411 0.748058 0.606103 0.067 Uiso 0.52(3) 1 calc R . P A 2
C94A C 0.9470(14) 0.7519(6) 0.5687(6) 0.055(4) Uani 0.52(3) 1 d G . P A 2
H94A H 0.950950 0.688346 0.568831 0.066 Uiso 0.52(3) 1 calc R . P A 2
C93A C 1.0170(12) 0.8095(14) 0.5463(8) 0.056(4) Uani 0.52(3) 1 d G . P A 2
H93A H 1.068800 0.785244 0.531180 0.068 Uiso 0.52(3) 1 calc R . P A 2
C92A C 1.0113(10) 0.9025(13) 0.5461(10) 0.066(4) Uani 0.52(3) 1 d G . P A 2
H92A H 1.059113 0.941853 0.530800 0.080 Uiso 0.52(3) 1 calc R . P A 2
C91A C 0.9355(13) 0.9380(6) 0.5682(9) 0.097(7) Uani 0.52(3) 1 d G . P A 2
H91A H 0.931575 1.001566 0.568071 0.116 Uiso 0.52(3) 1 calc R . P A 2
C96A C 0.8655(10) 0.8804(14) 0.5906(7) 0.082(5) Uani 0.52(3) 1 d G . P A 2
H96A H 0.813723 0.904670 0.605723 0.098 Uiso 0.52(3) 1 calc R . P A 2
C95B C 0.8621(6) 0.8471(15) 0.5820(8) 0.059(4) Uani 0.48(3) 1 d . . P A 1
H95B H 0.799817 0.849295 0.591247 0.071 Uiso 0.48(3) 1 calc R . P A 1
C94B C 0.8923(13) 0.7619(10) 0.5726(11) 0.060(5) Uani 0.48(3) 1 d G . P A 1
H94B H 0.850730 0.705951 0.575421 0.072 Uiso 0.48(3) 1 calc R . P A 1
C93B C 0.9834(16) 0.7587(6) 0.5591(9) 0.059(5) Uani 0.48(3) 1 d G . P A 1
H93B H 1.004048 0.700458 0.552720 0.071 Uiso 0.48(3) 1 calc R . P A 1
C92B C 1.0442(11) 0.8405(13) 0.5551(7) 0.058(4) Uani 0.48(3) 1 d G . P A 1
H92B H 1.106455 0.838309 0.545846 0.070 Uiso 0.48(3) 1 calc R . P A 1
C91B C 1.0140(8) 0.9257(8) 0.5645(9) 0.055(4) Uani 0.48(3) 1 d G . P A 1
H91B H 1.055544 0.981654 0.561671 0.066 Uiso 0.48(3) 1 calc R . P A 1
C96B C 0.9229(9) 0.9290(8) 0.5779(7) 0.049(4) Uani 0.48(3) 1 d G . P A 1
H96B H 0.902225 0.987149 0.584372 0.059 Uiso 0.48(3) 1 calc R . P A 1
C97 C 0.3314(3) 0.1099(2) 0.5729(2) 0.0590(11) Uani 1 1 d . . . . .
H97 H 0.324423 0.160291 0.550782 0.071 Uiso 1 1 calc R . . . .
C98 C 0.4034(3) 0.0622(2) 0.56345(18) 0.0485(9) Uani 1 1 d . . . . .
H98 H 0.447576 0.080823 0.535824 0.058 Uiso 1 1 calc R . . . .
C99 C 0.4119(3) -0.0127(2) 0.59399(19) 0.0478(9) Uani 1 1 d . . . . .
H99 H 0.462193 -0.045303 0.587569 0.057 Uiso 1 1 calc R . . . .
C100 C 0.3482(3) -0.0401(2) 0.63346(19) 0.0523(10) Uani 1 1 d . . . . .
H100 H 0.353869 -0.092541 0.653553 0.063 Uiso 1 1 calc R . . . .
C101 C 0.2762(3) 0.0074(3) 0.6444(3) 0.0731(13) Uani 1 1 d . . . . .
H101 H 0.232087 -0.012028 0.671817 0.088 Uiso 1 1 calc R . . . .
C102 C 0.2685(3) 0.0843(3) 0.6148(3) 0.0812(17) Uani 1 1 d . . . . .
H102 H 0.220439 0.119144 0.623248 0.097 Uiso 1 1 calc R . . . .
C103 C 0.9503(2) 0.0480(2) 1.04318(17) 0.0429(8) Uani 1 1 d . . . . .
H103 H 0.916290 0.081020 1.072496 0.052 Uiso 1 1 calc R . . . .
C104 C 0.9568(2) 0.0697(2) 0.98006(18) 0.0453(8) Uani 1 1 d . . . . .
H104 H 0.927051 0.117570 0.966494 0.054 Uiso 1 1 calc R . . . .
C105 C 1.0062(2) 0.0217(2) 0.93750(17) 0.0441(8) Uani 1 1 d . . . . .
H105 H 1.010397 0.036646 0.894726 0.053 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 H1A 1.03(3) . ?
N1 H1B 1.00(4) . ?
N1 H1C 0.98(4) . ?
N1 B1 1.620(3) . ?
N2 H2A 0.93(4) . ?
N2 H2B 1.04(4) . ?
N2 H2C 0.97(5) . ?
N2 B2 1.639(3) . ?
N3 H3A 0.99(4) . ?
N3 H3B 0.96(4) . ?
N3 H3C 0.95(5) . ?
N3 B3 1.635(3) . ?
N4 H4A 0.93(4) . ?
N4 H4B 1.00(4) . ?
N4 H4C 1.00(5) . ?
N4 B4 1.630(3) . ?
C1 C2 1.394(3) . ?
C1 C14 1.419(3) . ?
C1 C15 1.442(4) . ?
C2 C3 1.524(3) . ?
C2 C11 1.409(3) . ?
C3 H3 1.0000 . ?
C3 C4 1.514(3) . ?
C3 C45 1.611(3) . ?
C4 C5 1.395(4) . ?
C4 C9 1.410(3) . ?
C5 C6 1.408(3) . ?
C5 C29 1.437(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.386(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.389(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.389(4) . ?
C9 C10 1.507(4) . ?
C10 H10 1.0000 . ?
C10 C11 1.500(3) . ?
C10 C52 1.616(3) . ?
C11 C12 1.390(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.386(4) . ?
C13 H13 0.9500 . ?
C13 C14 1.380(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.209(4) . ?
C16 B1 1.590(4) . ?
C17 C18 1.395(4) . ?
C17 C22 1.395(4) . ?
C17 B1 1.624(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.392(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.380(6) . ?
C20 H20 0.9500 . ?
C20 C21 1.373(6) . ?
C21 H21 0.9500 . ?
C21 C22 1.403(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.400(4) . ?
C23 C28 1.406(4) . ?
C23 B1 1.616(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.380(5) . ?
C25 H25 0.9500 . ?
C25 C26 1.389(5) . ?
C26 H26 0.9500 . ?
C26 C27 1.374(6) . ?
C27 H27 0.9500 . ?
C27 C28 1.396(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.216(4) . ?
C30 B2 1.580(4) . ?
C31 C32 1.415(3) . ?
C31 C36 1.396(4) . ?
C31 B2 1.600(3) . ?
C32 H32 0.9500 . ?
C32 C33 1.390(3) . ?
C33 H33 0.9500 . ?
C33 C34 1.386(4) . ?
C34 H34 0.9500 . ?
C34 C35 1.392(4) . ?
C35 H35 0.9500 . ?
C35 C36 1.400(4) . ?
C36 H36 0.9500 . ?
C37 C38 1.402(4) . ?
C37 C42 1.399(3) . ?
C37 B2 1.622(3) . ?
C38 H38 0.9500 . ?
C38 C39 1.400(4) . ?
C39 H39 0.9500 . ?
C39 C40 1.384(4) . ?
C40 H40 0.9500 . ?
C40 C41 1.385(5) . ?
C41 H41 0.9500 . ?
C41 C42 1.400(4) . ?
C42 H42 0.9500 . ?
C43 C44 1.402(3) . ?
C43 C56 1.404(4) . ?
C43 C57 1.435(3) . ?
C44 C45 1.495(3) . ?
C44 C53 1.406(3) . ?
C45 H45 1.0000 . ?
C45 C46 1.521(3) . ?
C46 C47 1.402(3) . ?
C46 C51 1.404(3) . ?
C47 C48 1.404(3) . ?
C47 C71 1.434(4) . ?
C48 H48 0.9500 . ?
C48 C49 1.382(4) . ?
C49 H49 0.9500 . ?
C49 C50 1.400(3) . ?
C50 H50 0.9500 . ?
C50 C51 1.379(3) . ?
C51 C52 1.511(3) . ?
C52 H52 1.0000 . ?
C52 C53 1.522(3) . ?
C53 C54 1.382(4) . ?
C54 H54 0.9500 . ?
C54 C55 1.403(4) . ?
C55 H55 0.9500 . ?
C55 C56 1.378(4) . ?
C56 H56 0.9500 . ?
C57 C58 1.218(4) . ?
C58 B3 1.583(3) . ?
C59 C60 1.390(3) . ?
C59 C64 1.417(3) . ?
C59 B3 1.618(4) . ?
C60 H60 0.9500 . ?
C60 C61 1.392(4) . ?
C61 H61 0.9500 . ?
C61 C62 1.394(4) . ?
C62 H62 0.9500 . ?
C62 C63 1.380(4) . ?
C63 H63 0.9500 . ?
C63 C64 1.390(4) . ?
C64 H64 0.9500 . ?
C65 C66 1.406(4) . ?
C65 C70 1.402(4) . ?
C65 B3 1.623(4) . ?
C66 H66 0.9500 . ?
C66 C67 1.390(4) . ?
C67 H67 0.9500 . ?
C67 C68 1.385(4) . ?
C68 H68 0.9500 . ?
C68 C69 1.391(4) . ?
C69 H69 0.9500 . ?
C69 C70 1.404(4) . ?
C70 H70 0.9500 . ?
C71 C72 1.216(4) . ?
C72 B4 1.581(4) . ?
C73 C74 1.394(4) . ?
C73 C78 1.409(4) . ?
C73 B4 1.615(4) . ?
C74 H74 0.9500 . ?
C74 C75 1.399(4) . ?
C75 H75 0.9500 . ?
C75 C76 1.380(5) . ?
C76 H76 0.9500 . ?
C76 C77 1.390(4) . ?
C77 H77 0.9500 . ?
C77 C78 1.379(4) . ?
C78 H78 0.9500 . ?
C79 C80 1.397(3) . ?
C79 C84 1.402(4) . ?
C79 B4 1.626(4) . ?
C80 H80 0.9500 . ?
C80 C81 1.394(4) . ?
C81 H81 0.9500 . ?
C81 C82 1.379(4) . ?
C82 H82 0.9500 . ?
C82 C83 1.381(5) . ?
C83 H83 0.9500 . ?
C83 C84 1.391(4) . ?
C84 H84 0.9500 . ?
C85 H85 0.9500 . ?
C85 C86 1.371(7) . ?
C85 C90 1.386(6) . ?
C86 H86 0.9500 . ?
C86 C87 1.382(6) . ?
C87 H87 0.9500 . ?
C87 C88 1.383(5) . ?
C88 H88 0.9500 . ?
C88 C89 1.370(6) . ?
C89 H89 0.9500 . ?
C89 C90 1.376(6) . ?
C90 H90 0.9500 . ?
C95A H95A 0.9500 . ?
C95A C94A 1.3900 . ?
C95A C96A 1.3900 . ?
C94A H94A 0.9500 . ?
C94A C93A 1.3900 . ?
C93A H93A 0.9500 . ?
C93A C92A 1.3900 . ?
C92A H92A 0.9500 . ?
C92A C91A 1.3900 . ?
C91A H91A 0.9500 . ?
C91A C96A 1.3900 . ?
C96A H96A 0.9500 . ?
C95B H95B 0.9500 . ?
C95B C94B 1.3900 . ?
C95B C96B 1.3900 . ?
C94B H94B 0.9500 . ?
C94B C93B 1.3900 . ?
C93B H93B 0.9500 . ?
C93B C92B 1.3900 . ?
C92B H92B 0.9500 . ?
C92B C91B 1.3900 . ?
C91B H91B 0.9500 . ?
C91B C96B 1.3900 . ?
C96B H96B 0.9500 . ?
C97 H97 0.9500 . ?
C97 C98 1.369(6) . ?
C97 C102 1.388(8) . ?
C98 H98 0.9500 . ?
C98 C99 1.379(5) . ?
C99 H99 0.9500 . ?
C99 C100 1.367(6) . ?
C100 H100 0.9500 . ?
C100 C101 1.373(7) . ?
C101 H101 0.9500 . ?
C101 C102 1.393(7) . ?
C102 H102 0.9500 . ?
C103 H103 0.9500 . ?
C103 C104 1.400(5) . ?
C103 C105 1.380(5) 2_757 ?
C104 H104 0.9500 . ?
C104 C105 1.380(5) . ?
C105 H105 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
H1A N1 H1B 109(3) . . ?
H1A N1 H1C 106(3) . . ?
H1B N1 H1C 107(3) . . ?
B1 N1 H1A 108.3(18) . . ?
B1 N1 H1B 112(2) . . ?
B1 N1 H1C 115(2) . . ?
H2A N2 H2B 108(3) . . ?
H2A N2 H2C 111(3) . . ?
H2B N2 H2C 104(3) . . ?
B2 N2 H2A 110(2) . . ?
B2 N2 H2B 109(2) . . ?
B2 N2 H2C 115(2) . . ?
H3A N3 H3B 104(3) . . ?
H3A N3 H3C 106(3) . . ?
H3B N3 H3C 113(3) . . ?
B3 N3 H3A 117(2) . . ?
B3 N3 H3B 108(2) . . ?
B3 N3 H3C 109(2) . . ?
H4A N4 H4B 105(3) . . ?
H4A N4 H4C 106(3) . . ?
H4B N4 H4C 105(3) . . ?
B4 N4 H4A 110(2) . . ?
B4 N4 H4B 117(2) . . ?
B4 N4 H4C 113(2) . . ?
C2 C1 C14 119.5(2) . . ?
C2 C1 C15 124.7(2) . . ?
C14 C1 C15 115.7(2) . . ?
C1 C2 C3 124.8(2) . . ?
C1 C2 C11 118.3(2) . . ?
C11 C2 C3 116.88(19) . . ?
C2 C3 H3 108.5 . . ?
C2 C3 C45 114.2(2) . . ?
C4 C3 C2 108.64(18) . . ?
C4 C3 H3 108.5 . . ?
C4 C3 C45 108.29(16) . . ?
C45 C3 H3 108.5 . . ?
C5 C4 C3 124.4(2) . . ?
C5 C4 C9 119.8(2) . . ?
C9 C4 C3 115.8(2) . . ?
C4 C5 C6 119.6(2) . . ?
C4 C5 C29 122.2(2) . . ?
C6 C5 C29 117.7(2) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 C5 120.1(2) . . ?
C7 C6 H6 119.9 . . ?
C6 C7 H7 119.9 . . ?
C6 C7 C8 120.2(2) . . ?
C8 C7 H7 119.9 . . ?
C7 C8 H8 119.7 . . ?
C7 C8 C9 120.6(2) . . ?
C9 C8 H8 119.7 . . ?
C4 C9 C10 117.2(2) . . ?
C8 C9 C4 119.7(2) . . ?
C8 C9 C10 122.9(2) . . ?
C9 C10 H10 108.0 . . ?
C9 C10 C52 114.52(18) . . ?
C11 C10 C9 108.5(2) . . ?
C11 C10 H10 108.0 . . ?
C11 C10 C52 109.7(2) . . ?
C52 C10 H10 108.0 . . ?
C2 C11 C10 115.90(19) . . ?
C12 C11 C2 120.8(2) . . ?
C12 C11 C10 123.3(2) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 C11 120.4(2) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 H13 120.3 . . ?
C14 C13 C12 119.4(2) . . ?
C14 C13 H13 120.3 . . ?
C1 C14 H14 119.6 . . ?
C13 C14 C1 120.8(2) . . ?
C13 C14 H14 119.6 . . ?
C16 C15 C1 165.1(3) . . ?
C15 C16 B1 172.2(3) . . ?
C18 C17 B1 123.2(2) . . ?
C22 C17 C18 117.1(3) . . ?
C22 C17 B1 119.8(2) . . ?
C17 C18 H18 118.9 . . ?
C19 C18 C17 122.1(3) . . ?
C19 C18 H18 118.9 . . ?
C18 C19 H19 120.2 . . ?
C20 C19 C18 119.6(3) . . ?
C20 C19 H19 120.2 . . ?
C19 C20 H20 120.1 . . ?
C21 C20 C19 119.9(3) . . ?
C21 C20 H20 120.1 . . ?
C20 C21 H21 119.8 . . ?
C20 C21 C22 120.4(3) . . ?
C22 C21 H21 119.8 . . ?
C17 C22 C21 120.9(3) . . ?
C17 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C24 C23 C28 115.9(3) . . ?
C24 C23 B1 124.2(2) . . ?
C28 C23 B1 119.9(3) . . ?
C23 C24 H24 118.6 . . ?
C25 C24 C23 122.7(3) . . ?
C25 C24 H24 118.6 . . ?
C24 C25 H25 120.0 . . ?
C24 C25 C26 120.0(3) . . ?
C26 C25 H25 120.0 . . ?
C25 C26 H26 120.4 . . ?
C27 C26 C25 119.2(3) . . ?
C27 C26 H26 120.4 . . ?
C26 C27 H27 119.7 . . ?
C26 C27 C28 120.6(3) . . ?
C28 C27 H27 119.7 . . ?
C23 C28 H28 119.2 . . ?
C27 C28 C23 121.5(3) . . ?
C27 C28 H28 119.2 . . ?
C30 C29 C5 169.1(2) . . ?
C29 C30 B2 169.7(2) . . ?
C32 C31 B2 120.9(2) . . ?
C36 C31 C32 116.5(2) . . ?
C36 C31 B2 122.5(2) . . ?
C31 C32 H32 119.1 . . ?
C33 C32 C31 121.8(3) . . ?
C33 C32 H32 119.1 . . ?
C32 C33 H33 119.8 . . ?
C34 C33 C32 120.3(3) . . ?
C34 C33 H33 119.8 . . ?
C33 C34 H34 120.3 . . ?
C33 C34 C35 119.4(2) . . ?
C35 C34 H34 120.3 . . ?
C34 C35 H35 120.0 . . ?
C34 C35 C36 120.0(3) . . ?
C36 C35 H35 120.0 . . ?
C31 C36 C35 122.0(2) . . ?
C31 C36 H36 119.0 . . ?
C35 C36 H36 119.0 . . ?
C38 C37 B2 122.2(2) . . ?
C42 C37 C38 116.7(2) . . ?
C42 C37 B2 120.7(2) . . ?
C37 C38 H38 119.2 . . ?
C39 C38 C37 121.6(2) . . ?
C39 C38 H38 119.2 . . ?
C38 C39 H39 120.0 . . ?
C40 C39 C38 120.1(3) . . ?
C40 C39 H39 120.0 . . ?
C39 C40 H40 120.1 . . ?
C39 C40 C41 119.8(2) . . ?
C41 C40 H40 120.1 . . ?
C40 C41 H41 120.1 . . ?
C40 C41 C42 119.7(3) . . ?
C42 C41 H41 120.1 . . ?
C37 C42 C41 122.0(3) . . ?
C37 C42 H42 119.0 . . ?
C41 C42 H42 119.0 . . ?
C44 C43 C56 118.9(2) . . ?
C44 C43 C57 119.3(2) . . ?
C56 C43 C57 121.6(2) . . ?
C43 C44 C45 122.7(2) . . ?
C43 C44 C53 120.5(2) . . ?
C53 C44 C45 116.8(2) . . ?
C3 C45 H45 108.3 . . ?
C44 C45 C3 109.36(17) . . ?
C44 C45 H45 108.3 . . ?
C44 C45 C46 107.01(18) . . ?
C46 C45 C3 115.49(18) . . ?
C46 C45 H45 108.3 . . ?
C47 C46 C45 123.0(2) . . ?
C47 C46 C51 119.0(2) . . ?
C51 C46 C45 117.80(19) . . ?
C46 C47 C48 119.0(2) . . ?
C46 C47 C71 122.2(2) . . ?
C48 C47 C71 118.8(2) . . ?
C47 C48 H48 119.4 . . ?
C49 C48 C47 121.1(2) . . ?
C49 C48 H48 119.4 . . ?
C48 C49 H49 120.0 . . ?
C48 C49 C50 120.0(2) . . ?
C50 C49 H49 120.0 . . ?
C49 C50 H50 120.4 . . ?
C51 C50 C49 119.2(2) . . ?
C51 C50 H50 120.4 . . ?
C46 C51 C52 115.64(19) . . ?
C50 C51 C46 121.6(2) . . ?
C50 C51 C52 122.7(2) . . ?
C10 C52 H52 108.3 . . ?
C51 C52 C10 108.9(2) . . ?
C51 C52 H52 108.3 . . ?
C51 C52 C53 106.69(19) . . ?
C53 C52 C10 116.15(18) . . ?
C53 C52 H52 108.3 . . ?
C44 C53 C52 117.0(2) . . ?
C54 C53 C44 119.6(2) . . ?
C54 C53 C52 123.0(2) . . ?
C53 C54 H54 120.0 . . ?
C53 C54 C55 120.1(2) . . ?
C55 C54 H54 120.0 . . ?
C54 C55 H55 119.8 . . ?
C56 C55 C54 120.5(2) . . ?
C56 C55 H55 119.8 . . ?
C43 C56 H56 119.8 . . ?
C55 C56 C43 120.4(2) . . ?
C55 C56 H56 119.8 . . ?
C58 C57 C43 172.5(2) . . ?
C57 C58 B3 169.5(3) . . ?
C60 C59 C64 116.3(2) . . ?
C60 C59 B3 124.2(2) . . ?
C64 C59 B3 119.4(2) . . ?
C59 C60 H60 118.8 . . ?
C59 C60 C61 122.4(2) . . ?
C61 C60 H60 118.8 . . ?
C60 C61 H61 120.2 . . ?
C60 C61 C62 119.6(2) . . ?
C62 C61 H61 120.2 . . ?
C61 C62 H62 120.1 . . ?
C63 C62 C61 119.8(2) . . ?
C63 C62 H62 120.1 . . ?
C62 C63 H63 120.1 . . ?
C62 C63 C64 119.9(2) . . ?
C64 C63 H63 120.1 . . ?
C59 C64 H64 119.0 . . ?
C63 C64 C59 121.9(2) . . ?
C63 C64 H64 119.0 . . ?
C66 C65 B3 121.4(2) . . ?
C70 C65 C66 115.8(2) . . ?
C70 C65 B3 122.7(2) . . ?
C65 C66 H66 118.6 . . ?
C67 C66 C65 122.8(3) . . ?
C67 C66 H66 118.6 . . ?
C66 C67 H67 120.0 . . ?
C68 C67 C66 120.1(3) . . ?
C68 C67 H67 120.0 . . ?
C67 C68 H68 120.5 . . ?
C67 C68 C69 119.0(3) . . ?
C69 C68 H68 120.5 . . ?
C68 C69 H69 119.8 . . ?
C68 C69 C70 120.4(2) . . ?
C70 C69 H69 119.8 . . ?
C65 C70 C69 121.8(2) . . ?
C65 C70 H70 119.1 . . ?
C69 C70 H70 119.1 . . ?
C72 C71 C47 173.4(2) . . ?
C71 C72 B4 171.3(3) . . ?
C74 C73 C78 116.1(2) . . ?
C74 C73 B4 124.5(2) . . ?
C78 C73 B4 119.5(2) . . ?
C73 C74 H74 118.8 . . ?
C73 C74 C75 122.4(3) . . ?
C75 C74 H74 118.8 . . ?
C74 C75 H75 120.2 . . ?
C76 C75 C74 119.7(3) . . ?
C76 C75 H75 120.2 . . ?
C75 C76 H76 120.3 . . ?
C75 C76 C77 119.4(3) . . ?
C77 C76 H76 120.3 . . ?
C76 C77 H77 119.8 . . ?
C78 C77 C76 120.4(3) . . ?
C78 C77 H77 119.8 . . ?
C73 C78 H78 119.0 . . ?
C77 C78 C73 122.1(2) . . ?
C77 C78 H78 119.0 . . ?
C80 C79 C84 116.4(2) . . ?
C80 C79 B4 122.4(2) . . ?
C84 C79 B4 121.1(2) . . ?
C79 C80 H80 118.9 . . ?
C81 C80 C79 122.2(2) . . ?
C81 C80 H80 118.9 . . ?
C80 C81 H81 120.2 . . ?
C82 C81 C80 119.7(2) . . ?
C82 C81 H81 120.2 . . ?
C81 C82 H82 120.0 . . ?
C81 C82 C83 119.9(3) . . ?
C83 C82 H82 120.0 . . ?
C82 C83 H83 120.0 . . ?
C82 C83 C84 120.0(3) . . ?
C84 C83 H83 120.0 . . ?
C79 C84 H84 119.1 . . ?
C83 C84 C79 121.8(2) . . ?
C83 C84 H84 119.1 . . ?
N1 B1 C17 108.8(2) . . ?
C16 B1 N1 106.26(18) . . ?
C16 B1 C17 110.6(2) . . ?
C16 B1 C23 111.5(2) . . ?
C23 B1 N1 106.7(2) . . ?
C23 B1 C17 112.66(19) . . ?
C30 B2 N2 102.65(19) . . ?
C30 B2 C31 113.2(2) . . ?
C30 B2 C37 110.55(18) . . ?
C31 B2 N2 106.55(18) . . ?
C31 B2 C37 115.1(2) . . ?
C37 B2 N2 107.7(2) . . ?
C58 B3 N3 104.23(18) . . ?
C58 B3 C59 108.9(2) . . ?
C58 B3 C65 115.5(2) . . ?
C59 B3 N3 109.95(18) . . ?
C59 B3 C65 112.21(19) . . ?
C65 B3 N3 105.65(18) . . ?
C72 B4 N4 105.18(17) . . ?
C72 B4 C73 113.0(2) . . ?
C72 B4 C79 109.64(19) . . ?
C73 B4 N4 108.50(19) . . ?
C73 B4 C79 113.47(18) . . ?
C79 B4 N4 106.5(2) . . ?
C86 C85 H85 120.4 . . ?
C86 C85 C90 119.3(3) . . ?
C90 C85 H85 120.4 . . ?
C85 C86 H86 119.8 . . ?
C85 C86 C87 120.5(4) . . ?
C87 C86 H86 119.8 . . ?
C86 C87 H87 120.2 . . ?
C86 C87 C88 119.5(4) . . ?
C88 C87 H87 120.2 . . ?
C87 C88 H88 119.8 . . ?
C89 C88 C87 120.5(3) . . ?
C89 C88 H88 119.8 . . ?
C88 C89 H89 120.2 . . ?
C88 C89 C90 119.6(4) . . ?
C90 C89 H89 120.2 . . ?
C85 C90 H90 119.7 . . ?
C89 C90 C85 120.7(4) . . ?
C89 C90 H90 119.7 . . ?
C94A C95A H95A 120.0 . . ?
C94A C95A C96A 120.0 . . ?
C96A C95A H95A 120.0 . . ?
C95A C94A H94A 120.0 . . ?
C93A C94A C95A 120.0 . . ?
C93A C94A H94A 120.0 . . ?
C94A C93A H93A 120.0 . . ?
C94A C93A C92A 120.0 . . ?
C92A C93A H93A 120.0 . . ?
C93A C92A H92A 120.0 . . ?
C91A C92A C93A 120.0 . . ?
C91A C92A H92A 120.0 . . ?
C92A C91A H91A 120.0 . . ?
C92A C91A C96A 120.0 . . ?
C96A C91A H91A 120.0 . . ?
C95A C96A H96A 120.0 . . ?
C91A C96A C95A 120.0 . . ?
C91A C96A H96A 120.0 . . ?
C94B C95B H95B 120.0 . . ?
C94B C95B C96B 120.0 . . ?
C96B C95B H95B 120.0 . . ?
C95B C94B H94B 120.0 . . ?
C93B C94B C95B 120.0 . . ?
C93B C94B H94B 120.0 . . ?
C94B C93B H93B 120.0 . . ?
C94B C93B C92B 120.0 . . ?
C92B C93B H93B 120.0 . . ?
C93B C92B H92B 120.0 . . ?
C93B C92B C91B 120.0 . . ?
C91B C92B H92B 120.0 . . ?
C92B C91B H91B 120.0 . . ?
C96B C91B C92B 120.0 . . ?
C96B C91B H91B 120.0 . . ?
C95B C96B H96B 120.0 . . ?
C91B C96B C95B 120.0 . . ?
C91B C96B H96B 120.0 . . ?
C98 C97 H97 120.1 . . ?
C98 C97 C102 119.8(3) . . ?
C102 C97 H97 120.1 . . ?
C97 C98 H98 119.9 . . ?
C97 C98 C99 120.1(4) . . ?
C99 C98 H98 119.9 . . ?
C98 C99 H99 119.9 . . ?
C100 C99 C98 120.2(4) . . ?
C100 C99 H99 119.9 . . ?
C99 C100 H100 119.6 . . ?
C99 C100 C101 120.7(3) . . ?
C101 C100 H100 119.6 . . ?
C100 C101 H101 120.4 . . ?
C100 C101 C102 119.3(5) . . ?
C102 C101 H101 120.4 . . ?
C97 C102 C101 119.8(4) . . ?
C97 C102 H102 120.1 . . ?
C101 C102 H102 120.1 . . ?
C104 C103 H103 120.2 . . ?
C105 C103 H103 120.2 2_757 . ?
C105 C103 C104 119.5(4) 2_757 . ?
C103 C104 H104 119.9 . . ?
C105 C104 C103 120.2(4) . . ?
C105 C104 H104 119.9 . . ?
C103 C105 H105 119.9 2_757 . ?
C104 C105 C103 120.3(3) . 2_757 ?
C104 C105 H105 119.9 . . ?

_olex2_date_sample_data_collection 2019-04-17
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.459
_oxdiff_exptl_absorpt_empirical_full_min 0.452
####################################################################### 
# 
# 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_Syn-6
_database_code_depnum_ccdc_archive 'CCDC 1952349'
loop_
_audit_author_name
_audit_author_address
'Hans Georg Stammler'
;University of Bielefeld
Germany
;
_audit_update_record             
;
2019-09-09 deposited with the CCDC.	2021-05-06 downloaded from the CCDC.
;
# measured as niermeier55
_audit_creation_date             2017-07-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C48 H44 O4, C6 H6'
_chemical_formula_sum            'C54 H50 O4'
_chemical_formula_weight         762.94
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C54 H50 O4'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 1 2/n 1'
_space_group_name_Hall           '-P 2yac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'

_cell_length_a                   11.1578(3)
_cell_length_b                   11.0555(3)
_cell_length_c                   17.2821(4)
_cell_angle_alpha                90
_cell_angle_beta                 98.594(2)
_cell_angle_gamma                90
_cell_volume                     2107.90(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    18441
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.4030
_cell_measurement_theta_min      2.9980
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.620
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.15e (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             812
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 0 0.0283
1 0 0 0.0283
0 0 -1 0.0447
0 0 1 0.0447
0 1 0 0.1610
0 -1 0 0.1610
0 2 5 0.0829
3 -3 5 0.0779

_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.057
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
-0.9984 -0.0007 -0.0011 0.0262 0.0583 -0.0055
0.9984 0.0007 0.0011 -0.0262 -0.0583 0.0055
0.0008 0.0007 -1.0001 -0.0148 0.0099 -0.0375
-0.0008 -0.0007 1.0001 0.0148 -0.0099 0.0375
0.0008 0.9998 0.0002 0.0519 -0.0260 -0.0273
-0.0008 -0.9998 -0.0002 -0.0519 0.0260 0.0273
-0.0023 1.9961 5.0009 0.1776 -0.1014 0.1330
2.9887 -3.0008 5.0032 -0.1605 -0.1465 0.2860

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            47712
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.032
_diffrn_reflns_theta_min         2.608
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -74.00 -24.00   1.00  125.00    --  -18.03 126.00-123.20   50
  2  ω    -88.00   9.00   1.00  125.00    --  -18.03 -57.00-150.00   97
  3  ω    -92.00 -38.00   1.00  125.00    --  -18.03 153.00  -9.19   54
  4  ω      9.00  77.00   1.00  125.00    --   18.42-130.00-128.79   68
  5  ω     -1.00  91.00   1.00  125.00    --   18.42  38.00 120.00   92
  6  ω      2.00  91.00   1.00  125.00    --   18.42  38.00  30.00   89
  7  ω    -13.00  58.00   1.00  125.00    --   18.42  77.00-150.00   71
  8  ω    -46.00  41.00   1.00  125.00    --   18.42 -38.00 -60.00   87
  9  ω     41.00  68.00   1.00  125.00    --   18.42 178.00 -30.00   27
 10  ω    -50.00  45.00   1.00  125.00    --   18.42 -57.00  30.00   95
 11  ω    -50.00  11.00   1.00  125.00    --   18.42 -38.00  90.00   61
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0262738000
_diffrn_orient_matrix_UB_12      0.0519407000
_diffrn_orient_matrix_UB_13      0.0147679000
_diffrn_orient_matrix_UB_21      -0.0584097000
_diffrn_orient_matrix_UB_22      -0.0259421000
_diffrn_orient_matrix_UB_23      -0.0099403000
_diffrn_orient_matrix_UB_31      0.0054950000
_diffrn_orient_matrix_UB_32      -0.0273263000
_diffrn_orient_matrix_UB_33      0.0374970000
_diffrn_oxdiff_ac3_digest_frames 
;
012e1fa854c22c34c6f5709ef7e64d61f900825c67f
;
_diffrn_oxdiff_ac3_digest_hkl    
;
01b88c6da9b7e911185f08e7fcdfcc2cdf552d
;
_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              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5319
_reflns_number_total             6166
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_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 1.171.39.15e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_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         0.472
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         6166
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0477
_refine_ls_restrained_S_all      1.073
_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)+(0.0717P)²+1.0537P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1392
_refine_ls_wR_factor_ref         0.1452
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C3(H3), C10(H10)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14), C25(H25), C26(H26),
 C27(H27), C28(H28)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.68491(9) 0.64126(8) 0.35081(5) 0.01945(18) Uani 1 1 d . . . . .
H1 H 0.647(2) 0.631(2) 0.3122(14) 0.051(6) Uiso 1 1 d . . . . .
O2 O 0.57698(8) 0.64344(8) 0.18909(5) 0.01997(19) Uani 1 1 d . . . . .
H2 H 0.639(2) 0.6373(18) 0.1702(12) 0.036(5) Uiso 1 1 d . . . . .
C1 C 0.66023(10) 0.21470(10) 0.40628(6) 0.0141(2) Uani 1 1 d . . . . .
C2 C 0.67230(9) 0.15312(9) 0.33673(6) 0.01253(19) Uani 1 1 d . . . . .
C3 C 0.68165(9) 0.21659(9) 0.26002(6) 0.01163(19) Uani 1 1 d . . . . .
H3 H 0.655417 0.300665 0.264009 0.014 Uiso 1 1 calc R . . . .
C4 C 0.59402(9) 0.15384(9) 0.19710(6) 0.01233(19) Uani 1 1 d . . . . .
C5 C 0.51207(10) 0.21611(10) 0.14147(6) 0.0140(2) Uani 1 1 d . . . . .
C6 C 0.43555(10) 0.14948(10) 0.08468(7) 0.0180(2) Uani 1 1 d . . . . .
H6 H 0.381378 0.190067 0.047421 0.022 Uiso 1 1 calc R . . . .
C7 C 0.43997(11) 0.02442(11) 0.08362(7) 0.0194(2) Uani 1 1 d . . . . .
H7 H 0.390061 -0.018504 0.045237 0.023 Uiso 1 1 calc R . . . .
C8 C 0.51935(10) -0.03719(10) 0.14018(7) 0.0171(2) Uani 1 1 d . . . . .
H8 H 0.521290 -0.121284 0.140250 0.021 Uiso 1 1 calc R . . . .
C9 C 0.59542(10) 0.02733(9) 0.19633(6) 0.0136(2) Uani 1 1 d . . . . .
C10 C 0.68197(10) -0.03553(9) 0.25948(6) 0.0134(2) Uani 1 1 d . . . . .
H10 H 0.655635 -0.119678 0.262888 0.016 Uiso 1 1 calc R . . . .
C11 C 0.67202(10) 0.02631(9) 0.33631(6) 0.0136(2) Uani 1 1 d . . . . .
C12 C 0.66059(10) -0.03839(10) 0.40382(6) 0.0166(2) Uani 1 1 d . . . . .
H12 H 0.660197 -0.122496 0.402805 0.020 Uiso 1 1 calc R . . . .
C13 C 0.64972(11) 0.02268(11) 0.47304(7) 0.0187(2) Uani 1 1 d . . . . .
H13 H 0.642405 -0.020646 0.518225 0.022 Uiso 1 1 calc R . . . .
C14 C 0.64983(11) 0.14798(10) 0.47439(7) 0.0176(2) Uani 1 1 d . . . . .
H14 H 0.642967 0.188428 0.520706 0.021 Uiso 1 1 calc R . . . .
C15 C 0.65353(10) 0.34448(10) 0.40802(6) 0.0151(2) Uani 1 1 d . . . . .
C16 C 0.64328(10) 0.45265(10) 0.40915(6) 0.0157(2) Uani 1 1 d . . . . .
C17 C 0.62679(10) 0.58533(10) 0.41076(6) 0.0142(2) Uani 1 1 d . . . . .
C18 C 0.68581(13) 0.63565(11) 0.48971(7) 0.0221(2) Uani 1 1 d . . . . .
H18A H 0.771352 0.619859 0.496677 0.033 Uiso 1 1 calc GR . . . .
H18B H 0.650860 0.597377 0.530933 0.033 Uiso 1 1 calc GR . . . .
H18C H 0.672290 0.721327 0.491119 0.033 Uiso 1 1 calc GR . . . .
C19 C 0.49208(11) 0.61618(12) 0.39598(8) 0.0233(2) Uani 1 1 d . . . . .
H19A H 0.482237 0.701945 0.388999 0.035 Uiso 1 1 calc GR . . . .
H19B H 0.454931 0.590805 0.439935 0.035 Uiso 1 1 calc GR . . . .
H19C H 0.454278 0.575228 0.349711 0.035 Uiso 1 1 calc GR . . . .
C20 C 0.50254(10) 0.34587(10) 0.14262(6) 0.0154(2) Uani 1 1 d . . . . .
C21 C 0.49071(10) 0.45386(10) 0.14283(6) 0.0156(2) Uani 1 1 d . . . . .
C22 C 0.47531(10) 0.58703(9) 0.14117(6) 0.0142(2) Uani 1 1 d . . . . .
C23 C 0.36170(11) 0.62288(12) 0.17505(8) 0.0238(3) Uani 1 1 d . . . . .
H23A H 0.366832 0.592073 0.227380 0.036 Uiso 1 1 calc GR . . . .
H23B H 0.291567 0.589669 0.143194 0.036 Uiso 1 1 calc GR . . . .
H23C H 0.355244 0.709441 0.175899 0.036 Uiso 1 1 calc GR . . . .
C24 C 0.46622(12) 0.63332(11) 0.05721(7) 0.0214(2) Uani 1 1 d . . . . .
H24A H 0.455807 0.719532 0.056623 0.032 Uiso 1 1 calc GR . . . .
H24B H 0.398056 0.596271 0.025521 0.032 Uiso 1 1 calc GR . . . .
H24C H 0.539077 0.613259 0.036712 0.032 Uiso 1 1 calc GR . . . .
C25 C 0.250000 0.2907(3) 0.250000 0.0762(12) Uani 1 2 d S T P . .
H25 H 0.249998 0.374775 0.250001 0.091 Uiso 1 2 calc RS T P . .
C26 C 0.33670(19) 0.2300(3) 0.29675(14) 0.0693(8) Uani 1 1 d . . . . .
H26 H 0.396304 0.273378 0.328556 0.083 Uiso 1 1 calc R . . . .
C27 C 0.3398(2) 0.1093(3) 0.29887(15) 0.0719(9) Uani 1 1 d . . . . .
H27 H 0.399987 0.068643 0.331952 0.086 Uiso 1 1 calc R . . . .
C28 C 0.250000 0.0453(3) 0.250000 0.0979(18) Uani 1 2 d S T P . .
H28 H 0.249999 -0.038815 0.250001 0.117 Uiso 1 2 calc RS T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 H1 0.74(2) . ?
O1 C17 1.4413(13) . ?
O2 H2 0.81(2) . ?
O2 C22 1.4425(13) . ?
C1 C2 1.4052(14) . ?
C1 C14 1.4085(15) . ?
C1 C15 1.4373(15) . ?
C2 C3 1.5173(14) . ?
C2 C11 1.4019(14) . ?
C3 C3 1.614(2) 2_655 ?
C3 H3 0.9800 . ?
C3 C4 1.5172(14) . ?
C4 C5 1.4040(14) . ?
C4 C9 1.3989(14) . ?
C5 C6 1.4087(15) . ?
C5 C20 1.4389(15) . ?
C6 H6 0.9300 . ?
C6 C7 1.3837(16) . ?
C7 H7 0.9300 . ?
C7 C8 1.3947(15) . ?
C8 H8 0.9300 . ?
C8 C9 1.3873(14) . ?
C9 C10 1.5138(14) . ?
C10 C10 1.600(2) 2_655 ?
C10 H10 0.9800 . ?
C10 C11 1.5122(14) . ?
C11 C12 1.3905(14) . ?
C12 H12 0.9300 . ?
C12 C13 1.3947(16) . ?
C13 H13 0.9300 . ?
C13 C14 1.3855(16) . ?
C14 H14 0.9300 . ?
C15 C16 1.2018(16) . ?
C16 C17 1.4791(15) . ?
C17 C18 1.5285(15) . ?
C17 C19 1.5252(16) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 C21 1.2012(16) . ?
C21 C22 1.4820(15) . ?
C22 C23 1.5259(16) . ?
C22 C24 1.5278(15) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25 0.9300 . ?
C25 C26 1.343(3) 2 ?
C25 C26 1.343(3) . ?
C26 H26 0.9300 . ?
C26 C27 1.336(4) . ?
C27 H27 0.9300 . ?
C27 C28 1.401(4) . ?
C28 H28 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
C17 O1 H1 108.9(18) . . ?
C22 O2 H2 112.1(14) . . ?
C2 C1 C14 119.44(10) . . ?
C2 C1 C15 120.90(9) . . ?
C14 C1 C15 119.62(10) . . ?
C1 C2 C3 123.45(9) . . ?
C11 C2 C1 119.24(9) . . ?
C11 C2 C3 117.28(9) . . ?
C2 C3 C3 112.21(9) . 2_655 ?
C2 C3 H3 108.5 . . ?
C3 C3 H3 108.5 2_655 . ?
C4 C3 C2 107.08(8) . . ?
C4 C3 C3 112.01(9) . 2_655 ?
C4 C3 H3 108.5 . . ?
C5 C4 C3 123.40(9) . . ?
C9 C4 C3 117.20(9) . . ?
C9 C4 C5 119.40(9) . . ?
C4 C5 C6 119.05(10) . . ?
C4 C5 C20 121.42(9) . . ?
C6 C5 C20 119.51(9) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 C5 120.84(10) . . ?
C7 C6 H6 119.6 . . ?
C6 C7 H7 120.0 . . ?
C6 C7 C8 119.92(10) . . ?
C8 C7 H7 120.0 . . ?
C7 C8 H8 120.1 . . ?
C9 C8 C7 119.82(10) . . ?
C9 C8 H8 120.1 . . ?
C4 C9 C10 117.32(9) . . ?
C8 C9 C4 120.94(10) . . ?
C8 C9 C10 121.74(9) . . ?
C9 C10 C10 112.02(10) . 2_655 ?
C9 C10 H10 108.3 . . ?
C10 C10 H10 108.3 2_655 . ?
C11 C10 C9 107.63(8) . . ?
C11 C10 C10 112.10(9) . 2_655 ?
C11 C10 H10 108.3 . . ?
C2 C11 C10 117.15(9) . . ?
C12 C11 C2 120.69(10) . . ?
C12 C11 C10 122.14(10) . . ?
C11 C12 H12 120.0 . . ?
C11 C12 C13 120.09(10) . . ?
C13 C12 H12 120.0 . . ?
C12 C13 H13 120.1 . . ?
C14 C13 C12 119.90(10) . . ?
C14 C13 H13 120.1 . . ?
C1 C14 H14 119.7 . . ?
C13 C14 C1 120.63(10) . . ?
C13 C14 H14 119.7 . . ?
C16 C15 C1 177.55(12) . . ?
C15 C16 C17 178.28(12) . . ?
O1 C17 C16 109.96(9) . . ?
O1 C17 C18 107.78(9) . . ?
O1 C17 C19 108.76(9) . . ?
C16 C17 C18 109.85(9) . . ?
C16 C17 C19 109.93(9) . . ?
C19 C17 C18 110.51(10) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 C5 177.94(12) . . ?
C20 C21 C22 178.72(11) . . ?
O2 C22 C21 109.84(9) . . ?
O2 C22 C23 107.13(9) . . ?
O2 C22 C24 109.59(9) . . ?
C21 C22 C23 110.56(10) . . ?
C21 C22 C24 110.01(9) . . ?
C23 C22 C24 109.66(10) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 H25 119.9 2 . ?
C26 C25 H25 119.9 . . ?
C26 C25 C26 120.1(4) . 2 ?
C25 C26 H26 119.0 . . ?
C27 C26 C25 121.9(2) . . ?
C27 C26 H26 119.0 . . ?
C26 C27 H27 120.8 . . ?
C26 C27 C28 118.3(2) . . ?
C28 C27 H27 120.8 . . ?
C27 C28 C27 119.4(3) . 2 ?
C27 C28 H28 120.3 2 . ?
C27 C28 H28 120.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C3 104.21(10) . . . 2_655 ?
C1 C2 C3 C4 -132.49(10) . . . . ?
C1 C2 C11 C10 178.43(9) . . . . ?
C1 C2 C11 C12 -0.33(15) . . . . ?
C2 C1 C14 C13 -0.90(16) . . . . ?
C2 C3 C4 C5 132.64(10) . . . . ?
C2 C3 C4 C9 -46.43(12) . . . . ?
C2 C11 C12 C13 -0.25(17) . . . . ?
C3 C2 C11 C10 0.43(14) . . . . ?
C3 C2 C11 C12 -178.34(10) . . . . ?
C3 C3 C4 C5 -103.94(10) 2_655 . . . ?
C3 C3 C4 C9 76.99(10) 2_655 . . . ?
C3 C4 C5 C6 179.10(10) . . . . ?
C3 C4 C5 C20 -2.56(16) . . . . ?
C3 C4 C9 C8 -179.16(10) . . . . ?
C3 C4 C9 C10 1.46(14) . . . . ?
C4 C5 C6 C7 0.41(17) . . . . ?
C4 C9 C10 C10 -78.95(11) . . . 2_655 ?
C4 C9 C10 C11 44.71(12) . . . . ?
C5 C4 C9 C8 1.73(16) . . . . ?
C5 C4 C9 C10 -177.65(10) . . . . ?
C5 C6 C7 C8 1.20(18) . . . . ?
C6 C7 C8 C9 -1.34(18) . . . . ?
C7 C8 C9 C4 -0.13(17) . . . . ?
C7 C8 C9 C10 179.22(11) . . . . ?
C8 C9 C10 C10 101.67(10) . . . 2_655 ?
C8 C9 C10 C11 -134.67(11) . . . . ?
C9 C4 C5 C6 -1.85(16) . . . . ?
C9 C4 C5 C20 176.49(10) . . . . ?
C9 C10 C11 C2 -45.65(12) . . . . ?
C9 C10 C11 C12 133.09(11) . . . . ?
C10 C10 C11 C2 77.96(10) 2_655 . . . ?
C10 C10 C11 C12 -103.30(10) 2_655 . . . ?
C10 C11 C12 C13 -178.96(10) . . . . ?
C11 C2 C3 C3 -77.87(10) . . . 2_655 ?
C11 C2 C3 C4 45.42(12) . . . . ?
C11 C12 C13 C14 0.26(17) . . . . ?
C12 C13 C14 C1 0.32(17) . . . . ?
C14 C1 C2 C3 178.78(10) . . . . ?
C14 C1 C2 C11 0.90(15) . . . . ?
C15 C1 C2 C3 1.27(16) . . . . ?
C15 C1 C2 C11 -176.61(10) . . . . ?
C15 C1 C14 C13 176.64(11) . . . . ?
C20 C5 C6 C7 -177.97(11) . . . . ?
C25 C26 C27 C28 0.6(3) . . . . ?
C26 C25 C26 C27 -0.33(15) 2 . . . ?
C26 C27 C28 C27 -0.31(14) . . . 2 ?

_olex2_date_sample_data_collection 2017-07-28
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.199
_oxdiff_exptl_absorpt_empirical_full_min 0.802
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1952346'
loop_
_audit_author_name
_audit_author_address
'Hans Georg Stammler'
;University of Bielefeld
Germany
;
_audit_update_record             
;
2019-09-09 deposited with the CCDC.	2021-05-06 downloaded from the CCDC.
;
# measured as niermeier54
_audit_creation_date             2017-05-22
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H22 O2'
_chemical_formula_sum            'C24 H22 O2'
_chemical_formula_weight         342.41
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C24 H22 O2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'

_cell_length_a                   11.74087(5)
_cell_length_b                   32.16370(14)
_cell_length_c                   9.77293(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3690.55(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    48691
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.6820
_cell_measurement_theta_min      3.9600
_exptl_absorpt_coefficient_mu    0.603
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.756
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1456
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.0229
0 -1 0 0.0229
-5 -1 5 0.0626
-2 5 -6 0.0489
7 -5 2 0.0675
-1 -1 0 0.0787

_exptl_crystal_size_max          0.217
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.046
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
-0.0003 1.0008 0.0004 -0.0467 -0.0022 -0.0108
0.0003 -1.0008 -0.0004 0.0467 0.0022 0.0108
-4.7026 -0.9954 4.9847 -0.0885 -0.6813 0.7266
-2.2486 5.4183 -5.8347 -0.0304 -0.2238 -0.9742
6.7718 -5.4342 2.3973 0.1136 0.8623 0.4935
-0.9979 -1.0061 -0.0001 0.0552 -0.1281 0.0009

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0124
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            63776
_diffrn_reflns_point_group_measured_fraction_full 0.952
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.321
_diffrn_reflns_theta_min         2.748
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.9482
_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 -16.00   1.00    3.37    --  -42.33 -57.00 -90.00   26
  2  ω    -62.00 -11.00   1.00    3.37    --  -42.33 -77.00   0.00   51
  3  ω    -41.00 -16.00   1.00    3.37    --  -42.33 -57.00  90.00   25
  4  ω    -79.00 -11.00   1.00    3.37    --  -42.33 -77.00  90.00   68
  5  ω      1.00  74.00   1.00    3.37    --   42.33 -99.00  30.00   73
  6  ω     42.00  69.00   1.00   13.47    --  111.00 -94.00 150.00   27
  7  ω     38.00 104.00   1.00   13.47    --  111.00 -94.00  60.00   66
  8  ω     60.00 120.00   1.00   13.47    --  111.00-125.00  60.00   60
  9  ω     39.00 139.00   1.00   13.47    --  111.00 -77.00  60.00  100
 10  ω     68.00 117.00   1.00   13.47    --  111.00-125.00-120.00   49
 11  ω     47.00 105.00   1.00   13.47    --  111.00 -94.00-120.00   58
 12  ω     30.00  80.00   1.00   13.47    --  111.00 -94.00   0.00   50
 13  ω     31.00 106.00   1.00   13.47    --  111.00 -94.00 -60.00   75
 14  ω     83.00 109.00   1.00   13.47    --  111.00  61.00-150.00   26
 15  ω    110.00 170.00   1.00   13.47    --  111.00  77.00-120.00   60
 16  ω    139.00 178.00   1.00   13.47    --  111.00  77.00 -60.00   39
 17  ω    114.00 172.00   1.00   13.47    --  111.00  77.00 -90.00   58
 18  ω    112.00 176.00   1.00   13.47    --  111.00  77.00  30.00   64
 19  ω    129.00 157.00   1.00   13.47    --  111.00  64.00  63.46   28
 20  ω     85.00 148.00   1.00   13.47    --  111.00  55.00 -44.48   63
 21  ω     83.00 109.00   1.00   13.47    --  111.00  61.00  30.00   26
 22  ω     83.00 109.00   1.00   13.47    --  111.00  61.00  60.00   26
 23  ω     83.00 148.00   1.00   13.47    --  111.00  61.00  90.00   65
 24  ω     83.00 109.00   1.00   13.47    --  111.00  61.00   0.00   26
 25  ω     81.00 175.00   1.00   13.47    --  111.00  77.00 -30.00   94
 26  ω     83.00 109.00   1.00   13.47    --  111.00  61.00-120.00   26
 27  ω     83.00 126.00   1.00   13.47    --  111.00  61.00 -90.00   43
 28  ω     80.00 172.00   1.00   13.47    --  111.00  77.00-150.00   92
 29  ω     80.00 106.00   1.00   13.47    --  111.00  77.00-120.00   26
 30  ω     80.00 106.00   1.00   13.47    --  111.00  77.00 -90.00   26
 31  ω     80.00 106.00   1.00   13.47    --  111.00  77.00 -60.00   26
 32  ω     83.00 109.00   1.00   13.47    --  111.00  61.00 -60.00   26
 33  ω     83.00 109.00   1.00   13.47    --  111.00  61.00 -30.00   26
 34  ω     80.00 106.00   1.00   13.47    --  111.00  77.00  30.00   26
 35  ω     80.00 176.00   1.00   13.47    --  111.00  77.00   0.00   96
 36  ω     80.00 106.00   1.00   13.47    --  111.00  77.00-180.00   26
 37  ω     83.00 169.00   1.00   13.47    --  111.00  61.00-180.00   86
 38  ω     58.00 129.00   1.00    3.37    --   42.33 178.00 -90.00   71
 39  ω     80.00 106.00   1.00   13.47    --  111.00  77.00  60.00   26
 40  ω     80.00 177.00   1.00   13.47    --  111.00  77.00  90.00   97
 41  ω     83.00 109.00   1.00   13.47    --  111.00  61.00 120.00   26
 42  ω     83.00 152.00   1.00   13.47    --  111.00  61.00 150.00   69
 43  ω     80.00 169.00   1.00   13.47    --  111.00  77.00 150.00   89
 44  ω     83.00 123.00   1.00   13.47    --  111.00  64.00  63.46   40
 45  ω     80.00 149.00   1.00   13.47    --  111.00  77.00 120.00   69
 46  ω    -25.00  66.00   1.00    3.37    --   42.33 -57.00-120.00   91
 47  ω    -27.00  65.00   1.00    3.37    --   42.33 -38.00  30.00   92
 48  ω    -42.00 -16.00   1.00    3.37    --  -42.33 -57.00-180.00   26
 49  ω    -69.00 -43.00   1.00    3.37    --  -42.33 -57.00 -90.00   26
 50  ω    -79.00 -13.00   1.00    3.37    --  -42.33 -77.00 -90.00   66
 51  ω    -70.00 -11.00   1.00    3.37    --  -42.33 -77.00-180.00   59
 52  ω   -103.00 -52.00   1.00    3.37    --  -42.33 -57.00-180.00   51
 53  ω   -116.00 -89.00   1.00    3.37    --  -42.33 -77.00-180.00   27
 54  ω   -116.00 -90.00   1.00    3.37    --  -42.33 -77.00   0.00   26
 55  ω   -115.00 -24.00   1.00    3.37    --  -42.33 -38.00   0.00   91
 56  ω   -100.00 -52.00   1.00    3.37    --  -42.33 -57.00  90.00   48
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0082962000
_diffrn_orient_matrix_UB_12      -0.0466252000
_diffrn_orient_matrix_UB_13      -0.0348861000
_diffrn_orient_matrix_UB_21      0.1305604000
_diffrn_orient_matrix_UB_22      -0.0021286000
_diffrn_orient_matrix_UB_23      -0.0139390000
_diffrn_orient_matrix_UB_31      0.0100142000
_diffrn_orient_matrix_UB_32      -0.0108211000
_diffrn_orient_matrix_UB_33      0.1530526000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.791
_reflns_Friedel_fraction_full    0.898
_reflns_Friedel_fraction_max     0.896
_reflns_number_gt                6850
_reflns_number_total             6940
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     72.20
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.141
_refine_diff_density_min         -0.165
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details 
;
 Flack x determined using 2990 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         6940
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0256
_refine_ls_restrained_S_all      1.031
_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)+(0.0456P)²+0.4750P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0681
_refine_special_details          ?
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 1.10749(9) 0.56624(3) 0.46596(13) 0.0217(2) Uani 1 1 d . . . . .
H1 H 1.051(2) 0.5594(8) 0.525(3) 0.055(8) Uiso 1 1 d . . . . .
O2 O 0.87778(10) 0.57052(3) 0.89356(12) 0.0229(2) Uani 1 1 d . . . . .
H2 H 0.825(2) 0.5532(8) 0.928(3) 0.050(7) Uiso 1 1 d . . . . .
C1 C 0.86666(12) 0.69037(4) 0.40358(17) 0.0181(3) Uani 1 1 d . . . . .
C2 C 0.78870(12) 0.70932(4) 0.49944(16) 0.0167(3) Uani 1 1 d . . . . .
C3 C 0.77967(11) 0.69637(4) 0.63549(16) 0.0167(3) Uani 1 1 d . . . . .
H3A H 0.8242 0.6743 0.6659 0.020 Uiso 1 1 calc R U . . .
C4 C 0.70520(12) 0.71583(4) 0.72697(16) 0.0173(3) Uani 1 1 d . . . . .
C5 C 0.69258(12) 0.70254(4) 0.86715(17) 0.0188(3) Uani 1 1 d . . . . .
C6 C 0.61751(12) 0.72266(5) 0.95197(17) 0.0211(3) Uani 1 1 d . . . . .
H6 H 0.6094 0.7137 1.0419 0.025 Uiso 1 1 calc R U . . .
C7 C 0.55191(12) 0.75693(5) 0.90510(18) 0.0221(3) Uani 1 1 d . . . . .
H7 H 0.5025 0.7704 0.9648 0.027 Uiso 1 1 calc R U . . .
C8 C 0.56106(12) 0.77017(4) 0.77299(18) 0.0207(3) Uani 1 1 d . . . . .
H8 H 0.5176 0.7926 0.7432 0.025 Uiso 1 1 calc R U . . .
C9 C 0.63660(12) 0.74996(4) 0.67993(17) 0.0176(3) Uani 1 1 d . . . . .
C10 C 0.64404(12) 0.76209(4) 0.54331(17) 0.0191(3) Uani 1 1 d . . . . .
H10 H 0.5986 0.7839 0.5125 0.023 Uiso 1 1 calc R U . . .
C11 C 0.71734(12) 0.74261(4) 0.45163(17) 0.0179(3) Uani 1 1 d . . . . .
C12 C 0.72344(13) 0.75504(4) 0.31156(17) 0.0214(3) Uani 1 1 d . . . . .
H12 H 0.6760 0.7761 0.2799 0.026 Uiso 1 1 calc R U . . .
C13 C 0.79779(14) 0.73645(5) 0.22350(17) 0.0224(3) Uani 1 1 d . . . . .
H13 H 0.8010 0.7449 0.1326 0.027 Uiso 1 1 calc R U . . .
C14 C 0.87023(13) 0.70414(5) 0.27043(17) 0.0213(3) Uani 1 1 d . . . . .
H14 H 0.9213 0.6920 0.2097 0.026 Uiso 1 1 calc R U . . .
C15 C 0.94624(12) 0.65872(4) 0.44449(17) 0.0189(3) Uani 1 1 d . . . . .
C16 C 1.02163(12) 0.63441(4) 0.46577(17) 0.0194(3) Uani 1 1 d . . . . .
C17 C 1.12791(11) 0.60986(4) 0.48436(18) 0.0195(3) Uani 1 1 d . . . . .
C18 C 1.21072(14) 0.62261(5) 0.3721(2) 0.0276(4) Uani 1 1 d . . . . .
H18A H 1.2787 0.6061 0.3787 0.041 Uiso 1 1 calc R U . . .
H18B H 1.2297 0.6515 0.3824 0.041 Uiso 1 1 calc R U . . .
H18C H 1.1760 0.6183 0.2843 0.041 Uiso 1 1 calc R U . . .
C19 C 1.17640(14) 0.61746(5) 0.6265(2) 0.0284(4) Uani 1 1 d . . . . .
H19A H 1.1259 0.6059 0.6939 0.043 Uiso 1 1 calc R U . . .
H19B H 1.1842 0.6468 0.6415 0.043 Uiso 1 1 calc R U . . .
H19C H 1.2497 0.6044 0.6338 0.043 Uiso 1 1 calc R U . . .
C20 C 0.75922(12) 0.66798(4) 0.91601(16) 0.0198(3) Uani 1 1 d . . . . .
C21 C 0.81613(13) 0.63892(4) 0.95077(17) 0.0200(3) Uani 1 1 d . . . . .
C22 C 0.89300(12) 0.60416(4) 0.98906(16) 0.0192(3) Uani 1 1 d . . . . .
C23 C 1.01599(13) 0.61914(5) 0.9748(2) 0.0281(4) Uani 1 1 d . . . . .
H23A H 1.0670 0.5966 0.9941 0.042 Uiso 1 1 calc R U . . .
H23B H 1.0296 0.6414 1.0381 0.042 Uiso 1 1 calc R U . . .
H23C H 1.0286 0.6288 0.8831 0.042 Uiso 1 1 calc R U . . .
C24 C 0.86969(14) 0.58903(5) 1.13413(17) 0.0235(3) Uani 1 1 d . . . . .
H24A H 0.7923 0.5796 1.1407 0.035 Uiso 1 1 calc R U . . .
H24B H 0.8816 0.6114 1.1974 0.035 Uiso 1 1 calc R U . . .
H24C H 0.9204 0.5666 1.1557 0.035 Uiso 1 1 calc R U . . .
O3 O 0.93862(9) 0.53867(3) 0.63262(13) 0.0216(2) Uani 1 1 d . . . . .
H3 H 0.915(2) 0.5508(8) 0.708(3) 0.041(6) Uiso 1 1 d . . . . .
O4 O 0.75423(9) 0.50437(3) 0.99974(14) 0.0241(2) Uani 1 1 d . . . . .
H4 H 0.782(2) 0.4808(8) 0.993(3) 0.043(6) Uiso 1 1 d . . . . .
C25 C 0.61828(12) 0.61586(4) 0.47298(17) 0.0189(3) Uani 1 1 d . . . . .
C26 C 0.54874(11) 0.63169(4) 0.58368(16) 0.0170(3) Uani 1 1 d . . . . .
C27 C 0.54677(12) 0.61359(4) 0.71309(17) 0.0171(3) Uani 1 1 d . . . . .
H27 H 0.5934 0.5908 0.7308 0.020 Uiso 1 1 calc R U . . .
C28 C 0.47647(12) 0.62882(4) 0.81685(17) 0.0167(3) Uani 1 1 d . . . . .
C29 C 0.46844(12) 0.60937(4) 0.94946(17) 0.0184(3) Uani 1 1 d . . . . .
C30 C 0.39662(13) 0.62527(5) 1.04739(17) 0.0219(3) Uani 1 1 d . . . . .
H30 H 0.3911 0.6122 1.1320 0.026 Uiso 1 1 calc R U . . .
C31 C 0.33064(13) 0.66152(5) 1.02099(18) 0.0227(3) Uani 1 1 d . . . . .
H31 H 0.2831 0.6721 1.0888 0.027 Uiso 1 1 calc R U . . .
C32 C 0.33644(12) 0.68088(4) 0.89760(18) 0.0208(3) Uani 1 1 d . . . . .
H32 H 0.2931 0.7046 0.8820 0.025 Uiso 1 1 calc R U . . .
C33 C 0.40847(12) 0.66516(4) 0.79121(17) 0.0178(3) Uani 1 1 d . . . . .
C34 C 0.41187(12) 0.68357(4) 0.66254(17) 0.0186(3) Uani 1 1 d . . . . .
H34 H 0.3692 0.7074 0.6467 0.022 Uiso 1 1 calc R U . . .
C35 C 0.47759(12) 0.66715(4) 0.55659(16) 0.0176(3) Uani 1 1 d . . . . .
C36 C 0.47529(12) 0.68449(4) 0.42268(17) 0.0207(3) Uani 1 1 d . . . . .
H36 H 0.4306 0.7078 0.4053 0.025 Uiso 1 1 calc R U . . .
C37 C 0.53776(13) 0.66734(5) 0.31962(18) 0.0226(3) Uani 1 1 d . . . . .
H37 H 0.5327 0.6782 0.2317 0.027 Uiso 1 1 calc R U . . .
C38 C 0.61048(13) 0.63300(5) 0.34539(18) 0.0222(3) Uani 1 1 d . . . . .
H38 H 0.6536 0.6220 0.2743 0.027 Uiso 1 1 calc R U . . .
C39 C 0.69591(12) 0.58226(5) 0.49979(17) 0.0199(3) Uani 1 1 d . . . . .
C40 C 0.76164(12) 0.55478(5) 0.52499(17) 0.0205(3) Uani 1 1 d . . . . .
C41 C 0.84287(13) 0.52127(5) 0.55917(17) 0.0204(3) Uani 1 1 d . . . . .
C42 C 0.89282(14) 0.50200(5) 0.42988(18) 0.0243(3) Uani 1 1 d . . . . .
H42A H 0.9250 0.5235 0.3736 0.036 Uiso 1 1 calc R U . . .
H42B H 0.8338 0.4879 0.3802 0.036 Uiso 1 1 calc R U . . .
H42C H 0.9512 0.4825 0.4544 0.036 Uiso 1 1 calc R U . . .
C43 C 0.78449(15) 0.48849(6) 0.6480(2) 0.0306(4) Uani 1 1 d . . . . .
H43A H 0.8388 0.4676 0.6735 0.046 Uiso 1 1 calc R U . . .
H43B H 0.7234 0.4759 0.5975 0.046 Uiso 1 1 calc R U . . .
H43C H 0.7546 0.5014 0.7290 0.046 Uiso 1 1 calc R U . . .
C44 C 0.53238(12) 0.57226(4) 0.97882(16) 0.0191(3) Uani 1 1 d . . . . .
C45 C 0.58259(12) 0.54087(4) 1.00527(17) 0.0202(3) Uani 1 1 d . . . . .
C46 C 0.63689(13) 0.50076(4) 1.03990(17) 0.0195(3) Uani 1 1 d . . . . .
C47 C 0.57810(13) 0.46590(4) 0.96113(19) 0.0237(3) Uani 1 1 d . . . . .
H47A H 0.5922 0.4693 0.8650 0.036 Uiso 1 1 calc R U . . .
H47B H 0.4976 0.4670 0.9780 0.036 Uiso 1 1 calc R U . . .
H47C H 0.6075 0.4396 0.9909 0.036 Uiso 1 1 calc R U . . .
C48 C 0.62830(16) 0.49307(5) 1.19382(19) 0.0297(4) Uani 1 1 d . . . . .
H48A H 0.6678 0.4679 1.2166 0.045 Uiso 1 1 calc R U . . .
H48B H 0.5496 0.4906 1.2194 0.045 Uiso 1 1 calc R U . . .
H48C H 0.6621 0.5159 1.2422 0.045 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 H1 0.91(3) . ?
O1 C17 1.4346(16) . ?
O2 H2 0.90(3) . ?
O2 C22 1.4399(18) . ?
C1 C2 1.445(2) . ?
C1 C14 1.375(2) . ?
C1 C15 1.439(2) . ?
C2 C3 1.397(2) . ?
C2 C11 1.4376(19) . ?
C3 H3A 0.9300 . ?
C3 C4 1.398(2) . ?
C4 C5 1.443(2) . ?
C4 C9 1.4372(19) . ?
C5 C6 1.372(2) . ?
C5 C20 1.441(2) . ?
C6 H6 0.9300 . ?
C6 C7 1.421(2) . ?
C7 H7 0.9300 . ?
C7 C8 1.364(3) . ?
C8 H8 0.9300 . ?
C8 C9 1.427(2) . ?
C9 C10 1.394(2) . ?
C10 H10 0.9300 . ?
C10 C11 1.391(2) . ?
C11 C12 1.428(2) . ?
C12 H12 0.9300 . ?
C12 C13 1.364(2) . ?
C13 H13 0.9300 . ?
C13 C14 1.419(2) . ?
C14 H14 0.9300 . ?
C15 C16 1.199(2) . ?
C16 C17 1.4879(19) . ?
C17 C18 1.522(2) . ?
C17 C19 1.521(2) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 C21 1.198(2) . ?
C21 C22 1.485(2) . ?
C22 C23 1.529(2) . ?
C22 C24 1.524(2) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
O3 H3 0.87(3) . ?
O3 C41 1.4466(18) . ?
O4 H4 0.83(3) . ?
O4 C46 1.4372(18) . ?
C25 C26 1.448(2) . ?
C25 C38 1.367(2) . ?
C25 C39 1.438(2) . ?
C26 C27 1.392(2) . ?
C26 C35 1.4383(19) . ?
C27 H27 0.9300 . ?
C27 C28 1.396(2) . ?
C28 C29 1.442(2) . ?
C28 C33 1.4373(19) . ?
C29 C30 1.374(2) . ?
C29 C44 1.439(2) . ?
C30 H30 0.9300 . ?
C30 C31 1.423(2) . ?
C31 H31 0.9300 . ?
C31 C32 1.359(2) . ?
C32 H32 0.9300 . ?
C32 C33 1.432(2) . ?
C33 C34 1.390(2) . ?
C34 H34 0.9300 . ?
C34 C35 1.395(2) . ?
C35 C36 1.423(2) . ?
C36 H36 0.9300 . ?
C36 C37 1.363(2) . ?
C37 H37 0.9300 . ?
C37 C38 1.419(2) . ?
C38 H38 0.9300 . ?
C39 C40 1.199(2) . ?
C40 C41 1.477(2) . ?
C41 C42 1.525(2) . ?
C41 C43 1.528(2) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 C45 1.197(2) . ?
C45 C46 1.4784(19) . ?
C46 C47 1.525(2) . ?
C46 C48 1.528(2) . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C17 O1 H1 106.1(17) . . ?
C22 O2 H2 108.1(18) . . ?
C14 C1 C2 119.81(13) . . ?
C14 C1 C15 118.10(14) . . ?
C15 C1 C2 122.00(15) . . ?
C3 C2 C1 122.64(13) . . ?
C3 C2 C11 119.15(14) . . ?
C11 C2 C1 118.21(14) . . ?
C2 C3 H3A 119.3 . . ?
C2 C3 C4 121.49(13) . . ?
C4 C3 H3A 119.3 . . ?
C3 C4 C5 122.60(13) . . ?
C3 C4 C9 119.19(14) . . ?
C9 C4 C5 118.20(13) . . ?
C6 C5 C4 119.99(14) . . ?
C6 C5 C20 120.83(15) . . ?
C20 C5 C4 119.18(14) . . ?
C5 C6 H6 119.4 . . ?
C5 C6 C7 121.30(15) . . ?
C7 C6 H6 119.4 . . ?
C6 C7 H7 119.8 . . ?
C8 C7 C6 120.32(14) . . ?
C8 C7 H7 119.8 . . ?
C7 C8 H8 119.7 . . ?
C7 C8 C9 120.68(14) . . ?
C9 C8 H8 119.7 . . ?
C8 C9 C4 119.50(14) . . ?
C10 C9 C4 119.02(14) . . ?
C10 C9 C8 121.47(13) . . ?
C9 C10 H10 119.0 . . ?
C11 C10 C9 121.99(14) . . ?
C11 C10 H10 119.0 . . ?
C10 C11 C2 119.11(14) . . ?
C10 C11 C12 121.49(14) . . ?
C12 C11 C2 119.40(14) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 C11 120.94(14) . . ?
C13 C12 H12 119.5 . . ?
C12 C13 H13 120.0 . . ?
C12 C13 C14 120.05(15) . . ?
C14 C13 H13 120.0 . . ?
C1 C14 C13 121.56(15) . . ?
C1 C14 H14 119.2 . . ?
C13 C14 H14 119.2 . . ?
C16 C15 C1 171.52(16) . . ?
C15 C16 C17 170.49(15) . . ?
O1 C17 C16 111.31(11) . . ?
O1 C17 C18 106.25(13) . . ?
O1 C17 C19 109.52(13) . . ?
C16 C17 C18 107.74(13) . . ?
C16 C17 C19 109.89(13) . . ?
C19 C17 C18 112.09(13) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 C5 177.09(17) . . ?
C20 C21 C22 176.27(16) . . ?
O2 C22 C21 109.08(12) . . ?
O2 C22 C23 107.15(12) . . ?
O2 C22 C24 109.94(12) . . ?
C21 C22 C23 108.28(12) . . ?
C21 C22 C24 111.45(13) . . ?
C24 C22 C23 110.82(14) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C41 O3 H3 110.3(16) . . ?
C46 O4 H4 109.2(17) . . ?
C38 C25 C26 120.14(13) . . ?
C38 C25 C39 120.80(15) . . ?
C39 C25 C26 119.06(15) . . ?
C27 C26 C25 122.75(13) . . ?
C27 C26 C35 119.27(14) . . ?
C35 C26 C25 117.96(14) . . ?
C26 C27 H27 119.2 . . ?
C26 C27 C28 121.53(13) . . ?
C28 C27 H27 119.2 . . ?
C27 C28 C29 122.62(13) . . ?
C27 C28 C33 119.14(14) . . ?
C33 C28 C29 118.24(13) . . ?
C30 C29 C28 120.29(13) . . ?
C30 C29 C44 119.34(15) . . ?
C44 C29 C28 120.33(13) . . ?
C29 C30 H30 119.6 . . ?
C29 C30 C31 120.84(15) . . ?
C31 C30 H30 119.6 . . ?
C30 C31 H31 119.7 . . ?
C32 C31 C30 120.59(14) . . ?
C32 C31 H31 119.7 . . ?
C31 C32 H32 119.6 . . ?
C31 C32 C33 120.79(13) . . ?
C33 C32 H32 119.6 . . ?
C32 C33 C28 119.24(15) . . ?
C34 C33 C28 119.20(14) . . ?
C34 C33 C32 121.54(13) . . ?
C33 C34 H34 119.1 . . ?
C33 C34 C35 121.74(13) . . ?
C35 C34 H34 119.1 . . ?
C34 C35 C26 118.99(14) . . ?
C34 C35 C36 121.59(13) . . ?
C36 C35 C26 119.42(14) . . ?
C35 C36 H36 119.6 . . ?
C37 C36 C35 120.73(13) . . ?
C37 C36 H36 119.6 . . ?
C36 C37 H37 119.7 . . ?
C36 C37 C38 120.52(15) . . ?
C38 C37 H37 119.7 . . ?
C25 C38 C37 121.10(15) . . ?
C25 C38 H38 119.5 . . ?
C37 C38 H38 119.5 . . ?
C40 C39 C25 178.34(18) . . ?
C39 C40 C41 178.73(18) . . ?
O3 C41 C40 109.35(12) . . ?
O3 C41 C42 105.64(12) . . ?
O3 C41 C43 109.48(13) . . ?
C40 C41 C42 110.94(13) . . ?
C40 C41 C43 110.01(13) . . ?
C42 C41 C43 111.30(13) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C45 C44 C29 177.93(16) . . ?
C44 C45 C46 176.04(15) . . ?
O4 C46 C45 106.28(12) . . ?
O4 C46 C47 110.82(13) . . ?
O4 C46 C48 110.20(13) . . ?
C45 C46 C47 109.32(13) . . ?
C45 C46 C48 109.76(14) . . ?
C47 C46 C48 110.37(14) . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 178.64(12) . . . . ?
C1 C2 C11 C10 -178.15(12) . . . . ?
C1 C2 C11 C12 1.64(19) . . . . ?
C2 C1 C14 C13 -0.8(2) . . . . ?
C2 C3 C4 C5 178.73(13) . . . . ?
C2 C3 C4 C9 -0.1(2) . . . . ?
C2 C11 C12 C13 -1.5(2) . . . . ?
C3 C2 C11 C10 2.30(19) . . . . ?
C3 C2 C11 C12 -177.91(12) . . . . ?
C3 C4 C5 C6 -179.54(13) . . . . ?
C3 C4 C5 C20 0.2(2) . . . . ?
C3 C4 C9 C8 -179.52(12) . . . . ?
C3 C4 C9 C10 1.63(19) . . . . ?
C4 C5 C6 C7 -0.6(2) . . . . ?
C4 C9 C10 C11 -1.1(2) . . . . ?
C5 C4 C9 C8 1.58(19) . . . . ?
C5 C4 C9 C10 -177.27(12) . . . . ?
C5 C6 C7 C8 1.1(2) . . . . ?
C6 C7 C8 C9 -0.1(2) . . . . ?
C7 C8 C9 C4 -1.2(2) . . . . ?
C7 C8 C9 C10 177.64(13) . . . . ?
C8 C9 C10 C11 -179.98(13) . . . . ?
C9 C4 C5 C6 -0.7(2) . . . . ?
C9 C4 C5 C20 179.08(12) . . . . ?
C9 C10 C11 C2 -0.8(2) . . . . ?
C9 C10 C11 C12 179.40(13) . . . . ?
C10 C11 C12 C13 178.26(14) . . . . ?
C11 C2 C3 C4 -1.83(19) . . . . ?
C11 C12 C13 C14 0.2(2) . . . . ?
C12 C13 C14 C1 0.9(2) . . . . ?
C14 C1 C2 C3 179.01(13) . . . . ?
C14 C1 C2 C11 -0.51(19) . . . . ?
C15 C1 C2 C3 -4.5(2) . . . . ?
C15 C1 C2 C11 175.98(12) . . . . ?
C15 C1 C14 C13 -177.41(13) . . . . ?
C20 C5 C6 C7 179.59(13) . . . . ?
C25 C26 C27 C28 -178.19(13) . . . . ?
C25 C26 C35 C34 -178.49(12) . . . . ?
C25 C26 C35 C36 1.87(19) . . . . ?
C26 C25 C38 C37 2.2(2) . . . . ?
C26 C27 C28 C29 176.72(13) . . . . ?
C26 C27 C28 C33 -2.8(2) . . . . ?
C26 C35 C36 C37 1.4(2) . . . . ?
C27 C26 C35 C34 2.6(2) . . . . ?
C27 C26 C35 C36 -177.00(13) . . . . ?
C27 C28 C29 C30 -179.04(14) . . . . ?
C27 C28 C29 C44 -1.3(2) . . . . ?
C27 C28 C33 C32 -179.88(13) . . . . ?
C27 C28 C33 C34 1.8(2) . . . . ?
C28 C29 C30 C31 -1.2(2) . . . . ?
C28 C33 C34 C35 1.5(2) . . . . ?
C29 C28 C33 C32 0.53(19) . . . . ?
C29 C28 C33 C34 -177.78(13) . . . . ?
C29 C30 C31 C32 0.7(2) . . . . ?
C30 C31 C32 C33 0.3(2) . . . . ?
C31 C32 C33 C28 -1.0(2) . . . . ?
C31 C32 C33 C34 177.30(14) . . . . ?
C32 C33 C34 C35 -176.78(13) . . . . ?
C33 C28 C29 C30 0.5(2) . . . . ?
C33 C28 C29 C44 178.25(13) . . . . ?
C33 C34 C35 C26 -3.7(2) . . . . ?
C33 C34 C35 C36 175.92(13) . . . . ?
C34 C35 C36 C37 -178.24(14) . . . . ?
C35 C26 C27 C28 0.6(2) . . . . ?
C35 C36 C37 C38 -2.9(2) . . . . ?
C36 C37 C38 C25 1.1(2) . . . . ?
C38 C25 C26 C27 175.18(13) . . . . ?
C38 C25 C26 C35 -3.7(2) . . . . ?
C39 C25 C26 C27 -5.4(2) . . . . ?
C39 C25 C26 C35 175.78(12) . . . . ?
C39 C25 C38 C37 -177.20(13) . . . . ?
C44 C29 C30 C31 -178.92(14) . . . . ?

_olex2_date_sample_data_collection 2017-05-19
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.294
_oxdiff_exptl_absorpt_empirical_full_min 0.871
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_SHELXL_version_number     2014/7
_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.
;
####################################################################### 
# 
# 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_9
_database_code_depnum_ccdc_archive 'CCDC 1952351'
loop_
_audit_author_name
_audit_author_address
'Hans Georg Stammler'
;University of Bielefeld
Germany
;
_audit_update_record             
;
2019-09-09 deposited with the CCDC.	2021-05-06 downloaded from the CCDC.
;
# measured as niermeier85b
_audit_creation_date             2018-07-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C104 H76 B4 N4'
_chemical_formula_sum            'C104 H76 B4 N4'
_chemical_formula_weight         1424.92
_chemical_melting_point          ?
_chemical_oxdiff_formula         'c110 h82 B4 N4'
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'
B B 0.0090 0.0039 '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                   14.0002(4)
_cell_length_b                   40.8950(12)
_cell_length_c                   17.3331(6)
_cell_angle_alpha                90
_cell_angle_beta                 91.677(3)
_cell_angle_gamma                90
_cell_volume                     9919.6(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11562
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      71.9380
_cell_measurement_theta_min      3.2810
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.414
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.929
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.15e (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.954
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2992
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.0337
0 -1 0 0.0337
0 0 1 0.0783
0 0 -1 0.0783
1 0 0 0.0345
-1 0 0 0.0345
0 5 2 0.0527

_exptl_crystal_size_max          0.159
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.067
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
0.0002 0.9992 -0.0008 -0.0030 -0.0287 -0.0241
-0.0002 -0.9992 0.0008 0.0030 0.0287 0.0241
-0.0007 0.0021 0.9985 -0.0206 -0.0543 0.0672
0.0007 -0.0021 -0.9985 0.0206 0.0543 -0.0672
0.9987 -0.0007 0.0008 -0.1073 0.0210 -0.0116
-0.9987 0.0007 -0.0008 0.1073 -0.0210 0.0116
-0.0007 5.0003 1.9929 -0.0561 -0.2522 0.0136

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            66655
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.750
_diffrn_reflns_theta_max         66.750
_diffrn_reflns_theta_min         2.770
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -64.00  30.00   1.00   32.00    --  -38.50  57.00 -30.00   94
  2  ω   -107.00 -15.00   1.00   32.00    --  -38.50 -57.00-180.00   92
  3  ω    -79.00  -8.00   1.00   32.00    --  -38.50 125.00 -30.00   71
  4  ω    -57.00  33.00   1.00   32.00    --  -38.50  38.00 120.00   90
  5  ω     33.00  86.00   1.00   32.00    --   43.45-125.00-180.00   53
  6  ω     37.00 124.00   1.00  120.00    --  109.35 -30.00 -90.00   87
  7  ω     52.00 123.00   1.00  120.00    --  109.35 -30.00-180.00   71
  8  ω     44.00 117.00   1.00  120.00    --  109.35-125.00-180.00   73
  9  ω    139.00 171.00   1.00  120.00    --  109.35 125.00 -60.00   32
 10  ω     55.00 113.00   1.00  120.00    --  109.35 -30.00  90.00   58
 11  ω     50.00  77.00   1.00  120.00    --  109.35 -94.00 -60.00   27
 12  ω    100.00 176.00   1.00  120.00    --  109.35  30.00-120.00   76
 13  ω     89.00 117.00   1.00  120.00    --  109.35-125.00  30.00   28
 14  ω     32.00 107.00   1.00  120.00    --  109.35 -94.00-120.00   75
 15  ω     96.00 124.00   1.00  120.00    --  109.35 125.00 -60.00   28
 16  ω    118.00 169.00   1.00  120.00    --  109.35  30.00 -60.00   51
 17  ω     47.00 123.00   1.00  120.00    --  109.35 -45.00   0.00   76
 18  ω     43.00 131.00   1.00  120.00    --  109.35 -77.00 -30.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1073987000
_diffrn_orient_matrix_UB_12      -0.0029894000
_diffrn_orient_matrix_UB_13      -0.0206932000
_diffrn_orient_matrix_UB_21      0.0210568000
_diffrn_orient_matrix_UB_22      -0.0287885000
_diffrn_orient_matrix_UB_23      -0.0543226000
_diffrn_orient_matrix_UB_31      -0.0117347000
_diffrn_orient_matrix_UB_32      -0.0241039000
_diffrn_orient_matrix_UB_33      0.0673180000
_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              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10611
_reflns_number_total             17595
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.65
_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 1.171.39.15e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_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         0.501
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1113
_refine_ls_number_reflns         17595
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.1196
_refine_ls_R_factor_gt           0.0871
_refine_ls_restrained_S_all      1.063
_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)+(0.1445P)²+1.4548P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2509
_refine_ls_wR_factor_ref         0.2793
_refine_special_details          
'Crystal contains heavy disordered solvent molecules (chloroform and/or benzene), it was treated using the squeeze algorithm of Olex2. Three phenyl groups were disordered in different ratios:  C42-C47 71:29,  C69-C80 59:41. All disordered phenyl groups were constrained to have idealized geometry (AFIX 66). Hydrogen atoms were taken into account using a riding model.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C42-B2 \\sim C42B-B2 \\sim C69-B3 \\sim C69B-B3 \\sim C75-B3 \\sim C75B-B3
 with sigma of 0.02
3. Others
 Sof(C74B)=Sof(H74B)=Sof(C73B)=Sof(H73B)=Sof(C72B)=Sof(H72B)=Sof(C71B)=
 Sof(H71B)=Sof(C70B)=Sof(H70B)=Sof(C69B)=Sof(C75B)=Sof(C76B)=Sof(H76B)=
 Sof(C77B)=Sof(H77B)=Sof(C78B)=Sof(H78B)=Sof(C79B)=Sof(H79B)=Sof(C80B)=
 Sof(H80B)=1-FVAR(1)
 Sof(C69)=Sof(C70)=Sof(H70)=Sof(C71)=Sof(H71)=Sof(C72)=Sof(H72)=Sof(C73)=
 Sof(H73)=Sof(C74)=Sof(H74)=Sof(C76)=Sof(H76)=Sof(C77)=Sof(H77)=Sof(C78)=
 Sof(H78)=Sof(C79)=Sof(H79)=Sof(C80)=Sof(H80)=Sof(C75)=FVAR(1)
 Sof(C42B)=Sof(C47B)=Sof(H47B)=Sof(C46B)=Sof(H46B)=Sof(C45B)=Sof(H45B)=
 Sof(C44B)=Sof(H44B)=Sof(C43B)=Sof(H43B)=1-FVAR(2)
 Sof(C42)=Sof(C43)=Sof(H43)=Sof(C44)=Sof(H44)=Sof(C45)=Sof(H45)=Sof(C46)=
 Sof(H46)=Sof(C47)=Sof(H47)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C3(H3), C10(H10), C55(H55), C62(H62)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14), C18(H18), C19(H19),
 C20(H20), C21(H21), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28),
  C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C37(H37), C38(H38),
 C39(H39), C40(H40), C41(H41), C47B(H47B), C46B(H46B), C45B(H45B), C44B(H44B),
 C43B(H43B), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48),
 C49(H49), C50(H50), C51(H51), C52(H52), C58(H58), C59(H59), C60(H60), C64(H64),
  C65(H65), C66(H66), C70(H70), C71(H71), C72(H72), C73(H73), C74(H74),
 C74B(H74B), C73B(H73B), C72B(H72B), C71B(H71B), C70B(H70B), C76B(H76B),
 C77B(H77B), C78B(H78B), C79B(H79B), C80B(H80B), C76(H76), C77(H77), C78(H78),
 C79(H79), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84), C85(H85), C89(H89),
  C90(H90), C91(H91), C92(H92), C93(H93), C95(H95), C96(H96), C97(H97),
 C98(H98), C99(H99), C100(H100), C101(H101), C102(H102), C103(H103), C104(H104)
4.c Fitted hexagon refined as free rotating group:
 C42B(C47B,C46B,C45B,C44B,C43B), C69(C70,C71,C72,C73,C74), C74B(C73B,C72B,C71B,
 C70B,C69B), C75B(C76B,C77B,C78B,C79B,C80B), C76(C77,C78,C79,C80,C75)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.5565(2) 0.64525(7) 0.36733(19) 0.0746(8) Uani 1 1 d . . . . .
N2 N 0.4015(2) 0.53575(6) 0.41131(16) 0.0643(7) Uani 1 1 d . . . . .
N3 N 0.5363(2) 0.75731(6) 0.44719(16) 0.0663(7) Uani 1 1 d . . . . .
N4 N 0.06843(18) 0.65324(6) 0.54982(18) 0.0661(7) Uani 1 1 d . . . . .
C1 C 0.6567(2) 0.58888(7) 0.61862(18) 0.0601(7) Uani 1 1 d . . . . .
C2 C 0.5886(2) 0.59409(7) 0.67455(19) 0.0602(8) Uani 1 1 d . . . . .
C3 C 0.4919(2) 0.61037(7) 0.65774(19) 0.0595(7) Uani 1 1 d . . . . .
H3 H 0.479242 0.609972 0.600670 0.071 Uiso 1 1 calc R . . . .
C4 C 0.4170(2) 0.58977(7) 0.69529(19) 0.0596(7) Uani 1 1 d . . . . .
C5 C 0.3345(2) 0.57831(8) 0.6566(2) 0.0632(8) Uani 1 1 d . . . . .
C6 C 0.2657(3) 0.56188(9) 0.6995(2) 0.0766(10) Uani 1 1 d . . . . .
H6 H 0.207945 0.554845 0.674578 0.092 Uiso 1 1 calc R . . . .
C7 C 0.2804(3) 0.55579(10) 0.7772(2) 0.0834(11) Uani 1 1 d . . . . .
H7 H 0.232045 0.545658 0.806207 0.100 Uiso 1 1 calc R . . . .
C8 C 0.3666(3) 0.56466(9) 0.8121(2) 0.0759(10) Uani 1 1 d . . . . .
H8 H 0.379551 0.558905 0.864509 0.091 Uiso 1 1 calc R . . . .
C9 C 0.4341(2) 0.58176(8) 0.77192(19) 0.0628(8) Uani 1 1 d . . . . .
C10 C 0.5321(3) 0.59008(8) 0.8075(2) 0.0654(8) Uani 1 1 d . . . . .
H10 H 0.543301 0.575939 0.853999 0.079 Uiso 1 1 calc R . . . .
C11 C 0.6064(2) 0.58169(8) 0.74906(19) 0.0632(8) Uani 1 1 d . . . . .
C12 C 0.6879(3) 0.56430(8) 0.7675(2) 0.0712(9) Uani 1 1 d . . . . .
H12 H 0.698633 0.556317 0.818461 0.085 Uiso 1 1 calc R . . . .
C13 C 0.7546(3) 0.55843(9) 0.7112(2) 0.0714(9) Uani 1 1 d . . . . .
H13 H 0.810198 0.545904 0.723111 0.086 Uiso 1 1 calc R . . . .
C14 C 0.7395(2) 0.57088(8) 0.6381(2) 0.0691(9) Uani 1 1 d . . . . .
H14 H 0.785895 0.567240 0.600102 0.083 Uiso 1 1 calc R . . . .
C15 C 0.6469(2) 0.60207(8) 0.5430(2) 0.0631(8) Uani 1 1 d . . . . .
C16 C 0.6459(2) 0.61262(8) 0.4771(2) 0.0651(8) Uani 1 1 d . . . . .
C17 C 0.6682(3) 0.59479(9) 0.3330(2) 0.0720(9) Uani 1 1 d . . . . .
C18 C 0.6069(3) 0.58560(10) 0.2720(3) 0.0910(12) Uani 1 1 d . . . . .
H18 H 0.552497 0.598747 0.260185 0.109 Uiso 1 1 calc R . . . .
C19 C 0.6226(4) 0.55802(13) 0.2280(3) 0.1124(16) Uani 1 1 d . . . . .
H19 H 0.578872 0.552316 0.187321 0.135 Uiso 1 1 calc R . . . .
C20 C 0.7008(5) 0.53904(13) 0.2432(3) 0.1120(16) Uani 1 1 d . . . . .
H20 H 0.711737 0.520058 0.213090 0.134 Uiso 1 1 calc R . . . .
C21 C 0.7623(4) 0.54718(13) 0.3006(3) 0.1096(16) Uani 1 1 d . . . . .
H21 H 0.817244 0.534064 0.310606 0.132 Uiso 1 1 calc R . . . .
C22 C 0.7464(3) 0.57473(11) 0.3457(3) 0.0925(12) Uani 1 1 d . . . . .
H22 H 0.790762 0.579868 0.386391 0.111 Uiso 1 1 calc R . . . .
C23 C 0.7396(2) 0.65268(9) 0.3879(2) 0.0734(9) Uani 1 1 d . . . . .
C24 C 0.7422(3) 0.67823(9) 0.4402(3) 0.0842(11) Uani 1 1 d . . . . .
H24 H 0.693537 0.679395 0.477196 0.101 Uiso 1 1 calc R . . . .
C25 C 0.8124(3) 0.70226(11) 0.4416(3) 0.0947(13) Uani 1 1 d . . . . .
H25 H 0.812384 0.719040 0.479464 0.114 Uiso 1 1 calc R . . . .
C26 C 0.8812(3) 0.70139(12) 0.3875(3) 0.0937(13) Uani 1 1 d . . . . .
H26 H 0.928264 0.718111 0.386290 0.112 Uiso 1 1 calc R . . . .
C27 C 0.8825(3) 0.67626(13) 0.3348(3) 0.0959(13) Uani 1 1 d . . . . .
H27 H 0.932149 0.675251 0.298672 0.115 Uiso 1 1 calc R . . . .
C28 C 0.8119(3) 0.65229(11) 0.3339(2) 0.0845(11) Uani 1 1 d . . . . .
H28 H 0.812750 0.635474 0.296060 0.101 Uiso 1 1 calc R . . . .
C29 C 0.5505(3) 0.66009(9) 0.2991(2) 0.0760(10) Uani 1 1 d . . . . .
H29 H 0.602612 0.658563 0.265375 0.091 Uiso 1 1 calc R . . . .
C30 C 0.4692(3) 0.67791(10) 0.2755(3) 0.0931(13) Uani 1 1 d . . . . .
H30 H 0.466476 0.688402 0.226610 0.112 Uiso 1 1 calc R . . . .
C31 C 0.3948(3) 0.68000(13) 0.3231(4) 0.1176(18) Uani 1 1 d . . . . .
H31 H 0.339506 0.692197 0.308357 0.141 Uiso 1 1 calc R . . . .
C32 C 0.4002(4) 0.66437(15) 0.3926(4) 0.1264(19) Uani 1 1 d . . . . .
H32 H 0.347980 0.665042 0.426350 0.152 Uiso 1 1 calc R . . . .
C33 C 0.4823(3) 0.64762(13) 0.4130(3) 0.1017(14) Uani 1 1 d . . . . .
H33 H 0.486104 0.637268 0.462021 0.122 Uiso 1 1 calc R . . . .
C34 C 0.3235(2) 0.57876(7) 0.5745(2) 0.0639(8) Uani 1 1 d . . . . .
C35 C 0.3137(2) 0.57280(8) 0.5058(2) 0.0652(8) Uani 1 1 d . . . . .
C36 C 0.2150(3) 0.53087(8) 0.4200(2) 0.0708(9) Uani 1 1 d . . . . .
C37 C 0.1532(3) 0.52695(10) 0.3559(3) 0.0814(10) Uani 1 1 d . . . . .
H37 H 0.162555 0.539950 0.311301 0.098 Uiso 1 1 calc R . . . .
C38 C 0.0777(3) 0.50427(11) 0.3555(3) 0.0903(12) Uani 1 1 d . . . . .
H38 H 0.036861 0.502166 0.310999 0.108 Uiso 1 1 calc R . . . .
C39 C 0.0629(3) 0.48535(11) 0.4185(3) 0.0863(11) Uani 1 1 d . . . . .
H39 H 0.011943 0.470016 0.418212 0.104 Uiso 1 1 calc R . . . .
C40 C 0.1229(3) 0.48858(9) 0.4835(3) 0.0837(11) Uani 1 1 d . . . . .
H40 H 0.113296 0.475440 0.527798 0.100 Uiso 1 1 calc R . . . .
C41 C 0.1962(3) 0.51099(8) 0.4830(2) 0.0712(9) Uani 1 1 d . . . . .
H41 H 0.236139 0.512998 0.528047 0.085 Uiso 1 1 calc R . . . .
C42 C 0.2862(8) 0.58268(18) 0.3520(5) 0.063(2) Uani 0.698(12) 1 d D . P A 1
C42B C 0.3131(12) 0.5805(3) 0.3408(8) 0.080(9) Uani 0.302(12) 1 d D . P A 2
C47B C 0.3428(14) 0.5680(4) 0.2709(11) 0.131(10) Uani 0.302(12) 1 d G . P A 2
H47B H 0.372476 0.547106 0.269143 0.157 Uiso 0.302(12) 1 calc R . P A 2
C46B C 0.3291(15) 0.5860(5) 0.2035(8) 0.146(11) Uani 0.302(12) 1 d G . P A 2
H46B H 0.349410 0.577488 0.155725 0.175 Uiso 0.302(12) 1 calc R . P A 2
C45B C 0.2857(18) 0.6165(5) 0.2061(8) 0.20(2) Uani 0.302(12) 1 d G . P A 2
H45B H 0.276295 0.628884 0.160012 0.235 Uiso 0.302(12) 1 calc R . P A 2
C44B C 0.2559(19) 0.6290(3) 0.2760(10) 0.139(10) Uani 0.302(12) 1 d G . P A 2
H44B H 0.226245 0.649898 0.277717 0.167 Uiso 0.302(12) 1 calc R . P A 2
C43B C 0.2696(15) 0.6110(3) 0.3433(8) 0.100(6) Uani 0.302(12) 1 d G . P A 2
H43B H 0.249310 0.619517 0.391135 0.120 Uiso 0.302(12) 1 calc R . P A 2
C43 C 0.3481(6) 0.58366(17) 0.2890(5) 0.0749(19) Uani 0.698(12) 1 d . . P A 1
H43 H 0.404919 0.570968 0.290365 0.090 Uiso 0.698(12) 1 calc R . P A 1
C44 C 0.3260(6) 0.6032(2) 0.2249(4) 0.085(2) Uani 0.698(12) 1 d . . P A 1
H44 H 0.368351 0.604002 0.183134 0.102 Uiso 0.698(12) 1 calc R . P A 1
C45 C 0.2425(6) 0.6214(2) 0.2219(5) 0.090(2) Uani 0.698(12) 1 d . . P A 1
H45 H 0.226685 0.634388 0.177933 0.108 Uiso 0.698(12) 1 calc R . P A 1
C46 C 0.1826(6) 0.62043(16) 0.2837(4) 0.083(2) Uani 0.698(12) 1 d . . P A 1
H46 H 0.124984 0.632728 0.282504 0.100 Uiso 0.698(12) 1 calc R . P A 1
C47 C 0.2064(6) 0.60174(16) 0.3466(3) 0.078(2) Uani 0.698(12) 1 d . . P A 1
H47 H 0.164887 0.602012 0.388965 0.093 Uiso 0.698(12) 1 calc R . P A 1
C48 C 0.4012(3) 0.50908(8) 0.3667(2) 0.0740(9) Uani 1 1 d . . . . .
H48 H 0.342504 0.501954 0.343473 0.089 Uiso 1 1 calc R . . . .
C49 C 0.4820(3) 0.49182(9) 0.3536(2) 0.0774(10) Uani 1 1 d . . . . .
H49 H 0.479282 0.473115 0.321102 0.093 Uiso 1 1 calc R . . . .
C50 C 0.5681(3) 0.50144(8) 0.3874(2) 0.0772(10) Uani 1 1 d . . . . .
H50 H 0.624893 0.489308 0.379546 0.093 Uiso 1 1 calc R . . . .
C51 C 0.5695(3) 0.52927(8) 0.4331(2) 0.0721(9) Uani 1 1 d . . . . .
H51 H 0.627443 0.536833 0.456666 0.087 Uiso 1 1 calc R . . . .
C52 C 0.4852(3) 0.54572(8) 0.4435(2) 0.0681(8) Uani 1 1 d . . . . .
H52 H 0.486019 0.564847 0.474586 0.082 Uiso 1 1 calc R . . . .
C53 C 0.6400(2) 0.68144(8) 0.67604(18) 0.0619(8) Uani 1 1 d . . . . .
C54 C 0.5823(2) 0.65953(8) 0.71595(19) 0.0612(8) Uani 1 1 d . . . . .
C55 C 0.4846(2) 0.64796(7) 0.68682(18) 0.0587(7) Uani 1 1 d . . . . .
H55 H 0.463247 0.661971 0.642287 0.070 Uiso 1 1 calc R . . . .
C56 C 0.4159(2) 0.65263(7) 0.75237(19) 0.0590(7) Uani 1 1 d . . . . .
C57 C 0.3220(2) 0.66454(7) 0.7419(2) 0.0632(8) Uani 1 1 d . . . . .
C58 C 0.2670(3) 0.66960(8) 0.8076(2) 0.0734(9) Uani 1 1 d . . . . .
H58 H 0.204809 0.678692 0.801352 0.088 Uiso 1 1 calc R . . . .
C59 C 0.3005(3) 0.66180(9) 0.8801(2) 0.0760(9) Uani 1 1 d . . . . .
H59 H 0.262007 0.665381 0.923570 0.091 Uiso 1 1 calc R . . . .
C60 C 0.3914(3) 0.64860(8) 0.8895(2) 0.0683(8) Uani 1 1 d . . . . .
H60 H 0.414916 0.642715 0.939562 0.082 Uiso 1 1 calc R . . . .
C61 C 0.4471(3) 0.64403(7) 0.82692(19) 0.0630(8) Uani 1 1 d . . . . .
C62 C 0.5436(2) 0.62766(8) 0.83358(19) 0.0633(8) Uani 1 1 d . . . . .
H62 H 0.565376 0.628103 0.889047 0.076 Uiso 1 1 calc R . . . .
C63 C 0.6151(3) 0.64687(8) 0.78730(19) 0.0644(8) Uani 1 1 d . . . . .
C64 C 0.7067(3) 0.65337(9) 0.8144(2) 0.0729(9) Uani 1 1 d . . . . .
H64 H 0.728481 0.644699 0.862656 0.087 Uiso 1 1 calc R . . . .
C65 C 0.7666(3) 0.67250(9) 0.7715(2) 0.0798(10) Uani 1 1 d . . . . .
H65 H 0.830873 0.675843 0.788947 0.096 Uiso 1 1 calc R . . . .
C66 C 0.7340(3) 0.68689(9) 0.7032(2) 0.0730(9) Uani 1 1 d . . . . .
H66 H 0.775342 0.700453 0.674800 0.088 Uiso 1 1 calc R . . . .
C67 C 0.6033(2) 0.70233(8) 0.6152(2) 0.0629(8) Uani 1 1 d . . . . .
C68 C 0.5772(2) 0.72521(8) 0.57520(19) 0.0640(8) Uani 1 1 d . . . . .
C69 C 0.6187(5) 0.78854(11) 0.5639(3) 0.065(2) Uani 0.591(5) 1 d D . P B 1
C70 C 0.6156(4) 0.81770(11) 0.5227(3) 0.086(2) Uani 0.591(5) 1 d G . P B 1
H70 H 0.574809 0.819712 0.478172 0.104 Uiso 0.591(5) 1 calc R . P B 1
C71 C 0.6723(4) 0.84393(9) 0.5466(3) 0.097(3) Uani 0.591(5) 1 d G . P B 1
H71 H 0.670236 0.863856 0.518402 0.116 Uiso 0.591(5) 1 calc R . P B 1
C72 C 0.7321(3) 0.84099(13) 0.6117(3) 0.089(2) Uani 0.591(5) 1 d G . P B 1
H72 H 0.770822 0.858910 0.627990 0.107 Uiso 0.591(5) 1 calc R . P B 1
C73 C 0.7351(4) 0.81183(16) 0.6529(3) 0.087(7) Uani 0.591(5) 1 d G . P B 1
H73 H 0.775983 0.809820 0.697349 0.104 Uiso 0.591(5) 1 calc R . P B 1
C74 C 0.6785(5) 0.78561(13) 0.6290(3) 0.058(2) Uani 0.591(5) 1 d G . P B 1
H74 H 0.680557 0.765676 0.657120 0.070 Uiso 0.591(5) 1 calc R . P B 1
C74B C 0.6624(7) 0.7924(3) 0.6326(4) 0.057(3) Uani 0.409(5) 1 d . . P B 2
H74B H 0.624641 0.782576 0.670928 0.069 Uiso 0.409(5) 1 calc R . P B 2
C73B C 0.7371(7) 0.8132(2) 0.6542(3) 0.070(8) Uani 0.409(5) 1 d G . P B 2
H73B H 0.750354 0.817546 0.707313 0.084 Uiso 0.409(5) 1 calc R . P B 2
C72B C 0.7923(5) 0.82760(17) 0.5982(5) 0.093(3) Uani 0.409(5) 1 d G . P B 2
H72B H 0.843315 0.841796 0.612977 0.111 Uiso 0.409(5) 1 calc R . P B 2
C71B C 0.7728(5) 0.82123(18) 0.5206(4) 0.091(3) Uani 0.409(5) 1 d G . P B 2
H71B H 0.810564 0.831076 0.482255 0.109 Uiso 0.409(5) 1 calc R . P B 2
C70B C 0.6981(5) 0.80046(18) 0.4989(4) 0.084(3) Uani 0.409(5) 1 d G . P B 2
H70B H 0.684851 0.796106 0.445868 0.101 Uiso 0.409(5) 1 calc R . P B 2
C69B C 0.6429(6) 0.7861(2) 0.5550(5) 0.103(6) Uani 0.409(5) 1 d DG . P B 2
C75B C 0.4484(7) 0.7713(3) 0.5805(6) 0.050(3) Uani 0.409(5) 1 d D . P B 2
C76B C 0.4302(6) 0.8045(2) 0.5697(5) 0.075(4) Uani 0.409(5) 1 d G . P B 2
H76B H 0.475281 0.817803 0.544512 0.090 Uiso 0.409(5) 1 calc R . P B 2
C77B C 0.3461(6) 0.81807(18) 0.5958(8) 0.089(4) Uani 0.409(5) 1 d G . P B 2
H77B H 0.333662 0.840706 0.588408 0.107 Uiso 0.409(5) 1 calc R . P B 2
C78B C 0.2802(6) 0.7986(2) 0.6327(8) 0.076(4) Uani 0.409(5) 1 d G . P B 2
H78B H 0.222696 0.807851 0.650514 0.091 Uiso 0.409(5) 1 calc R . P B 2
C79B C 0.2984(7) 0.7654(2) 0.6435(7) 0.064(3) Uani 0.409(5) 1 d G . P B 2
H79B H 0.253350 0.752091 0.668725 0.077 Uiso 0.409(5) 1 calc R . P B 2
C80B C 0.3825(8) 0.7518(2) 0.6174(7) 0.054(4) Uani 0.409(5) 1 d G . P B 2
H80B H 0.394969 0.729187 0.624831 0.064 Uiso 0.409(5) 1 calc R . P B 2
C76 C 0.3894(5) 0.7999(2) 0.5573(4) 0.083(3) Uani 0.591(5) 1 d . . P B 1
H76 H 0.419209 0.815304 0.524670 0.100 Uiso 0.591(5) 1 calc R . P B 1
C77 C 0.3038(6) 0.80774(18) 0.5915(5) 0.098(4) Uani 0.591(5) 1 d G . P B 1
H77 H 0.275112 0.828479 0.582291 0.117 Uiso 0.591(5) 1 calc R . P B 1
C78 C 0.2603(5) 0.7852(2) 0.6392(5) 0.077(3) Uani 0.591(5) 1 d G . P B 1
H78 H 0.201792 0.790582 0.662574 0.093 Uiso 0.591(5) 1 calc R . P B 1
C79 C 0.3023(7) 0.75490(19) 0.6526(6) 0.078(3) Uani 0.591(5) 1 d G . P B 1
H79 H 0.272570 0.739511 0.685239 0.094 Uiso 0.591(5) 1 calc R . P B 1
C80 C 0.3879(8) 0.7471(2) 0.6184(7) 0.092(5) Uani 0.591(5) 1 d G . P B 1
H80 H 0.416666 0.726335 0.627618 0.111 Uiso 0.591(5) 1 calc R . P B 1
C75 C 0.4315(5) 0.7696(3) 0.5707(6) 0.086(4) Uani 0.591(5) 1 d DG . P B 1
C81 C 0.4583(3) 0.76406(11) 0.4063(2) 0.0887(12) Uani 1 1 d . . . . .
H81 H 0.400897 0.768437 0.432344 0.106 Uiso 1 1 calc R . . . .
C82 C 0.4570(3) 0.76499(10) 0.3264(2) 0.0884(12) Uani 1 1 d . . . . .
H82 H 0.399522 0.770207 0.298655 0.106 Uiso 1 1 calc R . . . .
C83 C 0.5368(3) 0.75855(10) 0.2882(2) 0.0823(11) Uani 1 1 d . . . . .
H83 H 0.537737 0.759468 0.233445 0.099 Uiso 1 1 calc R . . . .
C84 C 0.6155(3) 0.75074(16) 0.3306(3) 0.1219(19) Uani 1 1 d . . . . .
H84 H 0.673218 0.745605 0.305824 0.146 Uiso 1 1 calc R . . . .
C85 C 0.6124(3) 0.75018(14) 0.4090(2) 0.1081(16) Uani 1 1 d . . . . .
H85 H 0.668857 0.744279 0.437395 0.130 Uiso 1 1 calc R . . . .
C86 C 0.2764(2) 0.67147(8) 0.6687(2) 0.0653(8) Uani 1 1 d . . . . .
C87 C 0.2188(2) 0.67800(8) 0.6171(2) 0.0676(9) Uani 1 1 d . . . . .
C88 C 0.0578(2) 0.71131(8) 0.6126(2) 0.0717(9) Uani 1 1 d . . . . .
C89 C 0.0077(3) 0.73745(10) 0.5781(3) 0.0971(13) Uani 1 1 d . . . . .
H89 H 0.016888 0.742324 0.525231 0.117 Uiso 1 1 calc R . . . .
C90 C -0.0556(4) 0.75641(12) 0.6199(4) 0.1160(17) Uani 1 1 d . . . . .
H90 H -0.090071 0.773572 0.594833 0.139 Uiso 1 1 calc R . . . .
C91 C -0.0684(3) 0.75065(12) 0.6960(3) 0.0996(14) Uani 1 1 d . . . . .
H91 H -0.110322 0.763955 0.724611 0.119 Uiso 1 1 calc R . . . .
C92 C -0.0204(3) 0.72556(13) 0.7305(3) 0.0959(13) Uani 1 1 d . . . . .
H92 H -0.028802 0.721252 0.783697 0.115 Uiso 1 1 calc R . . . .
C93 C 0.0409(3) 0.70607(11) 0.6888(2) 0.0830(11) Uani 1 1 d . . . . .
H93 H 0.072403 0.688385 0.714397 0.100 Uiso 1 1 calc R . . . .
C94 C 0.1510(2) 0.70194(8) 0.4800(2) 0.0668(9) Uani 1 1 d . . . . .
C95 C 0.1942(3) 0.73258(11) 0.4734(3) 0.0978(14) Uani 1 1 d . . . . .
H95 H 0.218292 0.742701 0.519300 0.117 Uiso 1 1 calc R . . . .
C96 C 0.2044(3) 0.74910(11) 0.4050(3) 0.0952(13) Uani 1 1 d . . . . .
H96 H 0.232340 0.770269 0.404847 0.114 Uiso 1 1 calc R . . . .
C97 C 0.1738(3) 0.73475(10) 0.3369(3) 0.0833(11) Uani 1 1 d . . . . .
H97 H 0.180545 0.745965 0.289328 0.100 Uiso 1 1 calc R . . . .
C98 C 0.1341(3) 0.70472(11) 0.3378(3) 0.0901(12) Uani 1 1 d . . . . .
H98 H 0.113706 0.694400 0.291096 0.108 Uiso 1 1 calc R . . . .
C99 C 0.1233(3) 0.68883(9) 0.4094(2) 0.0777(10) Uani 1 1 d . . . . .
H99 H 0.095178 0.667699 0.408946 0.093 Uiso 1 1 calc R . . . .
C100 C -0.0271(2) 0.65338(9) 0.5412(2) 0.0756(10) Uani 1 1 d . . . . .
H100 H -0.060412 0.673402 0.547658 0.091 Uiso 1 1 calc R . . . .
C101 C -0.0785(3) 0.62574(10) 0.5236(3) 0.0881(12) Uani 1 1 d . . . . .
H101 H -0.146222 0.626550 0.518398 0.106 Uiso 1 1 calc R . . . .
C102 C -0.0306(3) 0.59683(10) 0.5135(3) 0.0961(14) Uani 1 1 d . . . . .
H102 H -0.064482 0.577355 0.500698 0.115 Uiso 1 1 calc R . . . .
C103 C 0.0678(3) 0.59656(10) 0.5221(3) 0.0938(13) Uani 1 1 d . . . . .
H103 H 0.102572 0.576831 0.515780 0.113 Uiso 1 1 calc R . . . .
C104 C 0.1150(3) 0.62526(8) 0.5401(3) 0.0790(10) Uani 1 1 d . . . . .
H104 H 0.182680 0.625063 0.545777 0.095 Uiso 1 1 calc R . . . .
B1 B 0.6547(3) 0.62538(10) 0.3903(3) 0.0713(10) Uani 1 1 d . . . . .
B2 B 0.3024(3) 0.55691(10) 0.4213(3) 0.0705(10) Uani 1 1 d D . . . .
B3 B 0.5437(3) 0.75968(10) 0.5413(2) 0.0703(10) Uani 1 1 d D . . . .
B4 B 0.1276(3) 0.68754(10) 0.5635(3) 0.0698(10) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C29 1.330(5) . ?
N1 C33 1.327(5) . ?
N1 B1 1.636(5) . ?
N2 C48 1.337(4) . ?
N2 C52 1.346(4) . ?
N2 B2 1.649(5) . ?
N3 C81 1.314(5) . ?
N3 C85 1.305(5) . ?
N3 B3 1.634(5) . ?
N4 C100 1.342(4) . ?
N4 C104 1.330(4) . ?
N4 B4 1.643(4) . ?
C1 C2 1.396(4) . ?
C1 C14 1.406(5) . ?
C1 C15 1.420(5) . ?
C2 C3 1.529(4) . ?
C2 C11 1.403(5) . ?
C3 H3 1.0000 . ?
C3 C4 1.508(4) . ?
C3 C55 1.622(4) . ?
C4 C5 1.399(5) . ?
C4 C9 1.382(5) . ?
C5 C6 1.406(5) . ?
C5 C34 1.427(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.378(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.383(6) . ?
C8 H8 0.9500 . ?
C8 C9 1.381(5) . ?
C9 C10 1.527(5) . ?
C10 H10 1.0000 . ?
C10 C11 1.512(5) . ?
C10 C62 1.609(4) . ?
C11 C12 1.374(5) . ?
C12 H12 0.9500 . ?
C12 C13 1.391(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.375(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.222(5) . ?
C16 B1 1.600(6) . ?
C17 C18 1.393(6) . ?
C17 C22 1.381(5) . ?
C17 B1 1.612(6) . ?
C18 H18 0.9500 . ?
C18 C19 1.382(6) . ?
C19 H19 0.9500 . ?
C19 C20 1.362(7) . ?
C20 H20 0.9500 . ?
C20 C21 1.338(7) . ?
C21 H21 0.9500 . ?
C21 C22 1.393(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.384(6) . ?
C23 C28 1.399(5) . ?
C23 B1 1.632(6) . ?
C24 H24 0.9500 . ?
C24 C25 1.389(5) . ?
C25 H25 0.9500 . ?
C25 C26 1.364(7) . ?
C26 H26 0.9500 . ?
C26 C27 1.375(7) . ?
C27 H27 0.9500 . ?
C27 C28 1.392(6) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C29 C30 1.402(5) . ?
C30 H30 0.9500 . ?
C30 C31 1.349(7) . ?
C31 H31 0.9500 . ?
C31 C32 1.363(8) . ?
C32 H32 0.9500 . ?
C32 C33 1.376(6) . ?
C33 H33 0.9500 . ?
C34 C35 1.218(5) . ?
C35 B2 1.606(6) . ?
C36 C37 1.398(5) . ?
C36 C41 1.392(5) . ?
C36 B2 1.622(5) . ?
C37 H37 0.9500 . ?
C37 C38 1.406(6) . ?
C38 H38 0.9500 . ?
C38 C39 1.360(6) . ?
C39 H39 0.9500 . ?
C39 C40 1.391(6) . ?
C40 H40 0.9500 . ?
C40 C41 1.376(5) . ?
C41 H41 0.9500 . ?
C42 C43 1.414(11) . ?
C42 C47 1.364(11) . ?
C42 B2 1.609(8) . ?
C42B C47B 1.3900 . ?
C42B C43B 1.3900 . ?
C42B B2 1.706(11) . ?
C47B H47B 0.9500 . ?
C47B C46B 1.3900 . ?
C46B H46B 0.9500 . ?
C46B C45B 1.3900 . ?
C45B H45B 0.9500 . ?
C45B C44B 1.3900 . ?
C44B H44B 0.9500 . ?
C44B C43B 1.3900 . ?
C43B H43B 0.9500 . ?
C43 H43 0.9500 . ?
C43 C44 1.396(10) . ?
C44 H44 0.9500 . ?
C44 C45 1.386(12) . ?
C45 H45 0.9500 . ?
C45 C46 1.380(11) . ?
C46 H46 0.9500 . ?
C46 C47 1.364(8) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
C48 C49 1.358(5) . ?
C49 H49 0.9500 . ?
C49 C50 1.383(5) . ?
C50 H50 0.9500 . ?
C50 C51 1.386(5) . ?
C51 H51 0.9500 . ?
C51 C52 1.375(5) . ?
C52 H52 0.9500 . ?
C53 C54 1.402(5) . ?
C53 C66 1.402(5) . ?
C53 C67 1.440(5) . ?
C54 C55 1.520(4) . ?
C54 C63 1.405(5) . ?
C55 H55 1.0000 . ?
C55 C56 1.522(4) . ?
C56 C57 1.408(5) . ?
C56 C61 1.397(5) . ?
C57 C58 1.409(5) . ?
C57 C86 1.432(5) . ?
C58 H58 0.9500 . ?
C58 C59 1.366(5) . ?
C59 H59 0.9500 . ?
C59 C60 1.387(5) . ?
C60 H60 0.9500 . ?
C60 C61 1.368(5) . ?
C61 C62 1.509(5) . ?
C62 H62 1.0000 . ?
C62 C63 1.519(5) . ?
C63 C64 1.379(5) . ?
C64 H64 0.9500 . ?
C64 C65 1.381(5) . ?
C65 H65 0.9500 . ?
C65 C66 1.388(5) . ?
C66 H66 0.9500 . ?
C67 C68 1.214(5) . ?
C68 B3 1.593(5) . ?
C69 C70 1.3900 . ?
C69 C74 1.3900 . ?
C69 B3 1.621(5) . ?
C70 H70 0.9500 . ?
C70 C71 1.3900 . ?
C71 H71 0.9500 . ?
C71 C72 1.3900 . ?
C72 H72 0.9500 . ?
C72 C73 1.3900 . ?
C73 H73 0.9500 . ?
C73 C74 1.3900 . ?
C74 H74 0.9500 . ?
C74B H74B 0.9500 . ?
C74B C73B 1.3900 . ?
C74B C69B 1.3900 . ?
C73B H73B 0.9500 . ?
C73B C72B 1.3900 . ?
C72B H72B 0.9500 . ?
C72B C71B 1.3900 . ?
C71B H71B 0.9500 . ?
C71B C70B 1.3900 . ?
C70B H70B 0.9500 . ?
C70B C69B 1.3900 . ?
C69B B3 1.770(7) . ?
C75B C76B 1.3900 . ?
C75B C80B 1.3900 . ?
C75B B3 1.588(8) . ?
C76B H76B 0.9500 . ?
C76B C77B 1.3900 . ?
C77B H77B 0.9500 . ?
C77B C78B 1.3900 . ?
C78B H78B 0.9500 . ?
C78B C79B 1.3900 . ?
C79B H79B 0.9500 . ?
C79B C80B 1.3900 . ?
C80B H80B 0.9500 . ?
C76 H76 0.9500 . ?
C76 C77 1.3900 . ?
C76 C75 1.3900 . ?
C77 H77 0.9500 . ?
C77 C78 1.3900 . ?
C78 H78 0.9500 . ?
C78 C79 1.3900 . ?
C79 H79 0.9500 . ?
C79 C80 1.3900 . ?
C80 H80 0.9500 . ?
C80 C75 1.3900 . ?
C75 B3 1.714(7) . ?
C81 H81 0.9500 . ?
C81 C82 1.384(5) . ?
C82 H82 0.9500 . ?
C82 C83 1.342(6) . ?
C83 H83 0.9500 . ?
C83 C84 1.344(6) . ?
C84 H84 0.9500 . ?
C84 C85 1.360(6) . ?
C85 H85 0.9500 . ?
C86 C87 1.217(5) . ?
C87 B4 1.604(5) . ?
C88 C89 1.403(6) . ?
C88 C93 1.366(5) . ?
C88 B4 1.634(6) . ?
C89 H89 0.9500 . ?
C89 C90 1.396(6) . ?
C90 H90 0.9500 . ?
C90 C91 1.356(7) . ?
C91 H91 0.9500 . ?
C91 C92 1.356(7) . ?
C92 H92 0.9500 . ?
C92 C93 1.389(6) . ?
C93 H93 0.9500 . ?
C94 C95 1.398(5) . ?
C94 C99 1.381(5) . ?
C94 B4 1.605(6) . ?
C95 H95 0.9500 . ?
C95 C96 1.375(6) . ?
C96 H96 0.9500 . ?
C96 C97 1.376(6) . ?
C97 H97 0.9500 . ?
C97 C98 1.348(6) . ?
C98 H98 0.9500 . ?
C98 C99 1.412(6) . ?
C99 H99 0.9500 . ?
C100 H100 0.9500 . ?
C100 C101 1.370(5) . ?
C101 H101 0.9500 . ?
C101 C102 1.373(6) . ?
C102 H102 0.9500 . ?
C102 C103 1.382(6) . ?
C103 H103 0.9500 . ?
C103 C104 1.378(5) . ?
C104 H104 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C29 N1 B1 118.3(3) . . ?
C33 N1 C29 117.8(4) . . ?
C33 N1 B1 123.9(3) . . ?
C48 N2 C52 118.3(3) . . ?
C48 N2 B2 120.0(3) . . ?
C52 N2 B2 121.5(3) . . ?
C81 N3 B3 123.6(3) . . ?
C85 N3 C81 116.8(3) . . ?
C85 N3 B3 119.4(3) . . ?
C100 N4 B4 120.6(3) . . ?
C104 N4 C100 118.7(3) . . ?
C104 N4 B4 120.4(3) . . ?
C2 C1 C14 119.2(3) . . ?
C2 C1 C15 122.3(3) . . ?
C14 C1 C15 118.5(3) . . ?
C1 C2 C3 123.6(3) . . ?
C1 C2 C11 118.6(3) . . ?
C11 C2 C3 117.7(3) . . ?
C2 C3 H3 108.2 . . ?
C2 C3 C55 114.7(3) . . ?
C4 C3 C2 107.3(3) . . ?
C4 C3 H3 108.2 . . ?
C4 C3 C55 110.1(3) . . ?
C55 C3 H3 108.2 . . ?
C5 C4 C3 123.7(3) . . ?
C9 C4 C3 116.3(3) . . ?
C9 C4 C5 119.9(3) . . ?
C4 C5 C6 118.4(3) . . ?
C4 C5 C34 122.5(3) . . ?
C6 C5 C34 118.6(3) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 C5 121.2(4) . . ?
C7 C6 H6 119.4 . . ?
C6 C7 H7 120.5 . . ?
C6 C7 C8 118.9(4) . . ?
C8 C7 H7 120.5 . . ?
C7 C8 H8 119.6 . . ?
C9 C8 C7 120.9(4) . . ?
C9 C8 H8 119.6 . . ?
C4 C9 C10 117.7(3) . . ?
C8 C9 C4 120.2(3) . . ?
C8 C9 C10 121.9(3) . . ?
C9 C10 H10 108.3 . . ?
C9 C10 C62 114.1(3) . . ?
C11 C10 C9 107.8(3) . . ?
C11 C10 H10 108.3 . . ?
C11 C10 C62 109.8(3) . . ?
C62 C10 H10 108.3 . . ?
C2 C11 C10 115.3(3) . . ?
C12 C11 C2 121.6(3) . . ?
C12 C11 C10 123.0(3) . . ?
C11 C12 H12 120.1 . . ?
C11 C12 C13 119.7(3) . . ?
C13 C12 H12 120.1 . . ?
C12 C13 H13 120.2 . . ?
C14 C13 C12 119.6(3) . . ?
C14 C13 H13 120.2 . . ?
C1 C14 H14 119.4 . . ?
C13 C14 C1 121.2(3) . . ?
C13 C14 H14 119.4 . . ?
C16 C15 C1 174.8(3) . . ?
C15 C16 B1 174.7(3) . . ?
C18 C17 B1 126.6(4) . . ?
C22 C17 C18 115.3(4) . . ?
C22 C17 B1 118.0(4) . . ?
C17 C18 H18 118.8 . . ?
C19 C18 C17 122.3(5) . . ?
C19 C18 H18 118.9 . . ?
C18 C19 H19 120.0 . . ?
C20 C19 C18 119.9(5) . . ?
C20 C19 H19 120.0 . . ?
C19 C20 H20 120.1 . . ?
C21 C20 C19 119.8(5) . . ?
C21 C20 H20 120.1 . . ?
C20 C21 H21 119.7 . . ?
C20 C21 C22 120.6(5) . . ?
C22 C21 H21 119.7 . . ?
C17 C22 C21 122.0(5) . . ?
C17 C22 H22 119.0 . . ?
C21 C22 H22 119.0 . . ?
C24 C23 C28 116.2(4) . . ?
C24 C23 B1 120.3(3) . . ?
C28 C23 B1 123.4(4) . . ?
C23 C24 H24 118.3 . . ?
C23 C24 C25 123.4(4) . . ?
C25 C24 H24 118.3 . . ?
C24 C25 H25 120.5 . . ?
C26 C25 C24 118.9(5) . . ?
C26 C25 H25 120.5 . . ?
C25 C26 H26 120.0 . . ?
C25 C26 C27 119.9(4) . . ?
C27 C26 H26 120.0 . . ?
C26 C27 H27 119.6 . . ?
C26 C27 C28 120.7(4) . . ?
C28 C27 H27 119.6 . . ?
C23 C28 H28 119.6 . . ?
C27 C28 C23 120.8(4) . . ?
C27 C28 H28 119.6 . . ?
N1 C29 H29 119.1 . . ?
N1 C29 C30 121.7(4) . . ?
C30 C29 H29 119.1 . . ?
C29 C30 H30 120.4 . . ?
C31 C30 C29 119.3(5) . . ?
C31 C30 H30 120.4 . . ?
C30 C31 H31 120.4 . . ?
C30 C31 C32 119.1(5) . . ?
C32 C31 H31 120.4 . . ?
C31 C32 H32 120.5 . . ?
C31 C32 C33 119.0(5) . . ?
C33 C32 H32 120.5 . . ?
N1 C33 C32 123.1(5) . . ?
N1 C33 H33 118.5 . . ?
C32 C33 H33 118.5 . . ?
C35 C34 C5 167.7(3) . . ?
C34 C35 B2 167.7(3) . . ?
C37 C36 B2 122.4(4) . . ?
C41 C36 C37 115.5(4) . . ?
C41 C36 B2 122.1(3) . . ?
C36 C37 H37 119.1 . . ?
C36 C37 C38 121.8(4) . . ?
C38 C37 H37 119.1 . . ?
C37 C38 H38 119.9 . . ?
C39 C38 C37 120.2(4) . . ?
C39 C38 H38 119.9 . . ?
C38 C39 H39 120.2 . . ?
C38 C39 C40 119.6(4) . . ?
C40 C39 H39 120.2 . . ?
C39 C40 H40 120.3 . . ?
C41 C40 C39 119.4(4) . . ?
C41 C40 H40 120.3 . . ?
C36 C41 H41 118.3 . . ?
C40 C41 C36 123.4(4) . . ?
C40 C41 H41 118.3 . . ?
C43 C42 B2 121.3(7) . . ?
C47 C42 C43 116.7(6) . . ?
C47 C42 B2 121.6(8) . . ?
C47B C42B C43B 120.0 . . ?
C47B C42B B2 122.8(10) . . ?
C43B C42B B2 115.6(9) . . ?
C42B C47B H47B 120.0 . . ?
C42B C47B C46B 120.0 . . ?
C46B C47B H47B 120.0 . . ?
C47B C46B H46B 120.0 . . ?
C45B C46B C47B 120.0 . . ?
C45B C46B H46B 120.0 . . ?
C46B C45B H45B 120.0 . . ?
C46B C45B C44B 120.0 . . ?
C44B C45B H45B 120.0 . . ?
C45B C44B H44B 120.0 . . ?
C43B C44B C45B 120.0 . . ?
C43B C44B H44B 120.0 . . ?
C42B C43B H43B 120.0 . . ?
C44B C43B C42B 120.0 . . ?
C44B C43B H43B 120.0 . . ?
C42 C43 H43 119.8 . . ?
C44 C43 C42 120.3(7) . . ?
C44 C43 H43 119.8 . . ?
C43 C44 H44 119.9 . . ?
C45 C44 C43 120.3(7) . . ?
C45 C44 H44 119.9 . . ?
C44 C45 H45 120.4 . . ?
C46 C45 C44 119.1(6) . . ?
C46 C45 H45 120.4 . . ?
C45 C46 H46 120.1 . . ?
C47 C46 C45 119.8(6) . . ?
C47 C46 H46 120.1 . . ?
C42 C47 H47 118.1 . . ?
C46 C47 C42 123.8(7) . . ?
C46 C47 H47 118.1 . . ?
N2 C48 H48 118.9 . . ?
N2 C48 C49 122.2(4) . . ?
C49 C48 H48 118.9 . . ?
C48 C49 H49 119.9 . . ?
C48 C49 C50 120.1(3) . . ?
C50 C49 H49 119.9 . . ?
C49 C50 H50 120.9 . . ?
C49 C50 C51 118.2(3) . . ?
C51 C50 H50 120.9 . . ?
C50 C51 H51 120.7 . . ?
C52 C51 C50 118.7(4) . . ?
C52 C51 H51 120.7 . . ?
N2 C52 C51 122.5(3) . . ?
N2 C52 H52 118.7 . . ?
C51 C52 H52 118.7 . . ?
C54 C53 C66 118.9(3) . . ?
C54 C53 C67 122.8(3) . . ?
C66 C53 C67 117.6(3) . . ?
C53 C54 C55 124.1(3) . . ?
C53 C54 C63 119.5(3) . . ?
C63 C54 C55 116.4(3) . . ?
C3 C55 H55 108.9 . . ?
C54 C55 C3 109.5(3) . . ?
C54 C55 H55 108.9 . . ?
C54 C55 C56 107.2(3) . . ?
C56 C55 C3 113.5(2) . . ?
C56 C55 H55 108.9 . . ?
C57 C56 C55 123.7(3) . . ?
C61 C56 C55 118.1(3) . . ?
C61 C56 C57 118.1(3) . . ?
C56 C57 C58 118.5(3) . . ?
C56 C57 C86 124.9(3) . . ?
C58 C57 C86 116.6(3) . . ?
C57 C58 H58 119.0 . . ?
C59 C58 C57 121.9(3) . . ?
C59 C58 H58 119.0 . . ?
C58 C59 H59 120.4 . . ?
C58 C59 C60 119.2(4) . . ?
C60 C59 H59 120.4 . . ?
C59 C60 H60 119.9 . . ?
C61 C60 C59 120.2(3) . . ?
C61 C60 H60 119.9 . . ?
C56 C61 C62 116.0(3) . . ?
C60 C61 C56 121.9(3) . . ?
C60 C61 C62 122.0(3) . . ?
C10 C62 H62 108.2 . . ?
C61 C62 C10 108.7(3) . . ?
C61 C62 H62 108.2 . . ?
C61 C62 C63 109.4(3) . . ?
C63 C62 C10 114.1(3) . . ?
C63 C62 H62 108.2 . . ?
C54 C63 C62 116.9(3) . . ?
C64 C63 C54 120.4(3) . . ?
C64 C63 C62 122.6(3) . . ?
C63 C64 H64 120.0 . . ?
C63 C64 C65 120.0(3) . . ?
C65 C64 H64 120.0 . . ?
C64 C65 H65 119.7 . . ?
C64 C65 C66 120.6(3) . . ?
C66 C65 H65 119.7 . . ?
C53 C66 H66 119.9 . . ?
C65 C66 C53 120.1(3) . . ?
C65 C66 H66 119.9 . . ?
C68 C67 C53 165.9(3) . . ?
C67 C68 B3 166.7(4) . . ?
C70 C69 C74 120.0 . . ?
C70 C69 B3 119.4(4) . . ?
C74 C69 B3 120.2(4) . . ?
C69 C70 H70 120.0 . . ?
C71 C70 C69 120.0 . . ?
C71 C70 H70 120.0 . . ?
C70 C71 H71 120.0 . . ?
C70 C71 C72 120.0 . . ?
C72 C71 H71 120.0 . . ?
C71 C72 H72 120.0 . . ?
C73 C72 C71 120.0 . . ?
C73 C72 H72 120.0 . . ?
C72 C73 H73 120.0 . . ?
C72 C73 C74 120.0 . . ?
C74 C73 H73 120.0 . . ?
C69 C74 H74 120.0 . . ?
C73 C74 C69 120.0 . . ?
C73 C74 H74 120.0 . . ?
C73B C74B H74B 120.0 . . ?
C73B C74B C69B 120.0 . . ?
C69B C74B H74B 120.0 . . ?
C74B C73B H73B 120.0 . . ?
C74B C73B C72B 120.0 . . ?
C72B C73B H73B 120.0 . . ?
C73B C72B H72B 120.0 . . ?
C73B C72B C71B 120.0 . . ?
C71B C72B H72B 120.0 . . ?
C72B C71B H71B 120.0 . . ?
C70B C71B C72B 120.0 . . ?
C70B C71B H71B 120.0 . . ?
C71B C70B H70B 120.0 . . ?
C71B C70B C69B 120.0 . . ?
C69B C70B H70B 120.0 . . ?
C74B C69B B3 112.0(5) . . ?
C70B C69B C74B 120.0 . . ?
C70B C69B B3 128.0(5) . . ?
C76B C75B C80B 120.0 . . ?
C76B C75B B3 112.8(6) . . ?
C80B C75B B3 127.0(6) . . ?
C75B C76B H76B 120.0 . . ?
C75B C76B C77B 120.0 . . ?
C77B C76B H76B 120.0 . . ?
C76B C77B H77B 120.0 . . ?
C78B C77B C76B 120.0 . . ?
C78B C77B H77B 120.0 . . ?
C77B C78B H78B 120.0 . . ?
C79B C78B C77B 120.0 . . ?
C79B C78B H78B 120.0 . . ?
C78B C79B H79B 120.0 . . ?
C78B C79B C80B 120.0 . . ?
C80B C79B H79B 120.0 . . ?
C75B C80B H80B 120.0 . . ?
C79B C80B C75B 120.0 . . ?
C79B C80B H80B 120.0 . . ?
C77 C76 H76 120.0 . . ?
C77 C76 C75 120.0 . . ?
C75 C76 H76 120.0 . . ?
C76 C77 H77 120.0 . . ?
C76 C77 C78 120.0 . . ?
C78 C77 H77 120.0 . . ?
C77 C78 H78 120.0 . . ?
C79 C78 C77 120.0 . . ?
C79 C78 H78 120.0 . . ?
C78 C79 H79 120.0 . . ?
C80 C79 C78 120.0 . . ?
C80 C79 H79 120.0 . . ?
C79 C80 H80 120.0 . . ?
C79 C80 C75 120.0 . . ?
C75 C80 H80 120.0 . . ?
C76 C75 B3 123.2(7) . . ?
C80 C75 C76 120.0 . . ?
C80 C75 B3 116.3(7) . . ?
N3 C81 H81 118.9 . . ?
N3 C81 C82 122.1(4) . . ?
C82 C81 H81 118.9 . . ?
C81 C82 H82 119.9 . . ?
C83 C82 C81 120.1(4) . . ?
C83 C82 H82 119.9 . . ?
C82 C83 H83 121.4 . . ?
C82 C83 C84 117.2(4) . . ?
C84 C83 H83 121.4 . . ?
C83 C84 H84 120.0 . . ?
C83 C84 C85 120.1(4) . . ?
C85 C84 H84 120.0 . . ?
N3 C85 C84 123.6(4) . . ?
N3 C85 H85 118.2 . . ?
C84 C85 H85 118.2 . . ?
C87 C86 C57 164.6(4) . . ?
C86 C87 B4 167.9(4) . . ?
C89 C88 B4 122.0(4) . . ?
C93 C88 C89 115.7(4) . . ?
C93 C88 B4 122.2(3) . . ?
C88 C89 H89 119.4 . . ?
C90 C89 C88 121.2(5) . . ?
C90 C89 H89 119.4 . . ?
C89 C90 H90 119.6 . . ?
C91 C90 C89 120.8(5) . . ?
C91 C90 H90 119.6 . . ?
C90 C91 H91 120.6 . . ?
C92 C91 C90 118.8(5) . . ?
C92 C91 H91 120.6 . . ?
C91 C92 H92 119.6 . . ?
C91 C92 C93 120.8(5) . . ?
C93 C92 H92 119.6 . . ?
C88 C93 C92 122.7(4) . . ?
C88 C93 H93 118.7 . . ?
C92 C93 H93 118.7 . . ?
C95 C94 B4 120.2(3) . . ?
C99 C94 C95 112.7(4) . . ?
C99 C94 B4 126.7(3) . . ?
C94 C95 H95 117.7 . . ?
C96 C95 C94 124.6(4) . . ?
C96 C95 H95 117.7 . . ?
C95 C96 H96 120.2 . . ?
C95 C96 C97 119.5(4) . . ?
C97 C96 H96 120.2 . . ?
C96 C97 H97 120.1 . . ?
C98 C97 C96 119.7(4) . . ?
C98 C97 H97 120.1 . . ?
C97 C98 H98 120.5 . . ?
C97 C98 C99 119.0(4) . . ?
C99 C98 H98 120.5 . . ?
C94 C99 C98 124.5(4) . . ?
C94 C99 H99 117.8 . . ?
C98 C99 H99 117.8 . . ?
N4 C100 H100 118.8 . . ?
N4 C100 C101 122.4(4) . . ?
C101 C100 H100 118.8 . . ?
C100 C101 H101 120.5 . . ?
C100 C101 C102 118.9(4) . . ?
C102 C101 H101 120.5 . . ?
C101 C102 H102 120.6 . . ?
C101 C102 C103 118.9(4) . . ?
C103 C102 H102 120.6 . . ?
C102 C103 H103 120.4 . . ?
C104 C103 C102 119.2(4) . . ?
C104 C103 H103 120.4 . . ?
N4 C104 C103 121.9(3) . . ?
N4 C104 H104 119.1 . . ?
C103 C104 H104 119.1 . . ?
C16 B1 N1 107.7(3) . . ?
C16 B1 C17 109.9(3) . . ?
C16 B1 C23 108.9(3) . . ?
C17 B1 N1 110.4(3) . . ?
C17 B1 C23 114.6(3) . . ?
C23 B1 N1 105.2(3) . . ?
N2 B2 C42B 96.7(6) . . ?
C35 B2 N2 104.3(3) . . ?
C35 B2 C36 109.4(3) . . ?
C35 B2 C42 115.1(4) . . ?
C35 B2 C42B 120.6(7) . . ?
C36 B2 N2 106.9(3) . . ?
C36 B2 C42B 116.3(7) . . ?
C42 B2 N2 111.5(5) . . ?
C42 B2 C36 109.3(5) . . ?
N3 B3 C69B 101.3(4) . . ?
N3 B3 C75 106.2(4) . . ?
C68 B3 N3 109.0(3) . . ?
C68 B3 C69 111.9(3) . . ?
C68 B3 C69B 105.6(4) . . ?
C68 B3 C75 111.2(4) . . ?
C69 B3 N3 107.8(3) . . ?
C69 B3 C75 110.4(5) . . ?
C75B B3 N3 114.6(5) . . ?
C75B B3 C68 110.5(4) . . ?
C75B B3 C69B 115.2(6) . . ?
C87 B4 N4 105.4(3) . . ?
C87 B4 C88 108.7(3) . . ?
C87 B4 C94 115.5(3) . . ?
C88 B4 N4 106.1(3) . . ?
C94 B4 N4 107.4(3) . . ?
C94 B4 C88 113.1(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C29 C30 C31 -0.3(7) . . . . ?
N2 C48 C49 C50 0.7(6) . . . . ?
N3 C81 C82 C83 0.7(7) . . . . ?
N4 C100 C101 C102 -0.7(7) . . . . ?
C1 C2 C3 C4 133.5(3) . . . . ?
C1 C2 C3 C55 -103.8(3) . . . . ?
C1 C2 C11 C10 176.5(3) . . . . ?
C1 C2 C11 C12 -1.0(5) . . . . ?
C2 C1 C14 C13 -0.2(5) . . . . ?
C2 C3 C4 C5 -128.4(3) . . . . ?
C2 C3 C4 C9 50.3(4) . . . . ?
C2 C3 C55 C54 7.0(4) . . . . ?
C2 C3 C55 C56 -112.7(3) . . . . ?
C2 C11 C12 C13 -0.6(5) . . . . ?
C3 C2 C11 C10 -8.0(4) . . . . ?
C3 C2 C11 C12 174.5(3) . . . . ?
C3 C4 C5 C6 -174.2(3) . . . . ?
C3 C4 C5 C34 14.3(5) . . . . ?
C3 C4 C9 C8 176.1(3) . . . . ?
C3 C4 C9 C10 -8.6(4) . . . . ?
C3 C55 C56 C57 -100.1(3) . . . . ?
C3 C55 C56 C61 78.6(4) . . . . ?
C4 C3 C55 C54 128.2(3) . . . . ?
C4 C3 C55 C56 8.5(4) . . . . ?
C4 C5 C6 C7 -2.9(5) . . . . ?
C4 C5 C34 C35 115.7(15) . . . . ?
C4 C9 C10 C11 -41.7(4) . . . . ?
C4 C9 C10 C62 80.6(4) . . . . ?
C5 C4 C9 C8 -5.1(5) . . . . ?
C5 C4 C9 C10 170.2(3) . . . . ?
C5 C6 C7 C8 -3.2(6) . . . . ?
C5 C34 C35 B2 -3(3) . . . . ?
C6 C5 C34 C35 -55.8(17) . . . . ?
C6 C7 C8 C9 5.3(6) . . . . ?
C7 C8 C9 C4 -1.2(5) . . . . ?
C7 C8 C9 C10 -176.3(3) . . . . ?
C8 C9 C10 C11 133.4(3) . . . . ?
C8 C9 C10 C62 -104.3(4) . . . . ?
C9 C4 C5 C6 7.0(5) . . . . ?
C9 C4 C5 C34 -164.4(3) . . . . ?
C9 C10 C11 C2 49.7(4) . . . . ?
C9 C10 C11 C12 -132.8(3) . . . . ?
C9 C10 C62 C61 8.8(4) . . . . ?
C9 C10 C62 C63 -113.6(3) . . . . ?
C10 C11 C12 C13 -177.9(3) . . . . ?
C10 C62 C63 C54 82.5(4) . . . . ?
C10 C62 C63 C64 -100.8(4) . . . . ?
C11 C2 C3 C4 -41.7(4) . . . . ?
C11 C2 C3 C55 80.9(4) . . . . ?
C11 C10 C62 C61 129.9(3) . . . . ?
C11 C10 C62 C63 7.6(4) . . . . ?
C11 C12 C13 C14 1.8(5) . . . . ?
C12 C13 C14 C1 -1.4(5) . . . . ?
C14 C1 C2 C3 -173.9(3) . . . . ?
C14 C1 C2 C11 1.4(5) . . . . ?
C15 C1 C2 C3 8.2(5) . . . . ?
C15 C1 C2 C11 -176.5(3) . . . . ?
C15 C1 C14 C13 177.8(3) . . . . ?
C17 C18 C19 C20 -0.9(8) . . . . ?
C18 C17 C22 C21 -0.3(6) . . . . ?
C18 C17 B1 N1 -0.1(5) . . . . ?
C18 C17 B1 C16 118.5(4) . . . . ?
C18 C17 B1 C23 -118.6(4) . . . . ?
C18 C19 C20 C21 -0.1(9) . . . . ?
C19 C20 C21 C22 0.8(9) . . . . ?
C20 C21 C22 C17 -0.6(8) . . . . ?
C22 C17 C18 C19 1.0(7) . . . . ?
C22 C17 B1 N1 -178.2(3) . . . . ?
C22 C17 B1 C16 -59.6(4) . . . . ?
C22 C17 B1 C23 63.3(5) . . . . ?
C23 C24 C25 C26 1.7(7) . . . . ?
C24 C23 C28 C27 1.1(6) . . . . ?
C24 C23 B1 N1 65.8(4) . . . . ?
C24 C23 B1 C16 -49.4(5) . . . . ?
C24 C23 B1 C17 -172.8(3) . . . . ?
C24 C25 C26 C27 -2.5(7) . . . . ?
C25 C26 C27 C28 2.6(7) . . . . ?
C26 C27 C28 C23 -1.9(6) . . . . ?
C28 C23 C24 C25 -1.0(6) . . . . ?
C28 C23 B1 N1 -113.2(4) . . . . ?
C28 C23 B1 C16 131.6(4) . . . . ?
C28 C23 B1 C17 8.2(5) . . . . ?
C29 N1 C33 C32 0.5(8) . . . . ?
C29 N1 B1 C16 175.5(3) . . . . ?
C29 N1 B1 C17 -64.6(4) . . . . ?
C29 N1 B1 C23 59.5(4) . . . . ?
C29 C30 C31 C32 -0.8(8) . . . . ?
C30 C31 C32 C33 1.7(9) . . . . ?
C31 C32 C33 N1 -1.6(9) . . . . ?
C33 N1 C29 C30 0.4(6) . . . . ?
C33 N1 B1 C16 -4.2(5) . . . . ?
C33 N1 B1 C17 115.7(4) . . . . ?
C33 N1 B1 C23 -120.2(4) . . . . ?
C34 C5 C6 C7 168.9(3) . . . . ?
C34 C35 B2 N2 -59.5(17) . . . . ?
C34 C35 B2 C36 54.6(17) . . . . ?
C34 C35 B2 C42 178.0(15) . . . . ?
C34 C35 B2 C42B -166.4(16) . . . . ?
C36 C37 C38 C39 -0.1(6) . . . . ?
C37 C36 C41 C40 0.5(5) . . . . ?
C37 C36 B2 N2 -104.5(4) . . . . ?
C37 C36 B2 C35 143.0(3) . . . . ?
C37 C36 B2 C42 16.2(6) . . . . ?
C37 C36 B2 C42B 2.1(8) . . . . ?
C37 C38 C39 C40 0.1(6) . . . . ?
C38 C39 C40 C41 0.2(6) . . . . ?
C39 C40 C41 C36 -0.5(6) . . . . ?
C41 C36 C37 C38 -0.2(5) . . . . ?
C41 C36 B2 N2 75.7(4) . . . . ?
C41 C36 B2 C35 -36.7(4) . . . . ?
C41 C36 B2 C42 -163.5(5) . . . . ?
C41 C36 B2 C42B -177.7(7) . . . . ?
C42 C43 C44 C45 -1.0(12) . . . . ?
C42B C47B C46B C45B 0.0 . . . . ?
C47B C42B C43B C44B 0.0 . . . . ?
C47B C42B B2 N2 41.9(10) . . . . ?
C47B C42B B2 C35 152.9(8) . . . . ?
C47B C42B B2 C36 -70.8(11) . . . . ?
C47B C46B C45B C44B 0.0 . . . . ?
C46B C45B C44B C43B 0.0 . . . . ?
C45B C44B C43B C42B 0.0 . . . . ?
C43B C42B C47B C46B 0.0 . . . . ?
C43B C42B B2 N2 -152.6(11) . . . . ?
C43B C42B B2 C35 -41.5(13) . . . . ?
C43B C42B B2 C36 94.8(13) . . . . ?
C43 C42 C47 C46 2.0(13) . . . . ?
C43 C42 B2 N2 4.9(10) . . . . ?
C43 C42 B2 C35 123.4(7) . . . . ?
C43 C42 B2 C36 -113.0(8) . . . . ?
C43 C44 C45 C46 1.2(12) . . . . ?
C44 C45 C46 C47 0.2(12) . . . . ?
C45 C46 C47 C42 -1.9(12) . . . . ?
C47 C42 C43 C44 -0.6(12) . . . . ?
C47 C42 B2 N2 176.8(6) . . . . ?
C47 C42 B2 C35 -64.6(9) . . . . ?
C47 C42 B2 C36 58.9(8) . . . . ?
C48 N2 C52 C51 -1.0(5) . . . . ?
C48 N2 B2 C35 150.8(3) . . . . ?
C48 N2 B2 C36 34.9(4) . . . . ?
C48 N2 B2 C42 -84.4(5) . . . . ?
C48 N2 B2 C42B -85.2(7) . . . . ?
C48 C49 C50 C51 -1.4(6) . . . . ?
C49 C50 C51 C52 0.9(6) . . . . ?
C50 C51 C52 N2 0.3(6) . . . . ?
C52 N2 C48 C49 0.5(5) . . . . ?
C52 N2 B2 C35 -33.2(4) . . . . ?
C52 N2 B2 C36 -149.1(3) . . . . ?
C52 N2 B2 C42 91.5(5) . . . . ?
C52 N2 B2 C42B 90.8(7) . . . . ?
C53 C54 C55 C3 106.6(3) . . . . ?
C53 C54 C55 C56 -130.0(3) . . . . ?
C53 C54 C63 C62 170.6(3) . . . . ?
C53 C54 C63 C64 -6.2(5) . . . . ?
C53 C67 C68 B3 -17(3) . . . . ?
C54 C53 C66 C65 -4.5(5) . . . . ?
C54 C53 C67 C68 113.2(14) . . . . ?
C54 C55 C56 C57 138.9(3) . . . . ?
C54 C55 C56 C61 -42.4(4) . . . . ?
C54 C63 C64 C65 0.2(6) . . . . ?
C55 C3 C4 C5 106.1(3) . . . . ?
C55 C3 C4 C9 -75.1(3) . . . . ?
C55 C54 C63 C62 -9.8(4) . . . . ?
C55 C54 C63 C64 173.4(3) . . . . ?
C55 C56 C57 C58 -176.4(3) . . . . ?
C55 C56 C57 C86 4.9(5) . . . . ?
C55 C56 C61 C60 177.5(3) . . . . ?
C55 C56 C61 C62 -5.9(4) . . . . ?
C56 C57 C58 C59 -3.2(5) . . . . ?
C56 C57 C86 C87 169.5(11) . . . . ?
C56 C61 C62 C10 -77.4(3) . . . . ?
C56 C61 C62 C63 47.7(4) . . . . ?
C57 C56 C61 C60 -3.7(5) . . . . ?
C57 C56 C61 C62 172.9(3) . . . . ?
C57 C58 C59 C60 0.2(6) . . . . ?
C57 C86 C87 B4 5(3) . . . . ?
C58 C57 C86 C87 -9.3(14) . . . . ?
C58 C59 C60 C61 1.2(5) . . . . ?
C59 C60 C61 C56 0.7(5) . . . . ?
C59 C60 C61 C62 -175.8(3) . . . . ?
C60 C61 C62 C10 99.2(4) . . . . ?
C60 C61 C62 C63 -135.7(3) . . . . ?
C61 C56 C57 C58 4.9(4) . . . . ?
C61 C56 C57 C86 -173.9(3) . . . . ?
C61 C62 C63 C54 -39.5(4) . . . . ?
C61 C62 C63 C64 137.2(3) . . . . ?
C62 C10 C11 C2 -75.1(4) . . . . ?
C62 C10 C11 C12 102.4(4) . . . . ?
C62 C63 C64 C65 -176.4(3) . . . . ?
C63 C54 C55 C3 -73.0(4) . . . . ?
C63 C54 C55 C56 50.4(4) . . . . ?
C63 C64 C65 C66 3.8(6) . . . . ?
C64 C65 C66 C53 -1.6(6) . . . . ?
C66 C53 C54 C55 -171.3(3) . . . . ?
C66 C53 C54 C63 8.3(5) . . . . ?
C66 C53 C67 C68 -57.4(16) . . . . ?
C67 C53 C54 C55 18.2(5) . . . . ?
C67 C53 C54 C63 -162.2(3) . . . . ?
C67 C53 C66 C65 166.5(3) . . . . ?
C67 C68 B3 N3 174.3(14) . . . . ?
C67 C68 B3 C69 55.2(16) . . . . ?
C67 C68 B3 C69B 66.2(16) . . . . ?
C67 C68 B3 C75B -58.9(17) . . . . ?
C67 C68 B3 C75 -68.9(16) . . . . ?
C69 C70 C71 C72 0.0 . . . . ?
C70 C69 C74 C73 0.0 . . . . ?
C70 C69 B3 N3 42.4(5) . . . . ?
C70 C69 B3 C68 162.3(4) . . . . ?
C70 C69 B3 C75 -73.2(6) . . . . ?
C70 C71 C72 C73 0.0 . . . . ?
C71 C72 C73 C74 0.0 . . . . ?
C72 C73 C74 C69 0.0 . . . . ?
C74 C69 C70 C71 0.0 . . . . ?
C74 C69 B3 N3 -144.6(3) . . . . ?
C74 C69 B3 C68 -24.7(5) . . . . ?
C74 C69 B3 C75 99.8(5) . . . . ?
C74B C73B C72B C71B 0.0 . . . . ?
C74B C69B B3 N3 178.7(3) . . . . ?
C74B C69B B3 C68 -67.7(4) . . . . ?
C74B C69B B3 C75B 54.5(6) . . . . ?
C73B C74B C69B C70B 0.0 . . . . ?
C73B C74B C69B B3 -178.8(7) . . . . ?
C73B C72B C71B C70B 0.0 . . . . ?
C72B C71B C70B C69B 0.0 . . . . ?
C71B C70B C69B C74B 0.0 . . . . ?
C71B C70B C69B B3 178.6(8) . . . . ?
C70B C69B B3 N3 0.0(8) . . . . ?
C70B C69B B3 C68 113.6(6) . . . . ?
C70B C69B B3 C75B -124.3(7) . . . . ?
C69B C74B C73B C72B 0.0 . . . . ?
C75B C76B C77B C78B 0.0 . . . . ?
C76B C75B C80B C79B 0.0 . . . . ?
C76B C75B B3 N3 -73.1(7) . . . . ?
C76B C75B B3 C68 163.4(5) . . . . ?
C76B C75B B3 C69B 43.9(8) . . . . ?
C76B C77B C78B C79B 0.0 . . . . ?
C77B C78B C79B C80B 0.0 . . . . ?
C78B C79B C80B C75B 0.0 . . . . ?
C80B C75B C76B C77B 0.0 . . . . ?
C80B C75B B3 N3 102.0(6) . . . . ?
C80B C75B B3 C68 -21.5(8) . . . . ?
C80B C75B B3 C69B -141.0(7) . . . . ?
C76 C77 C78 C79 0.0 . . . . ?
C76 C75 B3 N3 -69.5(7) . . . . ?
C76 C75 B3 C68 172.1(6) . . . . ?
C76 C75 B3 C69 47.2(8) . . . . ?
C77 C76 C75 C80 0.0 . . . . ?
C77 C76 C75 B3 -171.5(8) . . . . ?
C77 C78 C79 C80 0.0 . . . . ?
C78 C79 C80 C75 0.0 . . . . ?
C79 C80 C75 C76 0.0 . . . . ?
C79 C80 C75 B3 172.0(8) . . . . ?
C80 C75 B3 N3 118.8(4) . . . . ?
C80 C75 B3 C68 0.3(6) . . . . ?
C80 C75 B3 C69 -124.6(5) . . . . ?
C75 C76 C77 C78 0.0 . . . . ?
C81 N3 C85 C84 2.7(8) . . . . ?
C81 N3 B3 C68 123.7(4) . . . . ?
C81 N3 B3 C69 -114.6(4) . . . . ?
C81 N3 B3 C69B -125.4(5) . . . . ?
C81 N3 B3 C75B -0.7(6) . . . . ?
C81 N3 B3 C75 3.8(6) . . . . ?
C81 C82 C83 C84 1.2(7) . . . . ?
C82 C83 C84 C85 -1.2(8) . . . . ?
C83 C84 C85 N3 -0.9(9) . . . . ?
C85 N3 C81 C82 -2.6(6) . . . . ?
C85 N3 B3 C68 -60.4(5) . . . . ?
C85 N3 B3 C69 61.3(5) . . . . ?
C85 N3 B3 C69B 50.6(6) . . . . ?
C85 N3 B3 C75B 175.2(6) . . . . ?
C85 N3 B3 C75 179.7(5) . . . . ?
C86 C57 C58 C59 175.6(3) . . . . ?
C86 C87 B4 N4 -84.4(16) . . . . ?
C86 C87 B4 C88 29.0(17) . . . . ?
C86 C87 B4 C94 157.3(15) . . . . ?
C88 C89 C90 C91 1.8(8) . . . . ?
C89 C88 C93 C92 -1.2(6) . . . . ?
C89 C88 B4 N4 -104.1(4) . . . . ?
C89 C88 B4 C87 143.1(4) . . . . ?
C89 C88 B4 C94 13.3(5) . . . . ?
C89 C90 C91 C92 -1.6(8) . . . . ?
C90 C91 C92 C93 0.0(7) . . . . ?
C91 C92 C93 C88 1.4(6) . . . . ?
C93 C88 C89 C90 -0.4(6) . . . . ?
C93 C88 B4 N4 72.6(4) . . . . ?
C93 C88 B4 C87 -40.3(4) . . . . ?
C93 C88 B4 C94 -170.0(3) . . . . ?
C94 C95 C96 C97 -2.4(8) . . . . ?
C95 C94 C99 C98 -2.0(5) . . . . ?
C95 C94 B4 N4 174.7(3) . . . . ?
C95 C94 B4 C87 -68.1(5) . . . . ?
C95 C94 B4 C88 58.0(4) . . . . ?
C95 C96 C97 C98 0.1(7) . . . . ?
C96 C97 C98 C99 1.1(6) . . . . ?
C97 C98 C99 C94 -0.1(6) . . . . ?
C99 C94 C95 C96 3.2(6) . . . . ?
C99 C94 B4 N4 2.5(5) . . . . ?
C99 C94 B4 C87 119.7(4) . . . . ?
C99 C94 B4 C88 -114.1(4) . . . . ?
C100 N4 C104 C103 -0.4(6) . . . . ?
C100 N4 B4 C87 148.0(3) . . . . ?
C100 N4 B4 C88 32.8(5) . . . . ?
C100 N4 B4 C94 -88.3(4) . . . . ?
C100 C101 C102 C103 0.6(7) . . . . ?
C101 C102 C103 C104 -0.4(8) . . . . ?
C102 C103 C104 N4 0.4(7) . . . . ?
C104 N4 C100 C101 0.6(6) . . . . ?
C104 N4 B4 C87 -38.0(5) . . . . ?
C104 N4 B4 C88 -153.2(3) . . . . ?
C104 N4 B4 C94 85.6(4) . . . . ?
B1 N1 C29 C30 -179.2(4) . . . . ?
B1 N1 C33 C32 -179.8(5) . . . . ?
B1 C17 C18 C19 -177.1(4) . . . . ?
B1 C17 C22 C21 178.0(4) . . . . ?
B1 C23 C24 C25 179.9(4) . . . . ?
B1 C23 C28 C27 -179.9(4) . . . . ?
B2 N2 C48 C49 176.6(3) . . . . ?
B2 N2 C52 C51 -177.0(3) . . . . ?
B2 C36 C37 C38 180.0(3) . . . . ?
B2 C36 C41 C40 -179.7(3) . . . . ?
B2 C42 C43 C44 171.7(6) . . . . ?
B2 C42 C47 C46 -170.2(6) . . . . ?
B2 C42B C47B C46B 165.0(15) . . . . ?
B2 C42B C43B C44B -166.0(14) . . . . ?
B3 N3 C81 C82 173.4(4) . . . . ?
B3 N3 C85 C84 -173.4(5) . . . . ?
B3 C69 C70 C71 173.0(5) . . . . ?
B3 C69 C74 C73 -173.0(6) . . . . ?
B3 C75B C76B C77B 175.5(9) . . . . ?
B3 C75B C80B C79B -174.8(10) . . . . ?
B4 N4 C100 C101 174.6(4) . . . . ?
B4 N4 C104 C103 -174.5(4) . . . . ?
B4 C88 C89 C90 176.5(4) . . . . ?
B4 C88 C93 C92 -178.1(3) . . . . ?
B4 C94 C95 C96 -170.0(4) . . . . ?
B4 C94 C99 C98 170.7(4) . . . . ?

_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 -0.338 0.000 0.500 1446.1 291.4 ?
2 -0.757 0.500 0.000 1446.1 291.4 ?

_olex2_date_sample_data_collection 2018-06-08
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.159
_oxdiff_exptl_absorpt_empirical_full_min 0.516
####################################################################### 
# 
# 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_10b
_database_code_depnum_ccdc_archive 'CCDC 1952353'
loop_
_audit_author_name
_audit_author_address
'Hans Georg Stammler'
;University of Bielefeld
Germany
;
_audit_update_record             
;
2019-09-09 deposited with the CCDC.	2021-05-06 downloaded from the CCDC.
;
# measured as niermeier97
_audit_creation_date             2019-06-18
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
philipp.niemeier@uni-bielefeld.de
georg.stammler@uni-bielefeld.de
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C84 H68 B4 N4, 5.62(C2 H3 N)'
_chemical_formula_sum            'C95.25 H84.87 B4 N9.62'
_chemical_formula_weight         1407.49
_chemical_melting_point          ?
_chemical_oxdiff_formula         C95H84.5B4N9.5
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'
B B 0.0090 0.0039 '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      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   19.2454(7)
_cell_length_b                   28.1544(12)
_cell_length_c                   29.7705(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     16130.9(11)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    4594
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      71.8200
_cell_measurement_theta_min      3.1000
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.518
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.869
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.54a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             5950
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.0221
0 1 0 0.0093
1 0 1 0.0518
-1 0 -1 0.0764
0 -1 -1 0.0546
-1 0 0 0.0824
1 0 0 0.0649
1 1 -1 0.0640
1 0 -1 0.0743
-1 0 1 0.0628
0 0 -1 0.0856
-8 11 -10 0.0574

_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.031
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
-0.0018 -0.9994 -0.0005 0.0035 0.0399 0.0373
0.0018 0.9994 0.0005 -0.0035 -0.0399 -0.0373
0.9984 -0.0000 1.0009 0.0554 -0.0556 0.0539
-0.9984 0.0000 -1.0009 -0.0554 0.0556 -0.0539
-0.0004 -1.0005 -1.0009 -0.0481 0.0406 0.0414
-0.9998 0.0011 -0.0004 -0.0038 0.0549 -0.0581
0.9998 -0.0011 0.0004 0.0038 -0.0549 0.0581
1.0030 0.9972 -0.9995 -0.0513 -0.0940 0.0249
1.0012 -0.0022 -1.0000 -0.0478 -0.0541 0.0622
-1.0012 0.0022 1.0000 0.0478 0.0541 -0.0622
0.0014 -0.0011 -1.0004 -0.0516 0.0007 0.0041
-7.7824 10.5459 -10.1811 -0.5924 0.0159 -0.8055

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1485
_diffrn_reflns_av_unetI/netI     0.1206
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            54697
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.080
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         3.139
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      5.00  32.00   1.00   20.00    --  -38.50  38.00-150.00   27
  2  ω    -59.00  33.00   1.00   20.00    --  -38.50  38.00-180.00   92
  3  ω   -104.00 -64.00   1.00   20.00    --  -38.50-148.00 154.00   40
  4  ω     43.00  78.00   1.00   20.00    --   42.89 -99.00 150.00   35
  5  ω     95.00 121.00   1.00   80.00    --  106.24 -30.00-150.00   26
  6  ω     44.00 125.00   1.00   80.00    --  106.24 -45.00  60.00   81
  7  ω     39.00 111.00   1.00   80.00    --  106.24-125.00 -60.00   72
  8  ω     94.00 143.00   1.00   80.00    --  106.24 125.00-150.00   49
  9  ω     88.00 114.00   1.00   80.00    --  106.24-125.00  90.00   26
 10  ω     95.00 174.00   1.00   80.00    --  106.24 125.00 120.00   79
 11  ω     61.00 121.00   1.00   80.00    --  106.24 -77.00 120.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0037914000
_diffrn_orient_matrix_UB_12      -0.0035416000
_diffrn_orient_matrix_UB_13      0.0516179000
_diffrn_orient_matrix_UB_21      -0.0549323000
_diffrn_orient_matrix_UB_22      -0.0397855000
_diffrn_orient_matrix_UB_23      -0.0007842000
_diffrn_orient_matrix_UB_31      0.0580244000
_diffrn_orient_matrix_UB_32      -0.0374094000
_diffrn_orient_matrix_UB_33      -0.0039861000
_diffrn_oxdiff_digest_frames     
;
0105d0afcf403cd35decececa777ce7085005916eb1
;
_diffrn_oxdiff_digest_hkl        
;
01012b5f159d32d95cab87ea9cc4a075b1a4d8
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8076
_reflns_number_total             14388
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.54a (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         0.284
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.00016(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1081
_refine_ls_number_reflns         14388
_refine_ls_number_restraints     90
_refine_ls_R_factor_all          0.1349
_refine_ls_R_factor_gt           0.0687
_refine_ls_restrained_S_all      1.011
_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)+(0.0894P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1662
_refine_ls_wR_factor_ref         0.2177
_refine_special_details          
'Hydrogen atoms bonded to carbon were taken into account using a riding model, those ones bonded to nitrogen were refined isotropically. Ca. 5.6 molecules of acetonitrile were found per molecule. The occupation factors  of these solvent molecules were refined,atoms of molecules with occupation below 25% were refined isotropically, all others anisotropically.'
_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. Restrained distances
 N11-C97 \\sim N7B-C89B \\sim N13-C99 \\sim N10-C95 \\sim N6-C87A \\sim N6-C87B
\\sim N5-C85 \\sim N8-C91
 \\sim N9-C93 \\sim N7-C89
 with sigma of 0.02
 C97-C98 \\sim C89B-C90B \\sim C90-C89 \\sim C100-C99 \\sim C95-C96 \\sim
C87A-C88A \\sim C87B-C88B ~
 C86-C85 \\sim C92-C91 \\sim C94-C93
 with sigma of 0.02
3. Others
 Sof(C87B)=Sof(C88B)=Sof(H88D)=Sof(H88E)=Sof(H88F)=Sof(N10)=Sof(C95)=Sof(C96)=
 Sof(H96A)=Sof(H96B)=Sof(H96C)=1-FVAR(1)
 Sof(C87A)=Sof(C88A)=Sof(H88A)=Sof(H88B)=Sof(H88C)=FVAR(1)
 Sof(N7B)=Sof(C89B)=Sof(C90B)=Sof(H90D)=Sof(H90E)=Sof(H90F)=Sof(N11)=Sof(C97)=
 Sof(C98)=Sof(H98A)=Sof(H98B)=Sof(H98C)=Sof(N13)=Sof(C99)=Sof(C100)=Sof(H10A)=
 Sof(H10B)=Sof(H10C)=1-FVAR(2)
 Sof(N7)=Sof(C89)=Sof(C90)=Sof(H90A)=Sof(H90B)=Sof(H90C)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C3(H3), C10(H10), C45(H45), C52(H52)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14), C18(H18), C19(H19),
 C20(H20), C21(H21), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28),
  C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
 C40(H40), C41(H41), C42(H42), C48(H48), C49(H49), C50(H50), C54(H54), C55(H55),
  C56(H56), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C66(H66),
 C67(H67), C68(H68), C69(H69), C70(H70), C74(H74), C75(H75), C76(H76), C77(H77),
  C78(H78), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84)
4.c Idealised Me refined as rotating group:
 C86(H86A,H86B,H86C), C88A(H88A,H88B,H88C), C88B(H88D,H88E,H88F), C90(H90A,
 H90B,H90C), C90B(H90D,H90E,H90F), C92(H92A,H92B,H92C), C94(H94A,H94B,H94C),
 C96(H96A,H96B,H96C), C98(H98A,H98B,H98C), C100(H10A,H10B,H10C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.72795(18) 0.75469(12) 0.64824(11) 0.0305(7) Uani 1 1 d . . . . .
H1A H 0.705(2) 0.7356(17) 0.6277(15) 0.039(12) Uiso 1 1 d . . . . .
H1B H 0.689(3) 0.767(2) 0.6683(19) 0.071(17) Uiso 1 1 d . . . . .
H1C H 0.742(3) 0.783(2) 0.635(2) 0.079(19) Uiso 1 1 d . . . . .
N2 N 0.54975(17) 0.68906(13) 0.55985(11) 0.0336(7) Uani 1 1 d . . . . .
H2A H 0.556(3) 0.708(2) 0.530(2) 0.081(19) Uiso 1 1 d . . . . .
H2B H 0.593(3) 0.677(2) 0.5696(18) 0.068(17) Uiso 1 1 d . . . . .
H2C H 0.528(3) 0.662(2) 0.5452(17) 0.058(15) Uiso 1 1 d . . . . .
N3 N 0.83738(19) 0.58244(13) 0.57604(12) 0.0362(8) Uani 1 1 d . . . . .
H3A H 0.858(2) 0.5917(16) 0.5486(15) 0.035(11) Uiso 1 1 d . . . . .
H3B H 0.856(3) 0.603(3) 0.601(2) 0.09(2) Uiso 1 1 d . . . . .
H3C H 0.788(3) 0.5929(19) 0.5722(17) 0.058(15) Uiso 1 1 d . . . . .
N4 N 0.62213(16) 0.50623(11) 0.50995(10) 0.0254(6) Uani 1 1 d . . . . .
H4A H 0.635(2) 0.5163(19) 0.4772(18) 0.056(14) Uiso 1 1 d . . . . .
H4B H 0.665(3) 0.4957(17) 0.5233(16) 0.046(13) Uiso 1 1 d . . . . .
H4C H 0.590(3) 0.481(2) 0.5052(18) 0.066(16) Uiso 1 1 d . . . . .
C1 C 0.70179(17) 0.63222(12) 0.77021(10) 0.0200(7) Uani 1 1 d . . . . .
C2 C 0.64939(16) 0.59759(12) 0.76771(10) 0.0184(6) Uani 1 1 d . . . . .
C3 C 0.61169(16) 0.58419(12) 0.72481(10) 0.0193(7) Uani 1 1 d . . . . .
H3 H 0.623250 0.608159 0.701173 0.023 Uiso 1 1 calc R . . . .
C4 C 0.53441(16) 0.58711(12) 0.73475(11) 0.0202(7) Uani 1 1 d . . . . .
C5 C 0.48673(17) 0.61308(12) 0.70905(11) 0.0231(7) Uani 1 1 d . . . . .
C6 C 0.41592(18) 0.61172(13) 0.72168(13) 0.0286(8) Uani 1 1 d . . . . .
H6 H 0.382885 0.629042 0.704539 0.034 Uiso 1 1 calc R . . . .
C7 C 0.39373(18) 0.58589(14) 0.75822(12) 0.0291(8) Uani 1 1 d . . . . .
H7 H 0.345621 0.584311 0.765209 0.035 Uiso 1 1 calc R . . . .
C8 C 0.44181(18) 0.56208(13) 0.78494(11) 0.0258(7) Uani 1 1 d . . . . .
H8 H 0.426783 0.544993 0.810686 0.031 Uiso 1 1 calc R . . . .
C9 C 0.51168(17) 0.56342(12) 0.77379(11) 0.0205(7) Uani 1 1 d . . . . .
C10 C 0.56679(17) 0.54143(12) 0.80381(10) 0.0204(7) Uani 1 1 d . . . . .
H10 H 0.546174 0.537271 0.834391 0.025 Uiso 1 1 calc R . . . .
C11 C 0.62604(17) 0.57617(12) 0.80769(10) 0.0202(7) Uani 1 1 d . . . . .
C12 C 0.65461(19) 0.58825(13) 0.84882(11) 0.0270(8) Uani 1 1 d . . . . .
H12 H 0.638198 0.573660 0.875566 0.032 Uiso 1 1 calc R . . . .
C13 C 0.70781(19) 0.62210(13) 0.85076(12) 0.0292(8) Uani 1 1 d . . . . .
H13 H 0.728123 0.630276 0.878795 0.035 Uiso 1 1 calc R . . . .
C14 C 0.73048(18) 0.64342(13) 0.81197(10) 0.0233(7) Uani 1 1 d . . . . .
H14 H 0.766597 0.666358 0.813576 0.028 Uiso 1 1 calc R . . . .
C15 C 0.72565(17) 0.65960(12) 0.73210(11) 0.0222(7) Uani 1 1 d . . . . .
C16 C 0.75103(18) 0.68868(13) 0.70723(11) 0.0256(7) Uani 1 1 d . . . . .
C17 C 0.8129(2) 0.77122(14) 0.71441(12) 0.0315(8) Uani 1 1 d . . . . .
C18 C 0.8810(2) 0.78814(15) 0.71584(14) 0.0373(9) Uani 1 1 d . . . . .
H18 H 0.914509 0.775448 0.695738 0.045 Uiso 1 1 calc R . . . .
C19 C 0.9007(3) 0.82333(17) 0.74621(17) 0.0516(12) Uani 1 1 d . . . . .
H19 H 0.947607 0.833785 0.746957 0.062 Uiso 1 1 calc R . . . .
C20 C 0.8530(3) 0.8431(2) 0.77512(18) 0.0648(15) Uani 1 1 d . . . . .
H20 H 0.866929 0.867159 0.795616 0.078 Uiso 1 1 calc R . . . .
C21 C 0.7847(3) 0.8278(2) 0.77421(18) 0.0662(16) Uani 1 1 d . . . . .
H21 H 0.751292 0.841734 0.793649 0.079 Uiso 1 1 calc R . . . .
C22 C 0.7652(3) 0.79167(17) 0.74448(15) 0.0476(12) Uani 1 1 d . . . . .
H22 H 0.718478 0.780699 0.744638 0.057 Uiso 1 1 calc R . . . .
C23 C 0.84995(19) 0.71179(13) 0.64758(11) 0.0268(8) Uani 1 1 d . . . . .
C24 C 0.8754(2) 0.73745(17) 0.61109(13) 0.0409(10) Uani 1 1 d . . . . .
H24 H 0.852359 0.765937 0.602649 0.049 Uiso 1 1 calc R . . . .
C25 C 0.9331(2) 0.72303(19) 0.58653(15) 0.0489(12) Uani 1 1 d . . . . .
H25 H 0.948768 0.741692 0.561955 0.059 Uiso 1 1 calc R . . . .
C26 C 0.9677(2) 0.68174(19) 0.59767(14) 0.0482(11) Uani 1 1 d . . . . .
H26 H 1.007109 0.671646 0.580976 0.058 Uiso 1 1 calc R . . . .
C27 C 0.9439(3) 0.65562(18) 0.63342(16) 0.0511(12) Uani 1 1 d . . . . .
H27 H 0.967521 0.627338 0.641803 0.061 Uiso 1 1 calc R . . . .
C28 C 0.8858(2) 0.66999(15) 0.65753(14) 0.0382(9) Uani 1 1 d . . . . .
H28 H 0.869831 0.650702 0.681609 0.046 Uiso 1 1 calc R . . . .
C29 C 0.50476(17) 0.64234(12) 0.67117(12) 0.0244(7) Uani 1 1 d . . . . .
C30 C 0.50902(17) 0.67054(13) 0.64058(12) 0.0278(8) Uani 1 1 d . . . . .
C31 C 0.5462(2) 0.75858(15) 0.61867(14) 0.0353(9) Uani 1 1 d . . . . .
C32 C 0.5805(3) 0.78952(18) 0.58917(18) 0.0534(12) Uani 1 1 d . . . . .
H32 H 0.584093 0.781192 0.558337 0.064 Uiso 1 1 calc R . . . .
C33 C 0.6096(3) 0.8323(2) 0.6039(2) 0.0661(16) Uani 1 1 d . . . . .
H33 H 0.632176 0.852480 0.582910 0.079 Uiso 1 1 calc R . . . .
C34 C 0.6060(2) 0.84532(17) 0.6476(2) 0.0549(13) Uani 1 1 d . . . . .
H34 H 0.626556 0.874162 0.657486 0.066 Uiso 1 1 calc R . . . .
C35 C 0.5720(2) 0.81606(17) 0.67763(18) 0.0510(11) Uani 1 1 d . . . . .
H35 H 0.568599 0.824923 0.708343 0.061 Uiso 1 1 calc R . . . .
C36 C 0.5423(2) 0.77327(15) 0.66290(15) 0.0398(10) Uani 1 1 d . . . . .
H36 H 0.518820 0.753741 0.684031 0.048 Uiso 1 1 calc R . . . .
C37 C 0.42962(19) 0.72026(14) 0.58560(13) 0.0308(8) Uani 1 1 d . . . . .
C38 C 0.3726(2) 0.71554(17) 0.61405(16) 0.0444(11) Uani 1 1 d . . . . .
H38 H 0.379929 0.705920 0.644260 0.053 Uiso 1 1 calc R . . . .
C39 C 0.3050(2) 0.72453(19) 0.59949(18) 0.0550(14) Uani 1 1 d . . . . .
H39 H 0.267401 0.720718 0.619848 0.066 Uiso 1 1 calc R . . . .
C40 C 0.2920(2) 0.73868(17) 0.55655(18) 0.0510(12) Uani 1 1 d . . . . .
H40 H 0.245765 0.744541 0.546849 0.061 Uiso 1 1 calc R . . . .
C41 C 0.3469(2) 0.74433(17) 0.52747(15) 0.0464(11) Uani 1 1 d . . . . .
H41 H 0.338704 0.754181 0.497411 0.056 Uiso 1 1 calc R . . . .
C42 C 0.4144(2) 0.73563(17) 0.54205(14) 0.0407(10) Uani 1 1 d . . . . .
H42 H 0.451595 0.740326 0.521580 0.049 Uiso 1 1 calc R . . . .
C43 C 0.75681(17) 0.50172(12) 0.71725(10) 0.0203(7) Uani 1 1 d . . . . .
C44 C 0.68864(16) 0.50837(12) 0.73346(10) 0.0200(7) Uani 1 1 d . . . . .
C45 C 0.63157(16) 0.53201(12) 0.70613(11) 0.0211(7) Uani 1 1 d . . . . .
H45 H 0.648951 0.535752 0.674675 0.025 Uiso 1 1 calc R . . . .
C46 C 0.57104(16) 0.49690(12) 0.70516(10) 0.0182(7) Uani 1 1 d . . . . .
C47 C 0.53709(16) 0.48343(12) 0.66576(10) 0.0183(6) Uani 1 1 d . . . . .
C48 C 0.48655(18) 0.44712(13) 0.66758(12) 0.0251(7) Uani 1 1 d . . . . .
H48 H 0.463246 0.437764 0.640879 0.030 Uiso 1 1 calc R . . . .
C49 C 0.47050(17) 0.42496(13) 0.70783(12) 0.0252(7) Uani 1 1 d . . . . .
H49 H 0.437189 0.400066 0.708484 0.030 Uiso 1 1 calc R . . . .
C50 C 0.50311(17) 0.43914(12) 0.74719(11) 0.0225(7) Uani 1 1 d . . . . .
H50 H 0.491391 0.424450 0.774902 0.027 Uiso 1 1 calc R . . . .
C51 C 0.55303(16) 0.47493(12) 0.74603(10) 0.0189(7) Uani 1 1 d . . . . .
C52 C 0.59274(17) 0.49058(12) 0.78687(11) 0.0207(7) Uani 1 1 d . . . . .
H52 H 0.584339 0.467000 0.811394 0.025 Uiso 1 1 calc R . . . .
C53 C 0.66942(17) 0.48926(12) 0.77476(10) 0.0194(7) Uani 1 1 d . . . . .
C54 C 0.71723(18) 0.46580(13) 0.80120(11) 0.0250(7) Uani 1 1 d . . . . .
H54 H 0.703635 0.453385 0.829544 0.030 Uiso 1 1 calc R . . . .
C55 C 0.78576(18) 0.46028(14) 0.78634(12) 0.0285(8) Uani 1 1 d . . . . .
H55 H 0.819023 0.444656 0.804709 0.034 Uiso 1 1 calc R . . . .
C56 C 0.80461(18) 0.47775(13) 0.74472(12) 0.0260(7) Uani 1 1 d . . . . .
H56 H 0.850937 0.473449 0.734475 0.031 Uiso 1 1 calc R . . . .
C57 C 0.77797(16) 0.51486(13) 0.67295(11) 0.0221(7) Uani 1 1 d . . . . .
C58 C 0.80156(17) 0.52123(13) 0.63527(12) 0.0251(8) Uani 1 1 d . . . . .
C59 C 0.80465(17) 0.49671(14) 0.54819(11) 0.0264(8) Uani 1 1 d . . . . .
C60 C 0.80395(19) 0.51157(17) 0.50348(12) 0.0345(9) Uani 1 1 d . . . . .
H60 H 0.817836 0.543142 0.496665 0.041 Uiso 1 1 calc R . . . .
C61 C 0.7837(2) 0.4819(2) 0.46855(14) 0.0463(12) Uani 1 1 d . . . . .
H61 H 0.783609 0.493350 0.438540 0.056 Uiso 1 1 calc R . . . .
C62 C 0.7639(2) 0.4364(2) 0.47732(14) 0.0492(13) Uani 1 1 d . . . . .
H62 H 0.750610 0.416064 0.453360 0.059 Uiso 1 1 calc R . . . .
C63 C 0.7631(2) 0.41978(19) 0.52090(15) 0.0462(11) Uani 1 1 d . . . . .
H63 H 0.749336 0.388042 0.527053 0.055 Uiso 1 1 calc R . . . .
C64 C 0.7826(2) 0.44982(16) 0.55574(14) 0.0364(9) Uani 1 1 d . . . . .
H64 H 0.781057 0.438227 0.585688 0.044 Uiso 1 1 calc R . . . .
C65 C 0.91986(18) 0.50965(14) 0.59154(12) 0.0278(8) Uani 1 1 d . . . . .
C66 C 0.9723(2) 0.52937(18) 0.56482(14) 0.0422(10) Uani 1 1 d . . . . .
H66 H 0.961957 0.556294 0.546780 0.051 Uiso 1 1 calc R . . . .
C67 C 1.0392(2) 0.5105(2) 0.56401(16) 0.0511(12) Uani 1 1 d . . . . .
H67 H 1.074208 0.525140 0.546266 0.061 Uiso 1 1 calc R . . . .
C68 C 1.0545(2) 0.47058(18) 0.58903(14) 0.0413(11) Uani 1 1 d . . . . .
H68 H 1.099663 0.456991 0.587784 0.050 Uiso 1 1 calc R . . . .
C69 C 1.0041(2) 0.45055(16) 0.61578(14) 0.0378(9) Uani 1 1 d . . . . .
H69 H 1.014380 0.423194 0.633246 0.045 Uiso 1 1 calc R . . . .
C70 C 0.93807(18) 0.47050(14) 0.61714(13) 0.0314(8) Uani 1 1 d . . . . .
H70 H 0.904157 0.456763 0.636348 0.038 Uiso 1 1 calc R . . . .
C71 C 0.55475(17) 0.50470(13) 0.62357(11) 0.0223(7) Uani 1 1 d . . . . .
C72 C 0.56995(17) 0.52215(13) 0.58763(11) 0.0247(7) Uani 1 1 d . . . . .
C73 C 0.52054(17) 0.56918(13) 0.51766(11) 0.0240(7) Uani 1 1 d . . . . .
C74 C 0.51412(19) 0.57622(14) 0.47192(12) 0.0287(8) Uani 1 1 d . . . . .
H74 H 0.548438 0.563213 0.452558 0.034 Uiso 1 1 calc R . . . .
C75 C 0.4589(2) 0.60185(15) 0.45292(13) 0.0352(9) Uani 1 1 d . . . . .
H75 H 0.456050 0.605826 0.421281 0.042 Uiso 1 1 calc R . . . .
C76 C 0.4086(2) 0.62126(15) 0.48050(14) 0.0365(9) Uani 1 1 d . . . . .
H76 H 0.371845 0.639535 0.468021 0.044 Uiso 1 1 calc R . . . .
C77 C 0.4120(2) 0.61396(15) 0.52611(14) 0.0359(9) Uani 1 1 d . . . . .
H77 H 0.376893 0.626567 0.545104 0.043 Uiso 1 1 calc R . . . .
C78 C 0.46657(18) 0.58825(15) 0.54451(12) 0.0304(8) Uani 1 1 d . . . . .
H78 H 0.467748 0.583287 0.576066 0.036 Uiso 1 1 calc R . . . .
C79 C 0.64532(16) 0.58916(12) 0.54816(10) 0.0198(7) Uani 1 1 d . . . . .
C80 C 0.67537(19) 0.61241(14) 0.51144(11) 0.0282(8) Uani 1 1 d . . . . .
H80 H 0.666141 0.600811 0.482076 0.034 Uiso 1 1 calc R . . . .
C81 C 0.71808(19) 0.65171(14) 0.51626(12) 0.0308(8) Uani 1 1 d . . . . .
H81 H 0.737755 0.666364 0.490484 0.037 Uiso 1 1 calc R . . . .
C82 C 0.73198(18) 0.66948(13) 0.55827(12) 0.0282(8) Uani 1 1 d . . . . .
H82 H 0.760087 0.696997 0.561590 0.034 Uiso 1 1 calc R . . . .
C83 C 0.70453(18) 0.64687(13) 0.59609(12) 0.0268(8) Uani 1 1 d . . . . .
H83 H 0.714832 0.658325 0.625360 0.032 Uiso 1 1 calc R . . . .
C84 C 0.66166(17) 0.60711(12) 0.59037(11) 0.0232(7) Uani 1 1 d . . . . .
H84 H 0.643119 0.591893 0.616211 0.028 Uiso 1 1 calc R . . . .
B1 B 0.7880(2) 0.73004(15) 0.67930(13) 0.0262(9) Uani 1 1 d . . . . .
B2 B 0.5086(2) 0.70999(17) 0.60213(15) 0.0317(10) Uani 1 1 d . . . . .
B3 B 0.8394(2) 0.52682(16) 0.58829(13) 0.0272(9) Uani 1 1 d . . . . .
B4 B 0.58838(19) 0.54689(15) 0.54193(12) 0.0218(8) Uani 1 1 d . . . . .
N5 N 0.7880(2) 0.84491(14) 0.60789(14) 0.0494(10) Uani 1 1 d D . . . .
C85 C 0.8048(2) 0.87162(15) 0.63477(15) 0.0389(10) Uani 1 1 d D . . . .
C86 C 0.8253(3) 0.90629(18) 0.66815(19) 0.0564(13) Uani 1 1 d D . . . .
H86A H 0.818108 0.938346 0.656209 0.085 Uiso 1 1 calc GR . . . .
H86B H 0.874552 0.901940 0.675518 0.085 Uiso 1 1 calc GR . . . .
H86C H 0.797236 0.902036 0.695304 0.085 Uiso 1 1 calc GR . . . .
N6 N 0.5840(3) 0.7315(3) 0.47002(18) 0.091(2) Uani 1 1 d D . . . .
C87A C 0.5990(4) 0.7075(4) 0.4392(3) 0.106(4) Uani 0.866(7) 1 d D . P A 1
C87B C 0.598(2) 0.7454(18) 0.4348(8) 0.071(13) Uiso 0.134(7) 1 d D . P A 2
C88A C 0.6174(8) 0.6741(4) 0.4016(3) 0.151(6) Uani 0.866(7) 1 d D . P A 1
H88A H 0.589901 0.681964 0.374912 0.226 Uiso 0.866(7) 1 calc GR . P A 1
H88B H 0.607295 0.641356 0.410806 0.226 Uiso 0.866(7) 1 calc GR . P A 1
H88C H 0.666955 0.677041 0.394579 0.226 Uiso 0.866(7) 1 calc GR . P A 1
C88B C 0.617(3) 0.763(2) 0.3901(11) 0.101(19) Uiso 0.134(7) 1 d D . P A 2
H88D H 0.665313 0.754144 0.383464 0.151 Uiso 0.134(7) 1 calc GR . P A 2
H88E H 0.612779 0.797741 0.389491 0.151 Uiso 0.134(7) 1 calc GR . P A 2
H88F H 0.586231 0.749133 0.367538 0.151 Uiso 0.134(7) 1 calc GR . P A 2
N7 N 0.8917(4) 0.6248(2) 0.48773(19) 0.0504(15) Uani 0.755(4) 1 d D . P B 1
C89 C 0.8956(3) 0.6392(2) 0.45138(19) 0.0432(15) Uani 0.755(4) 1 d D . P B 1
C90 C 0.8984(4) 0.6563(2) 0.4049(2) 0.0553(19) Uani 0.755(4) 1 d D . P B 1
H90A H 0.875099 0.633430 0.385171 0.083 Uiso 0.755(4) 1 calc GR . P B 1
H90B H 0.946981 0.659786 0.395615 0.083 Uiso 0.755(4) 1 calc GR . P B 1
H90C H 0.874931 0.687126 0.402803 0.083 Uiso 0.755(4) 1 calc GR . P B 1
N7B N 0.9236(8) 0.6276(7) 0.4962(6) 0.037(5) Uiso 0.245(4) 1 d D . P B 3
C89B C 0.9816(7) 0.6218(6) 0.4937(5) 0.030(3) Uiso 0.245(4) 1 d D . P B 3
C90B C 1.0571(8) 0.6147(9) 0.4924(8) 0.051(5) Uiso 0.245(4) 1 d D . P B 3
H90D H 1.070005 0.599697 0.463876 0.076 Uiso 0.245(4) 1 calc GR . P B 3
H90E H 1.071093 0.594123 0.517368 0.076 Uiso 0.245(4) 1 calc GR . P B 3
H90F H 1.080493 0.645438 0.495060 0.076 Uiso 0.245(4) 1 calc GR . P B 3
N8 N 0.6546(2) 0.5303(2) 0.40989(13) 0.0650(14) Uani 1 1 d D . . . .
C91 C 0.6485(2) 0.4980(2) 0.38617(15) 0.0506(13) Uani 1 1 d D . . . .
C92 C 0.6390(3) 0.45762(19) 0.35625(17) 0.0559(13) Uani 1 1 d D . . . .
H92A H 0.630536 0.428913 0.374050 0.084 Uiso 1 1 calc GR . . . .
H92B H 0.680909 0.453276 0.338016 0.084 Uiso 1 1 calc GR . . . .
H92C H 0.599140 0.463484 0.336515 0.084 Uiso 1 1 calc GR . . . .
N9 N 0.5835(3) 0.79291(18) 0.79757(18) 0.0735(14) Uani 1 1 d D . . . .
C93 C 0.5694(3) 0.75441(18) 0.78905(18) 0.0533(12) Uani 1 1 d D . . . .
C94 C 0.5518(3) 0.70595(18) 0.7771(2) 0.0647(15) Uani 1 1 d D . . . .
H94A H 0.576721 0.696962 0.749648 0.097 Uiso 1 1 calc GR . . . .
H94B H 0.501637 0.703562 0.771891 0.097 Uiso 1 1 calc GR . . . .
H94C H 0.565153 0.684571 0.801576 0.097 Uiso 1 1 calc GR . . . .
N10 N 0.7781(13) 0.6054(11) 0.3997(10) 0.036(8) Uiso 0.134(7) 1 d D . P A 2
C95 C 0.7245(16) 0.6230(14) 0.3937(13) 0.053(10) Uiso 0.134(7) 1 d D . P A 2
C96 C 0.655(2) 0.643(3) 0.387(3) 0.15(3) Uiso 0.134(7) 1 d D . P A 2
H96A H 0.644012 0.642859 0.354705 0.229 Uiso 0.134(7) 1 calc GR . P A 2
H96B H 0.654311 0.675948 0.397903 0.229 Uiso 0.134(7) 1 calc GR . P A 2
H96C H 0.620829 0.624224 0.403227 0.229 Uiso 0.134(7) 1 calc GR . P A 2
N11 N 1.1200(19) 0.6620(12) 0.5313(12) 0.149(13) Uiso 0.245(4) 1 d D . P B 4
C97 C 1.0936(16) 0.6317(10) 0.5113(9) 0.087(8) Uiso 0.245(4) 1 d D . P B 4
C98 C 1.0622(11) 0.5970(9) 0.4811(8) 0.055(6) Uiso 0.245(4) 1 d D . P B 4
H98A H 1.065338 0.608607 0.450102 0.082 Uiso 0.245(4) 1 calc GR . P B 4
H98B H 1.013310 0.592473 0.489160 0.082 Uiso 0.245(4) 1 calc GR . P B 4
H98C H 1.086945 0.566717 0.483645 0.082 Uiso 0.245(4) 1 calc GR . P B 4
N13 N 0.7671(13) 0.6175(12) 0.3936(11) 0.092(10) Uiso 0.245(4) 1 d D . P B 3
C99 C 0.8204(10) 0.6368(8) 0.3924(7) 0.057(5) Uiso 0.245(4) 1 d D . P B 3
C100 C 0.8848(12) 0.6629(10) 0.3839(10) 0.071(8) Uiso 0.245(4) 1 d D . P B 3
H10A H 0.879422 0.682291 0.356751 0.106 Uiso 0.245(4) 1 calc GR . P B 3
H10B H 0.923100 0.640435 0.379675 0.106 Uiso 0.245(4) 1 calc GR . P B 3
H10C H 0.895026 0.683628 0.409536 0.106 Uiso 0.245(4) 1 calc GR . P B 3


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 B1 1.635(5) . ?
N2 B2 1.600(6) . ?
N3 B3 1.608(6) . ?
N4 B4 1.625(5) . ?
C1 C2 1.405(5) . ?
C1 C14 1.396(5) . ?
C1 C15 1.447(5) . ?
C2 C3 1.517(4) . ?
C2 C11 1.408(4) . ?
C3 C4 1.519(4) . ?
C3 C45 1.617(5) . ?
C4 C5 1.401(5) . ?
C4 C9 1.410(5) . ?
C5 C6 1.414(5) . ?
C5 C29 1.439(5) . ?
C6 C7 1.376(5) . ?
C7 C8 1.392(5) . ?
C8 C9 1.386(5) . ?
C9 C10 1.519(5) . ?
C10 C11 1.507(5) . ?
C10 C52 1.598(5) . ?
C11 C12 1.385(5) . ?
C12 C13 1.400(5) . ?
C13 C14 1.373(5) . ?
C15 C16 1.207(5) . ?
C16 B1 1.599(5) . ?
C17 C18 1.395(6) . ?
C17 C22 1.406(6) . ?
C17 B1 1.633(5) . ?
C18 C19 1.394(6) . ?
C19 C20 1.376(7) . ?
C20 C21 1.383(8) . ?
C21 C22 1.400(6) . ?
C23 C24 1.394(5) . ?
C23 C28 1.396(6) . ?
C23 B1 1.605(5) . ?
C24 C25 1.390(6) . ?
C25 C26 1.380(7) . ?
C26 C27 1.372(7) . ?
C27 C28 1.390(6) . ?
C29 C30 1.211(5) . ?
C30 B2 1.595(5) . ?
C31 C32 1.402(6) . ?
C31 C36 1.382(6) . ?
C31 B2 1.624(6) . ?
C32 C33 1.398(7) . ?
C33 C34 1.355(8) . ?
C34 C35 1.380(7) . ?
C35 C36 1.403(6) . ?
C37 C38 1.393(6) . ?
C37 C42 1.398(5) . ?
C37 B2 1.624(5) . ?
C38 C39 1.394(6) . ?
C39 C40 1.362(7) . ?
C40 C41 1.375(7) . ?
C41 C42 1.391(6) . ?
C43 C44 1.411(5) . ?
C43 C56 1.404(5) . ?
C43 C57 1.429(5) . ?
C44 C45 1.520(4) . ?
C44 C53 1.392(5) . ?
C45 C46 1.528(5) . ?
C46 C47 1.395(4) . ?
C46 C51 1.408(4) . ?
C47 C48 1.412(5) . ?
C47 C71 1.432(5) . ?
C48 C49 1.386(5) . ?
C49 C50 1.388(5) . ?
C50 C51 1.393(5) . ?
C51 C52 1.502(5) . ?
C52 C53 1.520(5) . ?
C53 C54 1.379(5) . ?
C54 C55 1.400(5) . ?
C55 C56 1.381(5) . ?
C57 C58 1.224(5) . ?
C58 B3 1.585(5) . ?
C59 C60 1.395(5) . ?
C59 C64 1.405(6) . ?
C59 B3 1.610(6) . ?
C60 C61 1.390(6) . ?
C61 C62 1.361(8) . ?
C62 C63 1.379(7) . ?
C63 C64 1.390(6) . ?
C65 C66 1.400(5) . ?
C65 C70 1.385(6) . ?
C65 B3 1.625(5) . ?
C66 C67 1.393(6) . ?
C67 C68 1.381(7) . ?
C68 C69 1.376(6) . ?
C69 C70 1.390(5) . ?
C71 C72 1.213(5) . ?
C72 B4 1.569(5) . ?
C73 C74 1.382(5) . ?
C73 C78 1.416(5) . ?
C73 B4 1.619(5) . ?
C74 C75 1.404(5) . ?
C75 C76 1.382(6) . ?
C76 C77 1.375(6) . ?
C77 C78 1.388(5) . ?
C79 C80 1.399(5) . ?
C79 C84 1.391(5) . ?
C79 B4 1.628(5) . ?
C80 C81 1.386(5) . ?
C81 C82 1.373(5) . ?
C82 C83 1.397(5) . ?
C83 C84 1.401(5) . ?
N5 C85 1.145(5) . ?
C85 C86 1.448(6) . ?
N6 C87A 1.177(10) . ?
N6 C87B 1.151(15) . ?
C87A C88A 1.505(11) . ?
C87B C88B 1.467(16) . ?
N7 C89 1.159(7) . ?
C89 C90 1.466(8) . ?
N7B C89B 1.131(13) . ?
C89B C90B 1.466(14) . ?
N8 C91 1.158(6) . ?
C91 C92 1.455(7) . ?
N9 C93 1.146(6) . ?
C93 C94 1.451(7) . ?
N10 C95 1.158(16) . ?
C95 C96 1.464(16) . ?
N11 C97 1.157(15) . ?
C97 C98 1.459(15) . ?
N13 C99 1.160(15) . ?
C99 C100 1.465(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C15 123.8(3) . . ?
C14 C1 C2 119.2(3) . . ?
C14 C1 C15 116.9(3) . . ?
C1 C2 C3 124.1(3) . . ?
C1 C2 C11 118.8(3) . . ?
C11 C2 C3 116.9(3) . . ?
C2 C3 C4 106.9(3) . . ?
C2 C3 C45 113.7(3) . . ?
C4 C3 C45 110.4(3) . . ?
C5 C4 C3 124.3(3) . . ?
C5 C4 C9 119.6(3) . . ?
C9 C4 C3 116.0(3) . . ?
C4 C5 C6 118.2(3) . . ?
C4 C5 C29 124.7(3) . . ?
C6 C5 C29 117.1(3) . . ?
C7 C6 C5 121.6(3) . . ?
C6 C7 C8 120.0(3) . . ?
C9 C8 C7 119.7(3) . . ?
C4 C9 C10 117.5(3) . . ?
C8 C9 C4 120.8(3) . . ?
C8 C9 C10 121.7(3) . . ?
C9 C10 C52 113.4(3) . . ?
C11 C10 C9 108.0(3) . . ?
C11 C10 C52 111.7(3) . . ?
C2 C11 C10 117.0(3) . . ?
C12 C11 C2 121.0(3) . . ?
C12 C11 C10 121.9(3) . . ?
C11 C12 C13 119.6(3) . . ?
C14 C13 C12 119.7(3) . . ?
C13 C14 C1 121.6(3) . . ?
C16 C15 C1 166.2(4) . . ?
C15 C16 B1 173.5(4) . . ?
C18 C17 C22 117.0(4) . . ?
C18 C17 B1 122.5(3) . . ?
C22 C17 B1 120.5(3) . . ?
C19 C18 C17 121.2(4) . . ?
C20 C19 C18 120.8(4) . . ?
C19 C20 C21 119.7(4) . . ?
C20 C21 C22 119.6(5) . . ?
C21 C22 C17 121.6(4) . . ?
C24 C23 C28 115.4(4) . . ?
C24 C23 B1 123.6(4) . . ?
C28 C23 B1 120.8(3) . . ?
C25 C24 C23 122.6(4) . . ?
C26 C25 C24 120.4(4) . . ?
C27 C26 C25 118.5(4) . . ?
C26 C27 C28 120.9(5) . . ?
C27 C28 C23 122.2(4) . . ?
C30 C29 C5 168.8(4) . . ?
C29 C30 B2 174.8(4) . . ?
C32 C31 B2 122.9(4) . . ?
C36 C31 C32 115.9(4) . . ?
C36 C31 B2 121.1(4) . . ?
C33 C32 C31 121.8(5) . . ?
C34 C33 C32 120.9(5) . . ?
C33 C34 C35 119.0(5) . . ?
C34 C35 C36 120.2(5) . . ?
C31 C36 C35 122.2(4) . . ?
C38 C37 C42 115.3(4) . . ?
C38 C37 B2 122.5(3) . . ?
C42 C37 B2 122.2(3) . . ?
C37 C38 C39 121.9(4) . . ?
C40 C39 C38 121.1(4) . . ?
C39 C40 C41 118.9(4) . . ?
C40 C41 C42 120.0(4) . . ?
C41 C42 C37 122.7(4) . . ?
C44 C43 C57 123.1(3) . . ?
C56 C43 C44 118.3(3) . . ?
C56 C43 C57 118.4(3) . . ?
C43 C44 C45 123.2(3) . . ?
C53 C44 C43 119.9(3) . . ?
C53 C44 C45 116.7(3) . . ?
C44 C45 C3 112.6(3) . . ?
C44 C45 C46 106.1(3) . . ?
C46 C45 C3 114.5(3) . . ?
C47 C46 C45 123.3(3) . . ?
C47 C46 C51 119.5(3) . . ?
C51 C46 C45 117.1(3) . . ?
C46 C47 C48 119.1(3) . . ?
C46 C47 C71 120.8(3) . . ?
C48 C47 C71 120.0(3) . . ?
C49 C48 C47 120.8(3) . . ?
C48 C49 C50 120.0(3) . . ?
C49 C50 C51 119.9(3) . . ?
C46 C51 C52 116.4(3) . . ?
C50 C51 C46 120.6(3) . . ?
C50 C51 C52 122.9(3) . . ?
C51 C52 C10 111.1(3) . . ?
C51 C52 C53 107.1(3) . . ?
C53 C52 C10 113.6(3) . . ?
C44 C53 C52 117.3(3) . . ?
C54 C53 C44 120.8(3) . . ?
C54 C53 C52 121.6(3) . . ?
C53 C54 C55 120.1(3) . . ?
C56 C55 C54 119.4(3) . . ?
C55 C56 C43 121.4(3) . . ?
C58 C57 C43 171.9(4) . . ?
C57 C58 B3 173.9(4) . . ?
C60 C59 C64 115.6(4) . . ?
C60 C59 B3 123.6(4) . . ?
C64 C59 B3 120.1(3) . . ?
C61 C60 C59 122.4(4) . . ?
C62 C61 C60 120.0(4) . . ?
C61 C62 C63 120.2(4) . . ?
C62 C63 C64 119.5(5) . . ?
C63 C64 C59 122.3(4) . . ?
C66 C65 B3 122.3(3) . . ?
C70 C65 C66 116.5(3) . . ?
C70 C65 B3 120.7(3) . . ?
C67 C66 C65 121.7(4) . . ?
C68 C67 C66 119.9(4) . . ?
C69 C68 C67 119.7(4) . . ?
C68 C69 C70 119.7(4) . . ?
C65 C70 C69 122.5(4) . . ?
C72 C71 C47 179.1(4) . . ?
C71 C72 B4 177.4(4) . . ?
C74 C73 C78 115.9(3) . . ?
C74 C73 B4 124.6(3) . . ?
C78 C73 B4 119.1(3) . . ?
C73 C74 C75 122.6(4) . . ?
C76 C75 C74 119.6(4) . . ?
C77 C76 C75 119.6(4) . . ?
C76 C77 C78 120.3(4) . . ?
C77 C78 C73 122.0(4) . . ?
C80 C79 B4 122.1(3) . . ?
C84 C79 C80 116.3(3) . . ?
C84 C79 B4 121.4(3) . . ?
C81 C80 C79 122.5(3) . . ?
C82 C81 C80 120.1(3) . . ?
C81 C82 C83 119.6(3) . . ?
C82 C83 C84 119.3(3) . . ?
C79 C84 C83 122.2(3) . . ?
C16 B1 N1 106.7(3) . . ?
C16 B1 C17 108.3(3) . . ?
C16 B1 C23 113.8(3) . . ?
C17 B1 N1 105.5(3) . . ?
C23 B1 N1 109.2(3) . . ?
C23 B1 C17 112.8(3) . . ?
N2 B2 C31 109.1(3) . . ?
N2 B2 C37 106.9(3) . . ?
C30 B2 N2 107.8(3) . . ?
C30 B2 C31 111.5(3) . . ?
C30 B2 C37 110.3(3) . . ?
C37 B2 C31 111.1(3) . . ?
N3 B3 C59 109.6(3) . . ?
N3 B3 C65 109.0(3) . . ?
C58 B3 N3 106.6(3) . . ?
C58 B3 C59 114.3(3) . . ?
C58 B3 C65 110.8(3) . . ?
C59 B3 C65 106.5(3) . . ?
N4 B4 C79 108.2(3) . . ?
C72 B4 N4 106.6(3) . . ?
C72 B4 C73 112.1(3) . . ?
C72 B4 C79 112.2(3) . . ?
C73 B4 N4 109.5(3) . . ?
C73 B4 C79 108.1(3) . . ?
N5 C85 C86 178.7(5) . . ?
N6 C87A C88A 176.3(9) . . ?
N6 C87B C88B 179(5) . . ?
N7 C89 C90 177.7(8) . . ?
N7B C89B C90B 177.7(18) . . ?
N8 C91 C92 178.7(5) . . ?
N9 C93 C94 178.5(7) . . ?
N10 C95 C96 177(6) . . ?
N11 C97 C98 173(4) . . ?
N13 C99 C100 171(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1C N5 0.92(7) 2.13(7) 3.038(5) 173(5) . yes
N2 H2A N6 1.05(6) 1.97(6) 3.003(6) 166(5) . yes
N3 H3A N7 0.94(5) 2.14(5) 3.070(6) 169(4) . yes
N3 H3A N7B 0.94(5) 2.25(5) 3.166(17) 164(4) . yes
N4 H4A N8 1.05(5) 2.08(5) 3.118(5) 174(4) . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -128.4(3) . . . . ?
C1 C2 C3 C45 109.5(4) . . . . ?
C1 C2 C11 C10 176.3(3) . . . . ?
C1 C2 C11 C12 -1.0(5) . . . . ?
C2 C1 C14 C13 -1.3(5) . . . . ?
C2 C1 C15 C16 161.7(14) . . . . ?
C2 C3 C4 C5 127.4(3) . . . . ?
C2 C3 C4 C9 -49.7(4) . . . . ?
C2 C3 C45 C44 -4.6(4) . . . . ?
C2 C3 C45 C46 116.7(3) . . . . ?
C2 C11 C12 C13 -0.3(5) . . . . ?
C3 C2 C11 C10 1.1(4) . . . . ?
C3 C2 C11 C12 -176.3(3) . . . . ?
C3 C4 C5 C6 178.6(3) . . . . ?
C3 C4 C5 C29 -3.2(5) . . . . ?
C3 C4 C9 C8 -177.2(3) . . . . ?
C3 C4 C9 C10 5.3(4) . . . . ?
C3 C45 C46 C47 105.1(4) . . . . ?
C3 C45 C46 C51 -79.7(4) . . . . ?
C4 C3 C45 C44 -124.7(3) . . . . ?
C4 C3 C45 C46 -3.4(4) . . . . ?
C4 C5 C6 C7 0.2(5) . . . . ?
C4 C5 C29 C30 -160.7(18) . . . . ?
C4 C9 C10 C11 42.6(4) . . . . ?
C4 C9 C10 C52 -81.8(4) . . . . ?
C5 C4 C9 C8 5.6(5) . . . . ?
C5 C4 C9 C10 -171.9(3) . . . . ?
C5 C6 C7 C8 3.0(6) . . . . ?
C6 C5 C29 C30 18(2) . . . . ?
C6 C7 C8 C9 -1.9(6) . . . . ?
C7 C8 C9 C4 -2.4(5) . . . . ?
C7 C8 C9 C10 175.0(3) . . . . ?
C8 C9 C10 C11 -134.9(3) . . . . ?
C8 C9 C10 C52 100.7(4) . . . . ?
C9 C4 C5 C6 -4.4(5) . . . . ?
C9 C4 C5 C29 173.7(3) . . . . ?
C9 C10 C11 C2 -45.9(4) . . . . ?
C9 C10 C11 C12 131.4(3) . . . . ?
C9 C10 C52 C51 -3.3(4) . . . . ?
C9 C10 C52 C53 117.6(3) . . . . ?
C10 C11 C12 C13 -177.5(3) . . . . ?
C10 C52 C53 C44 -78.1(4) . . . . ?
C10 C52 C53 C54 108.5(4) . . . . ?
C11 C2 C3 C4 46.6(4) . . . . ?
C11 C2 C3 C45 -75.5(4) . . . . ?
C11 C10 C52 C51 -125.6(3) . . . . ?
C11 C10 C52 C53 -4.7(4) . . . . ?
C11 C12 C13 C14 0.9(6) . . . . ?
C12 C13 C14 C1 0.0(6) . . . . ?
C14 C1 C2 C3 176.7(3) . . . . ?
C14 C1 C2 C11 1.8(5) . . . . ?
C14 C1 C15 C16 -14.5(17) . . . . ?
C15 C1 C2 C3 0.6(5) . . . . ?
C15 C1 C2 C11 -174.4(3) . . . . ?
C15 C1 C14 C13 175.1(3) . . . . ?
C17 C18 C19 C20 -1.3(8) . . . . ?
C18 C17 C22 C21 0.7(7) . . . . ?
C18 C17 B1 N1 -118.9(4) . . . . ?
C18 C17 B1 C16 127.1(4) . . . . ?
C18 C17 B1 C23 0.2(5) . . . . ?
C18 C19 C20 C21 0.3(9) . . . . ?
C19 C20 C21 C22 1.3(9) . . . . ?
C20 C21 C22 C17 -1.8(9) . . . . ?
C22 C17 C18 C19 0.8(6) . . . . ?
C22 C17 B1 N1 60.3(5) . . . . ?
C22 C17 B1 C16 -53.7(5) . . . . ?
C22 C17 B1 C23 179.4(4) . . . . ?
C23 C24 C25 C26 0.3(7) . . . . ?
C24 C23 C28 C27 1.6(6) . . . . ?
C24 C23 B1 N1 41.0(5) . . . . ?
C24 C23 B1 C16 160.1(4) . . . . ?
C24 C23 B1 C17 -76.0(5) . . . . ?
C24 C25 C26 C27 -0.2(8) . . . . ?
C25 C26 C27 C28 0.9(8) . . . . ?
C26 C27 C28 C23 -1.7(8) . . . . ?
C28 C23 C24 C25 -1.0(6) . . . . ?
C28 C23 B1 N1 -144.3(4) . . . . ?
C28 C23 B1 C16 -25.2(5) . . . . ?
C28 C23 B1 C17 98.7(4) . . . . ?
C29 C5 C6 C7 -178.1(3) . . . . ?
C31 C32 C33 C34 0.4(9) . . . . ?
C32 C31 C36 C35 -1.1(6) . . . . ?
C32 C31 B2 N2 31.6(5) . . . . ?
C32 C31 B2 C30 150.6(4) . . . . ?
C32 C31 B2 C37 -86.0(5) . . . . ?
C32 C33 C34 C35 -1.1(8) . . . . ?
C33 C34 C35 C36 0.7(7) . . . . ?
C34 C35 C36 C31 0.5(7) . . . . ?
C36 C31 C32 C33 0.7(7) . . . . ?
C36 C31 B2 N2 -152.5(4) . . . . ?
C36 C31 B2 C30 -33.5(5) . . . . ?
C36 C31 B2 C37 89.9(4) . . . . ?
C37 C38 C39 C40 -0.4(8) . . . . ?
C38 C37 C42 C41 -1.8(7) . . . . ?
C38 C37 B2 N2 147.1(4) . . . . ?
C38 C37 B2 C30 30.1(6) . . . . ?
C38 C37 B2 C31 -94.0(5) . . . . ?
C38 C39 C40 C41 -0.4(8) . . . . ?
C39 C40 C41 C42 0.0(8) . . . . ?
C40 C41 C42 C37 1.2(8) . . . . ?
C42 C37 C38 C39 1.4(7) . . . . ?
C42 C37 B2 N2 -34.6(5) . . . . ?
C42 C37 B2 C30 -151.5(4) . . . . ?
C42 C37 B2 C31 84.4(5) . . . . ?
C43 C44 C45 C3 -108.7(4) . . . . ?
C43 C44 C45 C46 125.3(3) . . . . ?
C43 C44 C53 C52 -170.2(3) . . . . ?
C43 C44 C53 C54 3.2(5) . . . . ?
C44 C43 C56 C55 1.0(5) . . . . ?
C44 C45 C46 C47 -130.1(3) . . . . ?
C44 C45 C46 C51 45.1(4) . . . . ?
C44 C53 C54 C55 -1.1(5) . . . . ?
C45 C3 C4 C5 -108.5(4) . . . . ?
C45 C3 C4 C9 74.5(3) . . . . ?
C45 C44 C53 C52 4.4(4) . . . . ?
C45 C44 C53 C54 177.9(3) . . . . ?
C45 C46 C47 C48 173.5(3) . . . . ?
C45 C46 C47 C71 -4.2(5) . . . . ?
C45 C46 C51 C50 -173.7(3) . . . . ?
C45 C46 C51 C52 3.5(4) . . . . ?
C46 C47 C48 C49 0.0(5) . . . . ?
C46 C51 C52 C10 75.9(4) . . . . ?
C46 C51 C52 C53 -48.7(4) . . . . ?
C47 C46 C51 C50 1.7(5) . . . . ?
C47 C46 C51 C52 178.9(3) . . . . ?
C47 C48 C49 C50 1.5(5) . . . . ?
C48 C49 C50 C51 -1.4(5) . . . . ?
C49 C50 C51 C46 -0.2(5) . . . . ?
C49 C50 C51 C52 -177.2(3) . . . . ?
C50 C51 C52 C10 -107.0(4) . . . . ?
C50 C51 C52 C53 128.4(3) . . . . ?
C51 C46 C47 C48 -1.6(5) . . . . ?
C51 C46 C47 C71 -179.3(3) . . . . ?
C51 C52 C53 C44 44.9(4) . . . . ?
C51 C52 C53 C54 -128.5(3) . . . . ?
C52 C10 C11 C2 79.5(4) . . . . ?
C52 C10 C11 C12 -103.2(4) . . . . ?
C52 C53 C54 C55 172.1(3) . . . . ?
C53 C44 C45 C3 76.8(4) . . . . ?
C53 C44 C45 C46 -49.2(4) . . . . ?
C53 C54 C55 C56 -1.1(6) . . . . ?
C54 C55 C56 C43 1.1(6) . . . . ?
C56 C43 C44 C45 -177.5(3) . . . . ?
C56 C43 C44 C53 -3.2(5) . . . . ?
C57 C43 C44 C45 -2.6(5) . . . . ?
C57 C43 C44 C53 171.8(3) . . . . ?
C57 C43 C56 C55 -174.2(3) . . . . ?
C59 C60 C61 C62 -0.4(6) . . . . ?
C60 C59 C64 C63 1.6(6) . . . . ?
C60 C59 B3 N3 27.9(5) . . . . ?
C60 C59 B3 C58 147.4(3) . . . . ?
C60 C59 B3 C65 -89.9(4) . . . . ?
C60 C61 C62 C63 0.8(7) . . . . ?
C61 C62 C63 C64 0.0(7) . . . . ?
C62 C63 C64 C59 -1.2(6) . . . . ?
C64 C59 C60 C61 -0.8(5) . . . . ?
C64 C59 B3 N3 -162.2(3) . . . . ?
C64 C59 B3 C58 -42.7(5) . . . . ?
C64 C59 B3 C65 80.0(4) . . . . ?
C65 C66 C67 C68 1.9(7) . . . . ?
C66 C65 C70 C69 -1.8(6) . . . . ?
C66 C65 B3 N3 -32.7(5) . . . . ?
C66 C65 B3 C58 -149.7(4) . . . . ?
C66 C65 B3 C59 85.4(4) . . . . ?
C66 C67 C68 C69 -2.1(7) . . . . ?
C67 C68 C69 C70 0.4(6) . . . . ?
C68 C69 C70 C65 1.6(6) . . . . ?
C70 C65 C66 C67 0.1(6) . . . . ?
C70 C65 B3 N3 155.4(3) . . . . ?
C70 C65 B3 C58 38.4(5) . . . . ?
C70 C65 B3 C59 -86.5(4) . . . . ?
C71 C47 C48 C49 177.7(3) . . . . ?
C73 C74 C75 C76 0.3(6) . . . . ?
C74 C73 C78 C77 -2.4(6) . . . . ?
C74 C73 B4 N4 -35.7(5) . . . . ?
C74 C73 B4 C72 -153.8(4) . . . . ?
C74 C73 B4 C79 82.0(4) . . . . ?
C74 C75 C76 C77 -2.1(6) . . . . ?
C75 C76 C77 C78 1.6(6) . . . . ?
C76 C77 C78 C73 0.7(6) . . . . ?
C78 C73 C74 C75 1.8(6) . . . . ?
C78 C73 B4 N4 152.2(3) . . . . ?
C78 C73 B4 C72 34.1(5) . . . . ?
C78 C73 B4 C79 -90.1(4) . . . . ?
C79 C80 C81 C82 -0.4(6) . . . . ?
C80 C79 C84 C83 1.4(5) . . . . ?
C80 C79 B4 N4 55.2(4) . . . . ?
C80 C79 B4 C72 172.5(3) . . . . ?
C80 C79 B4 C73 -63.3(4) . . . . ?
C80 C81 C82 C83 1.9(6) . . . . ?
C81 C82 C83 C84 -1.7(5) . . . . ?
C82 C83 C84 C79 0.1(5) . . . . ?
C84 C79 C80 C81 -1.2(5) . . . . ?
C84 C79 B4 N4 -131.1(3) . . . . ?
C84 C79 B4 C72 -13.7(5) . . . . ?
C84 C79 B4 C73 110.4(3) . . . . ?
B1 C17 C18 C19 -180.0(4) . . . . ?
B1 C17 C22 C21 -178.5(5) . . . . ?
B1 C23 C24 C25 174.0(4) . . . . ?
B1 C23 C28 C27 -173.5(4) . . . . ?
B2 C31 C32 C33 176.8(4) . . . . ?
B2 C31 C36 C35 -177.3(4) . . . . ?
B2 C37 C38 C39 179.9(5) . . . . ?
B2 C37 C42 C41 179.7(4) . . . . ?
B3 C59 C60 C61 169.6(3) . . . . ?
B3 C59 C64 C63 -169.1(4) . . . . ?
B3 C65 C66 C67 -172.1(4) . . . . ?
B3 C65 C70 C69 170.5(3) . . . . ?
B4 C73 C74 C75 -170.5(4) . . . . ?
B4 C73 C78 C77 170.4(4) . . . . ?
B4 C79 C80 C81 172.9(3) . . . . ?
B4 C79 C84 C83 -172.7(3) . . . . ?

_olex2_date_sample_data_collection 2019-06-16
_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 2.033
_oxdiff_exptl_absorpt_empirical_full_min 0.388
####################################################################### 
# 
# 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_11
_database_code_depnum_ccdc_archive 'CCDC 1952354'
loop_
_audit_author_name
_audit_author_address
'Hans Georg Stammler'
;University of Bielefeld
Germany
;
_audit_update_record             
;
2019-09-09 deposited with the CCDC.	2021-05-06 downloaded from the CCDC.
;
# measured as exp_1984
_audit_creation_date             2019-06-18
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C84 H72 B4 N8, 3.33(C H2 Cl2)'
_chemical_formula_sum            'C87.33 H78.66 B4 Cl6.66 N8'
_chemical_formula_weight         1519.63
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C84H76B4N10 Cl4'
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'
B B 0.0090 0.0039 '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      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'

_cell_length_a                   23.0669(4)
_cell_length_b                   22.8536(4)
_cell_length_c                   15.3750(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8105.2(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    39794
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.2340
_cell_measurement_theta_min      2.6740
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.518
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.756
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.54a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3168
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 1 0.0555
0 -1 0 0.0849
0 1 -1 0.0555
-1 0 0 0.0991
1 0 0 0.0991
-1 -5 -4 0.0891
1 5 4 0.0891
0 1 0 0.0849

_exptl_crystal_size_max          0.217
_exptl_crystal_size_mid          0.191
_exptl_crystal_size_min          0.111
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
-0.0098 -1.0312 0.9849 -0.0712 0.0690 -0.0689
0.0047 -0.9993 -0.0139 -0.0672 0.0006 0.0041
0.0098 1.0312 -0.9849 0.0712 -0.0690 0.0689
-0.9980 -0.0043 -0.0066 -0.0032 -0.0487 -0.0455
0.9980 0.0043 0.0066 0.0032 0.0487 0.0455
-0.9166 -4.8735 -4.0710 -0.3232 -0.3195 0.2668
0.9166 4.8735 4.0710 0.3232 0.3195 -0.2668
-0.0047 0.9993 0.0139 0.0672 -0.0006 -0.0041

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            91890
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.553
_diffrn_reflns_theta_min         2.722
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_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    -32.00  33.00   1.00   11.00    --  -38.50  38.00 150.00   65
  2  ω   -116.00  -6.00   1.00   11.00    --  -38.50 -19.00 -30.00  110
  3  ω    -72.00  22.00   1.00   11.00    --  -38.50  19.00 120.00   94
  4  ω      2.00  63.00   1.00   11.00    --   42.70 -99.00 -90.00   61
  5  ω     13.00  68.00   1.00   11.00    --   42.70  77.00   0.00   55
  6  ω     13.00  42.00   1.00   11.00    --   42.70  77.00  90.00   29
  7  ω     67.00  93.00   1.00   11.00    --   42.70  57.00  90.00   26
  8  ω     13.00  62.00   1.00   11.00    --   42.70  77.00-120.00   49
  9  ω     10.00  65.00   1.00   11.00    --   42.70 -99.00-150.00   55
 10  ω     13.00  59.00   1.00   11.00    --   42.70  77.00 -60.00   46
 11  ω     19.00  85.00   1.00   11.00    --   42.70  57.00-180.00   66
 12  ω    -27.00  44.00   1.00   11.00    --   42.70 -38.00 -60.00   71
 13  ω     46.00  96.00   1.00   11.00    --   42.70-125.00  90.00   50
 14  ω     15.00  55.00   1.00   11.00    --   42.70  77.00 120.00   40
 15  ω      9.00  34.00   1.00   11.00    --   42.70  86.00-176.10   25
 16  ω     18.00  57.00   1.00   11.00    --   42.70  57.00  90.00   39
 17  ω     22.00  87.00   1.00   11.00    --   42.70  38.00 150.00   65
 18  ω     53.00 104.00   1.00   27.50    --  111.00 -94.00 -90.00   51
 19  ω     31.00 109.00   1.00   27.50    --  111.00 -94.00  90.00   78
 20  ω    129.00 173.00   1.00   27.50    --  111.00  60.00 -14.24   44
 21  ω     89.00 115.00   1.00   27.50    --  111.00  45.00-150.00   26
 22  ω     85.00 178.00   1.00   27.50    --  111.00  61.00 -60.00   93
 23  ω     85.00 111.00   1.00   27.50    --  111.00  61.00  90.00   26
 24  ω     81.00 175.00   1.00   27.50    --  111.00  77.00  30.00   94
 25  ω     43.00  71.00   1.00   27.50    --  111.00 -94.00  30.00   28
 26  ω     85.00 144.00   1.00   27.50    --  111.00  61.00-120.00   59
 27  ω     85.00 111.00   1.00   27.50    --  111.00  61.00 -30.00   26
 28  ω     81.00 131.00   1.00   27.50    --  111.00  77.00 150.00   50
 29  ω     81.00 111.00   1.00   27.50    --  111.00  77.00 -90.00   30
 30  ω    115.00 166.00   1.00   27.50    --  111.00  77.00 -90.00   51
 31  ω     85.00 124.00   1.00   27.50    --  111.00  60.00 -14.24   39
 32  ω     82.00 108.00   1.00   27.50    --  111.00  71.00-153.10   26
 33  ω     85.00 111.00   1.00   27.50    --  111.00  61.00-150.00   26
 34  ω     81.00 108.00   1.00   27.50    --  111.00  77.00  90.00   27
 35  ω    106.00 140.00   1.00   27.50    --  111.00 -77.00 -60.00   34
 36  ω     49.00  86.00   1.00   27.50    --  111.00 -77.00 -60.00   37
 37  ω     81.00 175.00   1.00   27.50    --  111.00  77.00-120.00   94
 38  ω     81.00 107.00   1.00   27.50    --  111.00  77.00   0.00   26
 39  ω     85.00 111.00   1.00   27.50    --  111.00  61.00 150.00   26
 40  ω     43.00 126.00   1.00   27.50    --  111.00-136.00  56.84   83
 41  ω     81.00 106.00   1.00   27.50    --  111.00  77.00  60.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0029110000
_diffrn_orient_matrix_UB_12      0.0672737000
_diffrn_orient_matrix_UB_13      -0.0018002000
_diffrn_orient_matrix_UB_21      0.0483477000
_diffrn_orient_matrix_UB_22      -0.0012959000
_diffrn_orient_matrix_UB_23      0.0691551000
_diffrn_orient_matrix_UB_31      0.0460647000
_diffrn_orient_matrix_UB_32      -0.0028584000
_diffrn_orient_matrix_UB_33      -0.0724921000
_diffrn_oxdiff_digest_frames     
;
01256eeacb8a8a7093da01f43322aa5d21032919c66
;
_diffrn_oxdiff_digest_hkl        
;
01491ca4df2ba6d1c60b6f529ab5436a7a25ba
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.888
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.934
_reflns_number_gt                14362
_reflns_number_total             16668
_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 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.54a (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    'ShelXD (Sheldrick, 2008)'
_refine_diff_density_max         0.834
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 
;
 Flack x determined using 5642 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.006(7)
_refine_ls_extinction_coef       0.00132(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1126
_refine_ls_number_reflns         16668
_refine_ls_number_restraints     261
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0605
_refine_ls_restrained_S_all      1.068
_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)+(0.0894P)²+5.7809P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1554
_refine_ls_wR_factor_ref         0.1723
_refine_special_details          'Disordered CH2Cl2 with non-integer number.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl5-C87 \\sim Cl6-C87 \\sim Cl2-C85 \\sim Cl1-C85 \\sim Cl3_$1-C86_$1 \\sim
Cl4_$1-C86_$1 ~
 Cl11_$1-C90_$1 \\sim Cl12_$1-C90_$1 \\sim Cl13_$1-C91_$1 \\sim Cl14_$1-C91_$1
\\sim Cl10_$1-
 C89_$1 \\sim Cl9_$1-C89_$1 \\sim Cl8_$1-C88_$1 \\sim Cl7_$1-C88_$1
 with sigma of 0.02
 N6-H6A \\sim N6-H6B \\sim N5-H5A \\sim N5-H5B \\sim N7-H7A \\sim N7-H7B \\sim
N8-H8A \\sim N8-H8B \\sim N2-
 H2A \\sim N2-H2B \\sim N1-H1B \\sim N1-H1A \\sim N3-H3B \\sim N3-H3A \\sim
N4-H4A \\sim N4-H4B
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 Cl1, Cl2, C85, Cl3, Cl4, C86, Cl5, Cl6, C87, Cl7, Cl8, C88, Cl9, Cl10, C89,
 Cl11, Cl12, C90, Cl13, Cl14, C91
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(Cl1)=Sof(Cl2)=Sof(C85)=Sof(H85A)=Sof(H85B)=FVAR(1)
 Sof(Cl3)=Sof(Cl4)=Sof(C86)=Sof(H86A)=Sof(H86B)=FVAR(2)
 Sof(Cl5)=Sof(Cl6)=Sof(C87)=Sof(H87A)=Sof(H87B)=FVAR(3)
 Sof(Cl7)=Sof(Cl8)=Sof(C88)=Sof(H88A)=Sof(H88B)=FVAR(4)
 Sof(Cl9)=Sof(Cl10)=Sof(C89)=Sof(H89A)=Sof(H89B)=FVAR(5)
 Sof(Cl11)=Sof(Cl12)=Sof(C90)=Sof(H90A)=Sof(H90B)=FVAR(6)
 Sof(Cl13)=Sof(Cl14)=Sof(C91)=Sof(H91A)=Sof(H91B)=FVAR(7)
5.a Ternary CH refined with riding coordinates:
 C3(H3), C10(H10), C45(H45), C52(H52)
5.b Secondary CH2 refined with riding coordinates:
 C85(H85A,H85B), C86(H86A,H86B), C87(H87A,H87B), C88(H88A,H88B), C89(H89A,
 H89B), C90(H90A,H90B), C91(H91A,H91B)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14), C18(H18), C19(H19),
 C20(H20), C21(H21), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28),
  C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
 C40(H40), C41(H41), C42(H42), C48(H48), C49(H49), C50(H50), C54(H54), C55(H55),
  C56(H56), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C66(H66),
 C67(H67), C68(H68), C69(H69), C70(H70), C74(H74), C75(H75), C76(H76), C77(H77),
  C78(H78), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.77094(16) 0.69493(16) 0.2950(3) 0.0277(8) Uani 1 1 d D . . . .
N2 N 0.74564(16) 0.72733(16) 0.3672(3) 0.0270(8) Uani 1 1 d D . . . .
N3 N 0.64085(15) 0.79798(16) 0.3838(3) 0.0256(7) Uani 1 1 d D . . . .
N4 N 0.59402(16) 0.75609(16) 0.3976(3) 0.0289(8) Uani 1 1 d D . . . .
N5 N 0.97967(15) 0.67728(16) 0.4238(3) 0.0270(8) Uani 1 1 d D . . . .
N6 N 0.94461(17) 0.70874(17) 0.4871(3) 0.0309(8) Uani 1 1 d D . . . .
N7 N 0.83108(15) 0.82806(16) 0.5138(3) 0.0261(8) Uani 1 1 d D . . . .
N8 N 0.84642(17) 0.79022(17) 0.4409(3) 0.0287(8) Uani 1 1 d D . . . .
C1 C 0.66726(18) 0.55449(18) 0.4606(3) 0.0282(9) Uani 1 1 d . . . . .
C2 C 0.68766(18) 0.56637(18) 0.5456(3) 0.0256(9) Uani 1 1 d . . . . .
C3 C 0.72482(18) 0.61937(18) 0.5680(3) 0.0239(8) Uani 1 1 d . . . . .
H3 H 0.719730 0.648732 0.522199 0.029 Uiso 1 1 calc R . . . .
C4 C 0.70300(17) 0.64477(19) 0.6522(3) 0.0257(9) Uani 1 1 d . . . . .
C5 C 0.69210(18) 0.70427(19) 0.6646(3) 0.0270(9) Uani 1 1 d . . . . .
C6 C 0.6779(2) 0.7235(2) 0.7492(3) 0.0329(10) Uani 1 1 d . . . . .
H6 H 0.671307 0.763088 0.759373 0.039 Uiso 1 1 calc R . . . .
C7 C 0.6737(2) 0.6840(2) 0.8173(3) 0.0377(11) Uani 1 1 d . . . . .
H7 H 0.665581 0.697416 0.873093 0.045 Uiso 1 1 calc R . . . .
C8 C 0.6814(2) 0.6244(2) 0.8031(4) 0.0352(10) Uani 1 1 d . . . . .
H8 H 0.676809 0.597863 0.848469 0.042 Uiso 1 1 calc R . . . .
C9 C 0.69611(19) 0.6047(2) 0.7196(3) 0.0289(9) Uani 1 1 d . . . . .
C10 C 0.70154(19) 0.53962(19) 0.6976(3) 0.0289(9) Uani 1 1 d . . . . .
H10 H 0.681560 0.517057 0.742804 0.035 Uiso 1 1 calc R . . . .
C11 C 0.67170(19) 0.52887(19) 0.6125(3) 0.0282(9) Uani 1 1 d . . . . .
C12 C 0.6345(2) 0.4825(2) 0.5993(4) 0.0339(10) Uani 1 1 d . . . . .
H12 H 0.624077 0.458313 0.645324 0.041 Uiso 1 1 calc R . . . .
C13 C 0.6125(2) 0.4722(2) 0.5150(4) 0.0372(11) Uani 1 1 d . . . . .
H13 H 0.586762 0.441524 0.505338 0.045 Uiso 1 1 calc R . . . .
C14 C 0.6293(2) 0.5075(2) 0.4473(4) 0.0350(11) Uani 1 1 d . . . . .
H14 H 0.615190 0.500094 0.391678 0.042 Uiso 1 1 calc R . . . .
C15 C 0.68394(19) 0.58929(19) 0.3879(3) 0.0275(9) Uani 1 1 d . . . . .
C16 C 0.69899(19) 0.61541(19) 0.3229(3) 0.0291(10) Uani 1 1 d . . . . .
C17 C 0.6748(2) 0.6953(2) 0.2008(3) 0.0309(10) Uani 1 1 d . . . . .
C18 C 0.6167(2) 0.6791(2) 0.2001(4) 0.0391(11) Uani 1 1 d . . . . .
H18 H 0.604816 0.647401 0.233458 0.047 Uiso 1 1 calc R . . . .
C19 C 0.5755(2) 0.7096(3) 0.1502(4) 0.0501(14) Uani 1 1 d . . . . .
H19 H 0.536960 0.697747 0.150746 0.060 Uiso 1 1 calc R . . . .
C20 C 0.5919(3) 0.7567(3) 0.1006(4) 0.0546(16) Uani 1 1 d . . . . .
H20 H 0.564897 0.776314 0.066426 0.065 Uiso 1 1 calc R . . . .
C21 C 0.6490(3) 0.7744(3) 0.1024(4) 0.0536(15) Uani 1 1 d . . . . .
H21 H 0.660226 0.806874 0.069990 0.064 Uiso 1 1 calc R . . . .
C22 C 0.6899(2) 0.7449(2) 0.1514(4) 0.0401(12) Uani 1 1 d . . . . .
H22 H 0.728067 0.758041 0.151716 0.048 Uiso 1 1 calc R . . . .
C23 C 0.76040(19) 0.61703(19) 0.1753(3) 0.0292(9) Uani 1 1 d . . . . .
C24 C 0.7984(2) 0.5724(2) 0.2018(4) 0.0317(10) Uani 1 1 d . . . . .
H24 H 0.799851 0.562550 0.260480 0.038 Uiso 1 1 calc R . . . .
C25 C 0.8339(2) 0.5425(2) 0.1438(4) 0.0359(11) Uani 1 1 d . . . . .
H25 H 0.858686 0.513332 0.163626 0.043 Uiso 1 1 calc R . . . .
C26 C 0.8319(2) 0.5565(2) 0.0564(4) 0.0363(11) Uani 1 1 d . . . . .
H26 H 0.855854 0.537179 0.017168 0.044 Uiso 1 1 calc R . . . .
C27 C 0.7941(2) 0.5995(2) 0.0273(4) 0.0393(11) Uani 1 1 d . . . . .
H27 H 0.792174 0.608323 -0.031638 0.047 Uiso 1 1 calc R . . . .
C28 C 0.7595(2) 0.6291(2) 0.0856(3) 0.0344(10) Uani 1 1 d . . . . .
H28 H 0.734668 0.658048 0.064977 0.041 Uiso 1 1 calc R . . . .
C29 C 0.69036(18) 0.74579(18) 0.5940(3) 0.0251(9) Uani 1 1 d . . . . .
C30 C 0.68188(17) 0.78275(18) 0.5374(3) 0.0246(8) Uani 1 1 d . . . . .
C31 C 0.71195(18) 0.87753(17) 0.4430(3) 0.0245(8) Uani 1 1 d . . . . .
C32 C 0.74394(19) 0.87518(18) 0.3651(3) 0.0281(9) Uani 1 1 d . . . . .
H32 H 0.734426 0.847194 0.323591 0.034 Uiso 1 1 calc R . . . .
C33 C 0.7893(2) 0.9135(2) 0.3486(3) 0.0326(10) Uani 1 1 d . . . . .
H33 H 0.809414 0.910944 0.296319 0.039 Uiso 1 1 calc R . . . .
C34 C 0.8049(2) 0.9555(2) 0.4092(4) 0.0353(11) Uani 1 1 d . . . . .
H34 H 0.836091 0.980375 0.398802 0.042 Uiso 1 1 calc R . . . .
C35 C 0.7731(2) 0.9599(2) 0.4863(4) 0.0345(11) Uani 1 1 d . . . . .
H35 H 0.782242 0.988582 0.526924 0.041 Uiso 1 1 calc R . . . .
C36 C 0.72772(19) 0.92136(18) 0.5020(3) 0.0293(9) Uani 1 1 d . . . . .
H36 H 0.707045 0.924801 0.553655 0.035 Uiso 1 1 calc R . . . .
C37 C 0.60553(18) 0.86748(18) 0.5093(3) 0.0279(9) Uani 1 1 d . . . . .
C38 C 0.58583(19) 0.91789(19) 0.4664(3) 0.0305(10) Uani 1 1 d . . . . .
H38 H 0.605544 0.930865 0.417318 0.037 Uiso 1 1 calc R . . . .
C39 C 0.5378(2) 0.9490(2) 0.4950(4) 0.0383(12) Uani 1 1 d . . . . .
H39 H 0.525695 0.982121 0.464998 0.046 Uiso 1 1 calc R . . . .
C40 C 0.5080(2) 0.9307(3) 0.5684(4) 0.0457(14) Uani 1 1 d . . . . .
H40 H 0.475491 0.951161 0.587310 0.055 Uiso 1 1 calc R . . . .
C41 C 0.5271(2) 0.8813(3) 0.6138(4) 0.0431(12) Uani 1 1 d . . . . .
H41 H 0.507824 0.869117 0.663697 0.052 Uiso 1 1 calc R . . . .
C42 C 0.5751(2) 0.8506(2) 0.5839(3) 0.0339(10) Uani 1 1 d . . . . .
H42 H 0.587328 0.817683 0.614483 0.041 Uiso 1 1 calc R . . . .
C43 C 0.83295(18) 0.53678(19) 0.4633(3) 0.0257(9) Uani 1 1 d . . . . .
C44 C 0.80601(17) 0.54699(18) 0.5448(3) 0.0243(9) Uani 1 1 d . . . . .
C45 C 0.79345(18) 0.60730(17) 0.5797(3) 0.0238(8) Uani 1 1 d . . . . .
H45 H 0.814768 0.635871 0.544584 0.029 Uiso 1 1 calc R . . . .
C46 C 0.81749(17) 0.60882(18) 0.6722(3) 0.0246(9) Uani 1 1 d . . . . .
C47 C 0.85249(18) 0.65437(18) 0.7043(3) 0.0258(9) Uani 1 1 d . . . . .
C48 C 0.8802(2) 0.6478(2) 0.7847(3) 0.0326(10) Uani 1 1 d . . . . .
H48 H 0.904267 0.677351 0.805321 0.039 Uiso 1 1 calc R . . . .
C49 C 0.8722(2) 0.5977(2) 0.8339(3) 0.0347(10) Uani 1 1 d . . . . .
H49 H 0.892081 0.593191 0.886100 0.042 Uiso 1 1 calc R . . . .
C50 C 0.8347(2) 0.5544(2) 0.8056(3) 0.0322(10) Uani 1 1 d . . . . .
H50 H 0.827448 0.521912 0.840341 0.039 Uiso 1 1 calc R . . . .
C51 C 0.80794(19) 0.55976(19) 0.7248(3) 0.0264(9) Uani 1 1 d . . . . .
C52 C 0.76697(19) 0.51525(19) 0.6890(3) 0.0284(9) Uani 1 1 d . . . . .
H52 H 0.770215 0.479713 0.724367 0.034 Uiso 1 1 calc R . . . .
C53 C 0.78692(18) 0.50069(18) 0.5965(3) 0.0260(9) Uani 1 1 d . . . . .
C54 C 0.78980(19) 0.44370(19) 0.5642(3) 0.0295(10) Uani 1 1 d . . . . .
H54 H 0.776481 0.412512 0.597559 0.035 Uiso 1 1 calc R . . . .
C55 C 0.8128(2) 0.43385(19) 0.4815(3) 0.0319(10) Uani 1 1 d . . . . .
H55 H 0.813252 0.396101 0.458903 0.038 Uiso 1 1 calc R . . . .
C56 C 0.83487(19) 0.47927(19) 0.4331(3) 0.0288(9) Uani 1 1 d . . . . .
H56 H 0.851379 0.471481 0.379101 0.035 Uiso 1 1 calc R . . . .
C57 C 0.86097(17) 0.58316(18) 0.4167(3) 0.0231(8) Uani 1 1 d . . . . .
C58 C 0.89133(17) 0.61872(18) 0.3789(3) 0.0243(8) Uani 1 1 d . . . . .
C59 C 0.98894(18) 0.61411(19) 0.2878(3) 0.0262(9) Uani 1 1 d . . . . .
C60 C 0.9852(2) 0.5534(2) 0.2871(3) 0.0308(10) Uani 1 1 d . . . . .
H60 H 0.953488 0.535537 0.313444 0.037 Uiso 1 1 calc R . . . .
C61 C 1.0274(2) 0.5184(2) 0.2481(4) 0.0356(11) Uani 1 1 d . . . . .
H61 H 1.023622 0.477884 0.248362 0.043 Uiso 1 1 calc R . . . .
C62 C 1.0752(2) 0.5444(2) 0.2088(3) 0.0358(11) Uani 1 1 d . . . . .
H62 H 1.103755 0.521392 0.183160 0.043 Uiso 1 1 calc R . . . .
C63 C 1.0800(2) 0.6047(2) 0.2083(4) 0.0359(11) Uani 1 1 d . . . . .
H63 H 1.111716 0.622481 0.181985 0.043 Uiso 1 1 calc R . . . .
C64 C 1.0376(2) 0.6386(2) 0.2469(3) 0.0312(10) Uani 1 1 d . . . . .
H64 H 1.041465 0.679101 0.245813 0.037 Uiso 1 1 calc R . . . .
C65 C 0.92480(17) 0.71226(19) 0.2807(3) 0.0277(9) Uani 1 1 d . . . . .
C66 C 0.89309(19) 0.7031(2) 0.2041(3) 0.0310(10) Uani 1 1 d . . . . .
H66 H 0.883228 0.664949 0.188929 0.037 Uiso 1 1 calc R . . . .
C67 C 0.8759(2) 0.7482(2) 0.1501(4) 0.0412(12) Uani 1 1 d . . . . .
H67 H 0.854468 0.740304 0.100200 0.049 Uiso 1 1 calc R . . . .
C68 C 0.8908(3) 0.8061(2) 0.1709(4) 0.0464(14) Uani 1 1 d . . . . .
H68 H 0.878770 0.836905 0.135882 0.056 Uiso 1 1 calc R . . . .
C69 C 0.9240(3) 0.8165(2) 0.2447(4) 0.0423(12) Uani 1 1 d . . . . .
H69 H 0.935158 0.854535 0.258394 0.051 Uiso 1 1 calc R . . . .
C70 C 0.9405(2) 0.7701(2) 0.2985(4) 0.0331(10) Uani 1 1 d . . . . .
H70 H 0.962655 0.777986 0.347699 0.040 Uiso 1 1 calc R . . . .
C71 C 0.85811(18) 0.70931(19) 0.6599(3) 0.0274(9) Uani 1 1 d . . . . .
C72 C 0.86283(18) 0.75851(18) 0.6327(3) 0.0260(9) Uani 1 1 d . . . . .
C73 C 0.93707(19) 0.83818(18) 0.5780(3) 0.0289(9) Uani 1 1 d . . . . .
C74 C 0.9549(2) 0.8727(2) 0.5086(4) 0.0386(12) Uani 1 1 d . . . . .
H74 H 0.927272 0.890231 0.473129 0.046 Uiso 1 1 calc R . . . .
C75 C 1.0141(2) 0.8817(3) 0.4913(5) 0.0494(15) Uani 1 1 d . . . . .
H75 H 1.025162 0.904423 0.443928 0.059 Uiso 1 1 calc R . . . .
C76 C 1.0554(2) 0.8572(2) 0.5435(5) 0.0482(15) Uani 1 1 d . . . . .
H76 H 1.094502 0.862609 0.531142 0.058 Uiso 1 1 calc R . . . .
C77 C 1.0388(2) 0.8243(2) 0.6152(5) 0.0466(14) Uani 1 1 d . . . . .
H77 H 1.066612 0.808574 0.652222 0.056 Uiso 1 1 calc R . . . .
C78 C 0.9805(2) 0.8150(2) 0.6311(4) 0.0378(12) Uani 1 1 d . . . . .
H78 H 0.969871 0.792555 0.678946 0.045 Uiso 1 1 calc R . . . .
C79 C 0.83913(19) 0.86998(19) 0.6649(3) 0.0284(9) Uani 1 1 d . . . . .
C80 C 0.8591(2) 0.9276(2) 0.6748(3) 0.0319(10) Uani 1 1 d . . . . .
H80 H 0.892707 0.938829 0.645899 0.038 Uiso 1 1 calc R . . . .
C81 C 0.8308(2) 0.9684(2) 0.7259(4) 0.0390(12) Uani 1 1 d . . . . .
H81 H 0.844839 1.006488 0.730046 0.047 Uiso 1 1 calc R . . . .
C82 C 0.7814(2) 0.9521(2) 0.7706(4) 0.0406(12) Uani 1 1 d . . . . .
H82 H 0.762855 0.978834 0.806688 0.049 Uiso 1 1 calc R . . . .
C83 C 0.7599(2) 0.8967(2) 0.7618(4) 0.0426(12) Uani 1 1 d . . . . .
H83 H 0.726173 0.886103 0.791095 0.051 Uiso 1 1 calc R . . . .
C84 C 0.7883(2) 0.8558(2) 0.7089(4) 0.0340(10) Uani 1 1 d . . . . .
H84 H 0.772907 0.818377 0.703052 0.041 Uiso 1 1 calc R . . . .
B1 B 0.7235(2) 0.6538(2) 0.2456(4) 0.0299(11) Uani 1 1 d . . . . .
B2 B 0.6611(2) 0.8323(2) 0.4713(3) 0.0247(9) Uani 1 1 d . . . . .
B3 B 0.9435(2) 0.6562(2) 0.3387(4) 0.0265(10) Uani 1 1 d . . . . .
B4 B 0.8700(2) 0.8241(2) 0.6011(3) 0.0239(9) Uani 1 1 d . . . . .
Cl1 Cl 0.62065(12) 0.57496(14) 0.0275(2) 0.0582(10) Uani 0.536(6) 1 d D U P A 1
Cl2 Cl 0.5224(2) 0.5559(2) 0.1431(3) 0.0637(14) Uani 0.536(6) 1 d D U P A 1
C85 C 0.5466(5) 0.5718(12) 0.0374(9) 0.114(8) Uani 0.536(6) 1 d D U P A 1
H85A H 0.531928 0.542089 -0.001908 0.137 Uiso 0.536(6) 1 calc R . P A 1
H85B H 0.530389 0.609057 0.019533 0.137 Uiso 0.536(6) 1 calc R . P A 1
Cl3 Cl 0.4502(2) 0.50225(18) 0.3128(3) 0.0574(11) Uani 0.537(8) 1 d D U P B 1
Cl4 Cl 0.5007(3) 0.3863(3) 0.3304(4) 0.136(3) Uani 0.537(8) 1 d D U P B 1
C86 C 0.4691(8) 0.4361(6) 0.2633(11) 0.085(5) Uani 0.537(8) 1 d D U P B 1
H86A H 0.434476 0.418756 0.238589 0.102 Uiso 0.537(8) 1 calc R . P B 1
H86B H 0.495550 0.444303 0.215792 0.102 Uiso 0.537(8) 1 calc R . P B 1
Cl5 Cl 0.4562(6) 0.4798(9) 0.3211(10) 0.185(8) Uani 0.416(9) 1 d D U P C 2
Cl6 Cl 0.5200(3) 0.5363(3) 0.1790(11) 0.148(6) Uani 0.416(9) 1 d D U P C 2
C87 C 0.4911(8) 0.4728(7) 0.2208(12) 0.077(6) Uani 0.416(9) 1 d D U P C 2
H87A H 0.522030 0.444370 0.226840 0.092 Uiso 0.416(9) 1 calc R . P C 2
H87B H 0.463551 0.457264 0.179063 0.092 Uiso 0.416(9) 1 calc R . P C 2
Cl7 Cl 0.4440(4) 0.1408(7) 0.3782(5) 0.180(7) Uani 0.388(8) 1 d D U P D 2
Cl8 Cl 0.5249(4) 0.1321(6) 0.5231(8) 0.100(5) Uani 0.388(8) 1 d D U P D 2
C88 C 0.4757(9) 0.1016(11) 0.4581(15) 0.083(12) Uani 0.388(8) 1 d D U P D 2
H88A H 0.444914 0.086711 0.494946 0.100 Uiso 0.388(8) 1 calc R . P D 2
H88B H 0.493853 0.067932 0.430962 0.100 Uiso 0.388(8) 1 calc R . P D 2
Cl9 Cl 0.45897(16) 0.09149(18) 0.4840(3) 0.0515(11) Uani 0.529(7) 1 d D U P E 1
Cl10 Cl 0.54377(13) 0.18488(19) 0.4866(2) 0.0709(14) Uani 0.529(7) 1 d D U P E
1
C89 C 0.5223(11) 0.1181(10) 0.5289(16) 0.049(5) Uani 0.529(7) 1 d D U P E 1
H89A H 0.552998 0.089753 0.519367 0.059 Uiso 0.529(7) 1 calc R . P E 1
H89B H 0.517057 0.122098 0.591201 0.059 Uiso 0.529(7) 1 calc R . P E 1
Cl11 Cl 0.6153(4) 0.3080(3) 0.3988(5) 0.095(3) Uani 0.435(11) 1 d D U P F 1
Cl12 Cl 0.7321(3) 0.2879(3) 0.4559(4) 0.073(2) Uani 0.435(11) 1 d D U P F 1
C90 C 0.6751(6) 0.2652(8) 0.3941(11) 0.067(5) Uani 0.435(11) 1 d D U P F 1
H90A H 0.687665 0.262966 0.333971 0.080 Uiso 0.435(11) 1 calc R . P F 1
H90B H 0.664451 0.225967 0.412152 0.080 Uiso 0.435(11) 1 calc R . P F 1
Cl13 Cl 0.5807(3) 0.2944(4) 0.4308(4) 0.121(3) Uani 0.489(11) 1 d D U P G 2
Cl14 Cl 0.7037(5) 0.2932(5) 0.4430(7) 0.158(5) Uani 0.489(11) 1 d D U P G 2
C91 C 0.6458(7) 0.3208(16) 0.390(2) 0.17(2) Uani 0.489(11) 1 d D U P G 2
H91A H 0.648671 0.310736 0.328488 0.207 Uiso 0.489(11) 1 calc R . P G 2
H91B H 0.646286 0.363148 0.394246 0.207 Uiso 0.489(11) 1 calc R . P G 2
H3A H 0.624(2) 0.8255(18) 0.343(3) 0.023(12) Uiso 1 1 d D . . . .
H6A H 0.9154(17) 0.6814(18) 0.506(3) 0.025(12) Uiso 1 1 d D . . . .
H5A H 0.997(2) 0.6440(19) 0.455(4) 0.045(16) Uiso 1 1 d D . . . .
H8A H 0.8789(18) 0.766(2) 0.460(4) 0.043(16) Uiso 1 1 d D . . . .
H4A H 0.595(2) 0.7251(19) 0.355(3) 0.035(14) Uiso 1 1 d D . . . .
H8B H 0.857(3) 0.815(2) 0.392(3) 0.052(18) Uiso 1 1 d D . . . .
H7A H 0.832(2) 0.8675(13) 0.494(4) 0.037(15) Uiso 1 1 d D . . . .
H2A H 0.728(2) 0.699(2) 0.406(3) 0.041(16) Uiso 1 1 d D . . . .
H4B H 0.608(3) 0.732(3) 0.445(3) 0.07(2) Uiso 1 1 d D . . . .
H3B H 0.673(2) 0.777(3) 0.357(5) 0.06(2) Uiso 1 1 d D . . . .
H2B H 0.7777(17) 0.745(2) 0.400(3) 0.028(13) Uiso 1 1 d D . . . .
H1A H 0.787(3) 0.723(2) 0.255(3) 0.044(16) Uiso 1 1 d D . . . .
H1B H 0.804(2) 0.671(3) 0.308(5) 0.06(2) Uiso 1 1 d D . . . .
H7B H 0.7914(12) 0.819(2) 0.526(3) 0.022(12) Uiso 1 1 d D . . . .
H5B H 1.0105(19) 0.703(2) 0.405(4) 0.042(16) Uiso 1 1 d D . . . .
H6B H 0.966(4) 0.719(4) 0.539(4) 0.10(3) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 N2 1.456(5) . ?
N1 B1 1.631(6) . ?
N1 H1A 0.96(2) . ?
N1 H1B 0.96(2) . ?
N2 H2A 0.97(2) . ?
N2 H2B 0.98(2) . ?
N3 N4 1.459(5) . ?
N3 B2 1.626(6) . ?
N3 H3A 0.97(2) . ?
N3 H3B 0.97(3) . ?
N4 H4A 0.97(2) . ?
N4 H4B 0.97(3) . ?
N5 N6 1.456(5) . ?
N5 B3 1.625(7) . ?
N5 H5A 0.98(2) . ?
N5 H5B 0.97(2) . ?
N6 H6A 0.97(2) . ?
N6 H6B 0.97(3) . ?
N7 N8 1.459(5) . ?
N7 B4 1.618(6) . ?
N7 H7A 0.95(2) . ?
N7 H7B 0.96(2) . ?
N8 H8A 0.97(2) . ?
N8 H8B 0.97(2) . ?
C1 C2 1.416(7) . ?
C1 C14 1.401(6) . ?
C1 C15 1.424(7) . ?
C2 C3 1.523(6) . ?
C2 C11 1.389(6) . ?
C3 H3 0.9800 . ?
C3 C4 1.505(6) . ?
C3 C45 1.617(6) . ?
C4 C5 1.396(6) . ?
C4 C9 1.393(6) . ?
C5 C6 1.412(7) . ?
C5 C29 1.443(6) . ?
C6 H6 0.9300 . ?
C6 C7 1.387(7) . ?
C7 H7 0.9300 . ?
C7 C8 1.391(7) . ?
C8 H8 0.9300 . ?
C8 C9 1.402(7) . ?
C9 C10 1.529(6) . ?
C10 H10 0.9800 . ?
C10 C11 1.499(7) . ?
C10 C52 1.614(6) . ?
C11 C12 1.378(6) . ?
C12 H12 0.9300 . ?
C12 C13 1.412(8) . ?
C13 H13 0.9300 . ?
C13 C14 1.373(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.215(7) . ?
C16 B1 1.581(7) . ?
C17 C18 1.389(7) . ?
C17 C22 1.410(7) . ?
C17 B1 1.623(7) . ?
C18 H18 0.9300 . ?
C18 C19 1.406(8) . ?
C19 H19 0.9300 . ?
C19 C20 1.371(10) . ?
C20 H20 0.9300 . ?
C20 C21 1.379(10) . ?
C21 H21 0.9300 . ?
C21 C22 1.384(8) . ?
C22 H22 0.9300 . ?
C23 C24 1.405(6) . ?
C23 C28 1.406(7) . ?
C23 B1 1.612(7) . ?
C24 H24 0.9300 . ?
C24 C25 1.391(7) . ?
C25 H25 0.9300 . ?
C25 C26 1.382(8) . ?
C26 H26 0.9300 . ?
C26 C27 1.386(8) . ?
C27 H27 0.9300 . ?
C27 C28 1.379(7) . ?
C28 H28 0.9300 . ?
C29 C30 1.228(6) . ?
C30 B2 1.596(6) . ?
C31 C32 1.407(7) . ?
C31 C36 1.400(6) . ?
C31 B2 1.622(6) . ?
C32 H32 0.9300 . ?
C32 C33 1.388(6) . ?
C33 H33 0.9300 . ?
C33 C34 1.386(8) . ?
C34 H34 0.9300 . ?
C34 C35 1.397(8) . ?
C35 H35 0.9300 . ?
C35 C36 1.389(6) . ?
C36 H36 0.9300 . ?
C37 C38 1.403(6) . ?
C37 C42 1.401(7) . ?
C37 B2 1.622(6) . ?
C38 H38 0.9300 . ?
C38 C39 1.387(6) . ?
C39 H39 0.9300 . ?
C39 C40 1.386(9) . ?
C40 H40 0.9300 . ?
C40 C41 1.399(8) . ?
C41 H41 0.9300 . ?
C41 C42 1.388(7) . ?
C42 H42 0.9300 . ?
C43 C44 1.419(6) . ?
C43 C56 1.395(6) . ?
C43 C57 1.433(6) . ?
C44 C45 1.507(6) . ?
C44 C53 1.395(6) . ?
C45 H45 0.9800 . ?
C45 C46 1.527(6) . ?
C46 C47 1.406(6) . ?
C46 C51 1.400(6) . ?
C47 C48 1.401(7) . ?
C47 C71 1.435(6) . ?
C48 H48 0.9300 . ?
C48 C49 1.383(7) . ?
C49 H49 0.9300 . ?
C49 C50 1.385(7) . ?
C50 H50 0.9300 . ?
C50 C51 1.392(7) . ?
C51 C52 1.494(6) . ?
C52 H52 0.9800 . ?
C52 C53 1.532(7) . ?
C53 C54 1.395(6) . ?
C54 H54 0.9300 . ?
C54 C55 1.397(7) . ?
C55 H55 0.9300 . ?
C55 C56 1.375(7) . ?
C56 H56 0.9300 . ?
C57 C58 1.220(6) . ?
C58 B3 1.602(7) . ?
C59 C60 1.390(6) . ?
C59 C64 1.403(6) . ?
C59 B3 1.622(6) . ?
C60 H60 0.9300 . ?
C60 C61 1.397(6) . ?
C61 H61 0.9300 . ?
C61 C62 1.390(7) . ?
C62 H62 0.9300 . ?
C62 C63 1.384(7) . ?
C63 H63 0.9300 . ?
C63 C64 1.381(6) . ?
C64 H64 0.9300 . ?
C65 C66 1.403(7) . ?
C65 C70 1.398(6) . ?
C65 B3 1.620(7) . ?
C66 H66 0.9300 . ?
C66 C67 1.383(7) . ?
C67 H67 0.9300 . ?
C67 C68 1.403(8) . ?
C68 H68 0.9300 . ?
C68 C69 1.388(9) . ?
C69 H69 0.9300 . ?
C69 C70 1.399(7) . ?
C70 H70 0.9300 . ?
C71 C72 1.205(6) . ?
C72 B4 1.583(6) . ?
C73 C74 1.389(7) . ?
C73 C78 1.398(7) . ?
C73 B4 1.621(6) . ?
C74 H74 0.9300 . ?
C74 C75 1.405(7) . ?
C75 H75 0.9300 . ?
C75 C76 1.366(9) . ?
C76 H76 0.9300 . ?
C76 C77 1.389(10) . ?
C77 H77 0.9300 . ?
C77 C78 1.382(7) . ?
C78 H78 0.9300 . ?
C79 C80 1.404(6) . ?
C79 C84 1.391(7) . ?
C79 B4 1.603(7) . ?
C80 H80 0.9300 . ?
C80 C81 1.382(7) . ?
C81 H81 0.9300 . ?
C81 C82 1.382(8) . ?
C82 H82 0.9300 . ?
C82 C83 1.367(8) . ?
C83 H83 0.9300 . ?
C83 C84 1.403(7) . ?
C84 H84 0.9300 . ?
Cl1 C85 1.717(12) . ?
Cl2 C85 1.756(14) . ?
C85 H85A 0.9700 . ?
C85 H85B 0.9700 . ?
Cl3 C86 1.748(12) . ?
Cl4 C86 1.699(15) . ?
C86 H86A 0.9700 . ?
C86 H86B 0.9700 . ?
Cl5 C87 1.747(16) . ?
Cl6 C87 1.723(16) . ?
C87 H87A 0.9700 . ?
C87 H87B 0.9700 . ?
Cl7 C88 1.687(17) . ?
Cl8 C88 1.665(18) . ?
C88 H88A 0.9700 . ?
C88 H88B 0.9700 . ?
Cl9 C89 1.726(17) . ?
Cl10 C89 1.732(18) . ?
C89 H89A 0.9700 . ?
C89 H89B 0.9700 . ?
Cl11 C90 1.692(15) . ?
Cl12 C90 1.705(13) . ?
C90 H90A 0.9700 . ?
C90 H90B 0.9700 . ?
Cl13 C91 1.739(17) . ?
Cl14 C91 1.690(17) . ?
C91 H91A 0.9700 . ?
C91 H91B 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
N2 N1 B1 112.3(3) . . ?
N2 N1 H1A 107(4) . . ?
N2 N1 H1B 117(4) . . ?
B1 N1 H1A 111(4) . . ?
B1 N1 H1B 107(4) . . ?
H1A N1 H1B 102(6) . . ?
N1 N2 H2A 107(4) . . ?
N1 N2 H2B 107(3) . . ?
H2A N2 H2B 107(5) . . ?
N4 N3 B2 114.2(3) . . ?
N4 N3 H3A 103(3) . . ?
N4 N3 H3B 107(4) . . ?
B2 N3 H3A 110(3) . . ?
B2 N3 H3B 112(4) . . ?
H3A N3 H3B 111(5) . . ?
N3 N4 H4A 111(3) . . ?
N3 N4 H4B 103(5) . . ?
H4A N4 H4B 95(5) . . ?
N6 N5 B3 113.6(3) . . ?
N6 N5 H5A 107(4) . . ?
N6 N5 H5B 108(4) . . ?
B3 N5 H5A 112(4) . . ?
B3 N5 H5B 108(4) . . ?
H5A N5 H5B 109(5) . . ?
N5 N6 H6A 106(3) . . ?
N5 N6 H6B 113(6) . . ?
H6A N6 H6B 105(6) . . ?
N8 N7 B4 118.0(3) . . ?
N8 N7 H7A 108(4) . . ?
N8 N7 H7B 105(3) . . ?
B4 N7 H7A 108(4) . . ?
B4 N7 H7B 110(3) . . ?
H7A N7 H7B 106(4) . . ?
N7 N8 H8A 107(4) . . ?
N7 N8 H8B 108(4) . . ?
H8A N8 H8B 112(5) . . ?
C2 C1 C15 121.8(4) . . ?
C14 C1 C2 119.3(4) . . ?
C14 C1 C15 118.9(4) . . ?
C1 C2 C3 123.3(4) . . ?
C11 C2 C1 118.5(4) . . ?
C11 C2 C3 118.2(4) . . ?
C2 C3 H3 108.3 . . ?
C2 C3 C45 116.1(3) . . ?
C4 C3 C2 108.2(3) . . ?
C4 C3 H3 108.3 . . ?
C4 C3 C45 107.3(3) . . ?
C45 C3 H3 108.3 . . ?
C5 C4 C3 123.6(4) . . ?
C9 C4 C3 115.1(4) . . ?
C9 C4 C5 121.3(4) . . ?
C4 C5 C6 118.1(4) . . ?
C4 C5 C29 122.9(4) . . ?
C6 C5 C29 118.8(4) . . ?
C5 C6 H6 119.7 . . ?
C7 C6 C5 120.6(4) . . ?
C7 C6 H6 119.7 . . ?
C6 C7 H7 119.6 . . ?
C6 C7 C8 120.7(5) . . ?
C8 C7 H7 119.6 . . ?
C7 C8 H8 120.3 . . ?
C7 C8 C9 119.3(5) . . ?
C9 C8 H8 120.3 . . ?
C4 C9 C8 119.8(4) . . ?
C4 C9 C10 117.8(4) . . ?
C8 C9 C10 122.3(4) . . ?
C9 C10 H10 108.4 . . ?
C9 C10 C52 115.5(4) . . ?
C11 C10 C9 108.3(4) . . ?
C11 C10 H10 108.4 . . ?
C11 C10 C52 107.5(4) . . ?
C52 C10 H10 108.4 . . ?
C2 C11 C10 115.1(4) . . ?
C12 C11 C2 122.0(5) . . ?
C12 C11 C10 122.7(4) . . ?
C11 C12 H12 120.4 . . ?
C11 C12 C13 119.2(5) . . ?
C13 C12 H12 120.4 . . ?
C12 C13 H13 120.1 . . ?
C14 C13 C12 119.7(4) . . ?
C14 C13 H13 120.1 . . ?
C1 C14 H14 119.4 . . ?
C13 C14 C1 121.1(5) . . ?
C13 C14 H14 119.4 . . ?
C16 C15 C1 175.5(5) . . ?
C15 C16 B1 173.2(5) . . ?
C18 C17 C22 116.6(5) . . ?
C18 C17 B1 121.1(4) . . ?
C22 C17 B1 121.9(4) . . ?
C17 C18 H18 119.2 . . ?
C17 C18 C19 121.7(5) . . ?
C19 C18 H18 119.2 . . ?
C18 C19 H19 119.8 . . ?
C20 C19 C18 120.4(6) . . ?
C20 C19 H19 119.8 . . ?
C19 C20 H20 120.6 . . ?
C19 C20 C21 118.9(5) . . ?
C21 C20 H20 120.6 . . ?
C20 C21 H21 119.4 . . ?
C20 C21 C22 121.3(6) . . ?
C22 C21 H21 119.4 . . ?
C17 C22 H22 119.4 . . ?
C21 C22 C17 121.2(5) . . ?
C21 C22 H22 119.4 . . ?
C24 C23 C28 115.9(4) . . ?
C24 C23 B1 120.8(5) . . ?
C28 C23 B1 123.2(4) . . ?
C23 C24 H24 118.7 . . ?
C25 C24 C23 122.5(5) . . ?
C25 C24 H24 118.7 . . ?
C24 C25 H25 120.3 . . ?
C26 C25 C24 119.4(5) . . ?
C26 C25 H25 120.3 . . ?
C25 C26 H26 120.1 . . ?
C25 C26 C27 119.9(5) . . ?
C27 C26 H26 120.1 . . ?
C26 C27 H27 119.9 . . ?
C28 C27 C26 120.2(5) . . ?
C28 C27 H27 119.9 . . ?
C23 C28 H28 118.9 . . ?
C27 C28 C23 122.1(5) . . ?
C27 C28 H28 118.9 . . ?
C30 C29 C5 171.9(4) . . ?
C29 C30 B2 170.9(4) . . ?
C32 C31 B2 125.7(4) . . ?
C36 C31 C32 116.3(4) . . ?
C36 C31 B2 118.0(4) . . ?
C31 C32 H32 119.1 . . ?
C33 C32 C31 121.8(4) . . ?
C33 C32 H32 119.1 . . ?
C32 C33 H33 119.7 . . ?
C34 C33 C32 120.7(5) . . ?
C34 C33 H33 119.7 . . ?
C33 C34 H34 120.6 . . ?
C33 C34 C35 118.9(4) . . ?
C35 C34 H34 120.6 . . ?
C34 C35 H35 120.1 . . ?
C36 C35 C34 119.9(5) . . ?
C36 C35 H35 120.1 . . ?
C31 C36 H36 118.8 . . ?
C35 C36 C31 122.5(5) . . ?
C35 C36 H36 118.8 . . ?
C38 C37 B2 119.6(4) . . ?
C42 C37 C38 116.7(4) . . ?
C42 C37 B2 123.7(4) . . ?
C37 C38 H38 119.0 . . ?
C39 C38 C37 122.0(5) . . ?
C39 C38 H38 119.0 . . ?
C38 C39 H39 120.0 . . ?
C40 C39 C38 120.0(5) . . ?
C40 C39 H39 120.0 . . ?
C39 C40 H40 120.2 . . ?
C39 C40 C41 119.5(5) . . ?
C41 C40 H40 120.2 . . ?
C40 C41 H41 120.2 . . ?
C42 C41 C40 119.7(5) . . ?
C42 C41 H41 120.2 . . ?
C37 C42 H42 119.0 . . ?
C41 C42 C37 122.1(5) . . ?
C41 C42 H42 119.0 . . ?
C44 C43 C57 121.2(4) . . ?
C56 C43 C44 117.6(4) . . ?
C56 C43 C57 121.1(4) . . ?
C43 C44 C45 123.3(4) . . ?
C53 C44 C43 121.2(4) . . ?
C53 C44 C45 115.4(4) . . ?
C3 C45 H45 108.4 . . ?
C44 C45 C3 107.7(3) . . ?
C44 C45 H45 108.4 . . ?
C44 C45 C46 106.4(3) . . ?
C46 C45 C3 117.1(3) . . ?
C46 C45 H45 108.4 . . ?
C47 C46 C45 123.5(4) . . ?
C51 C46 C45 117.5(4) . . ?
C51 C46 C47 118.8(4) . . ?
C46 C47 C71 122.2(4) . . ?
C48 C47 C46 119.5(4) . . ?
C48 C47 C71 118.2(4) . . ?
C47 C48 H48 119.6 . . ?
C49 C48 C47 120.7(4) . . ?
C49 C48 H48 119.6 . . ?
C48 C49 H49 119.9 . . ?
C48 C49 C50 120.2(5) . . ?
C50 C49 H49 119.9 . . ?
C49 C50 H50 120.2 . . ?
C49 C50 C51 119.6(4) . . ?
C51 C50 H50 120.2 . . ?
C46 C51 C52 115.6(4) . . ?
C50 C51 C46 121.0(4) . . ?
C50 C51 C52 123.3(4) . . ?
C10 C52 H52 108.2 . . ?
C51 C52 C10 109.0(4) . . ?
C51 C52 H52 108.2 . . ?
C51 C52 C53 107.5(4) . . ?
C53 C52 C10 115.6(4) . . ?
C53 C52 H52 108.2 . . ?
C44 C53 C52 117.4(4) . . ?
C44 C53 C54 119.4(4) . . ?
C54 C53 C52 123.2(4) . . ?
C53 C54 H54 120.2 . . ?
C53 C54 C55 119.5(4) . . ?
C55 C54 H54 120.2 . . ?
C54 C55 H55 119.6 . . ?
C56 C55 C54 120.8(4) . . ?
C56 C55 H55 119.6 . . ?
C43 C56 H56 119.4 . . ?
C55 C56 C43 121.3(5) . . ?
C55 C56 H56 119.4 . . ?
C58 C57 C43 171.7(4) . . ?
C57 C58 B3 166.3(4) . . ?
C60 C59 C64 116.4(4) . . ?
C60 C59 B3 123.7(4) . . ?
C64 C59 B3 119.7(4) . . ?
C59 C60 H60 118.9 . . ?
C59 C60 C61 122.1(4) . . ?
C61 C60 H60 118.9 . . ?
C60 C61 H61 120.2 . . ?
C62 C61 C60 119.7(5) . . ?
C62 C61 H61 120.2 . . ?
C61 C62 H62 120.3 . . ?
C63 C62 C61 119.4(4) . . ?
C63 C62 H62 120.3 . . ?
C62 C63 H63 120.0 . . ?
C64 C63 C62 120.0(5) . . ?
C64 C63 H63 120.0 . . ?
C59 C64 H64 118.8 . . ?
C63 C64 C59 122.4(5) . . ?
C63 C64 H64 118.8 . . ?
C66 C65 B3 118.8(4) . . ?
C70 C65 C66 116.2(4) . . ?
C70 C65 B3 124.9(4) . . ?
C65 C66 H66 118.6 . . ?
C67 C66 C65 122.8(5) . . ?
C67 C66 H66 118.6 . . ?
C66 C67 H67 120.2 . . ?
C66 C67 C68 119.7(5) . . ?
C68 C67 H67 120.2 . . ?
C67 C68 H68 120.5 . . ?
C69 C68 C67 119.0(5) . . ?
C69 C68 H68 120.5 . . ?
C68 C69 H69 119.9 . . ?
C68 C69 C70 120.2(5) . . ?
C70 C69 H69 119.9 . . ?
C65 C70 C69 122.1(5) . . ?
C65 C70 H70 119.0 . . ?
C69 C70 H70 119.0 . . ?
C72 C71 C47 171.9(5) . . ?
C71 C72 B4 177.4(5) . . ?
C74 C73 C78 116.8(4) . . ?
C74 C73 B4 124.4(4) . . ?
C78 C73 B4 118.8(4) . . ?
C73 C74 H74 119.4 . . ?
C73 C74 C75 121.1(5) . . ?
C75 C74 H74 119.4 . . ?
C74 C75 H75 119.8 . . ?
C76 C75 C74 120.4(6) . . ?
C76 C75 H75 119.8 . . ?
C75 C76 H76 120.1 . . ?
C75 C76 C77 119.7(5) . . ?
C77 C76 H76 120.1 . . ?
C76 C77 H77 120.3 . . ?
C78 C77 C76 119.5(5) . . ?
C78 C77 H77 120.3 . . ?
C73 C78 H78 118.8 . . ?
C77 C78 C73 122.4(6) . . ?
C77 C78 H78 118.8 . . ?
C80 C79 B4 122.3(4) . . ?
C84 C79 C80 116.3(4) . . ?
C84 C79 B4 121.2(4) . . ?
C79 C80 H80 118.7 . . ?
C81 C80 C79 122.7(5) . . ?
C81 C80 H80 118.7 . . ?
C80 C81 H81 120.4 . . ?
C82 C81 C80 119.3(5) . . ?
C82 C81 H81 120.4 . . ?
C81 C82 H82 120.0 . . ?
C83 C82 C81 120.1(5) . . ?
C83 C82 H82 120.0 . . ?
C82 C83 H83 119.9 . . ?
C82 C83 C84 120.3(5) . . ?
C84 C83 H83 119.9 . . ?
C79 C84 C83 121.4(4) . . ?
C79 C84 H84 119.3 . . ?
C83 C84 H84 119.3 . . ?
C16 B1 N1 102.1(4) . . ?
C16 B1 C17 113.3(4) . . ?
C16 B1 C23 113.8(4) . . ?
C17 B1 N1 108.9(4) . . ?
C23 B1 N1 105.0(4) . . ?
C23 B1 C17 112.6(4) . . ?
C30 B2 N3 105.7(3) . . ?
C30 B2 C31 114.0(4) . . ?
C30 B2 C37 111.1(4) . . ?
C31 B2 N3 107.1(4) . . ?
C31 B2 C37 110.7(3) . . ?
C37 B2 N3 108.0(3) . . ?
C58 B3 N5 103.5(4) . . ?
C58 B3 C59 110.8(4) . . ?
C58 B3 C65 115.8(4) . . ?
C59 B3 N5 103.5(3) . . ?
C65 B3 N5 110.1(4) . . ?
C65 B3 C59 112.1(4) . . ?
N7 B4 C73 109.6(4) . . ?
C72 B4 N7 104.5(3) . . ?
C72 B4 C73 110.8(3) . . ?
C72 B4 C79 112.7(4) . . ?
C79 B4 N7 103.0(3) . . ?
C79 B4 C73 115.4(4) . . ?
Cl1 C85 Cl2 114.0(9) . . ?
Cl1 C85 H85A 108.7 . . ?
Cl1 C85 H85B 108.7 . . ?
Cl2 C85 H85A 108.7 . . ?
Cl2 C85 H85B 108.7 . . ?
H85A C85 H85B 107.6 . . ?
Cl3 C86 H86A 108.5 . . ?
Cl3 C86 H86B 108.5 . . ?
Cl4 C86 Cl3 115.0(9) . . ?
Cl4 C86 H86A 108.5 . . ?
Cl4 C86 H86B 108.5 . . ?
H86A C86 H86B 107.5 . . ?
Cl5 C87 H87A 108.4 . . ?
Cl5 C87 H87B 108.4 . . ?
Cl6 C87 Cl5 115.6(13) . . ?
Cl6 C87 H87A 108.4 . . ?
Cl6 C87 H87B 108.4 . . ?
H87A C87 H87B 107.4 . . ?
Cl7 C88 H88A 107.2 . . ?
Cl7 C88 H88B 107.2 . . ?
Cl8 C88 Cl7 120.7(15) . . ?
Cl8 C88 H88A 107.2 . . ?
Cl8 C88 H88B 107.2 . . ?
H88A C88 H88B 106.8 . . ?
Cl9 C89 Cl10 113.7(13) . . ?
Cl9 C89 H89A 108.8 . . ?
Cl9 C89 H89B 108.8 . . ?
Cl10 C89 H89A 108.8 . . ?
Cl10 C89 H89B 108.8 . . ?
H89A C89 H89B 107.7 . . ?
Cl11 C90 Cl12 115.4(10) . . ?
Cl11 C90 H90A 108.4 . . ?
Cl11 C90 H90B 108.4 . . ?
Cl12 C90 H90A 108.4 . . ?
Cl12 C90 H90B 108.4 . . ?
H90A C90 H90B 107.5 . . ?
Cl13 C91 H91A 109.2 . . ?
Cl13 C91 H91B 109.2 . . ?
Cl14 C91 Cl13 112.1(13) . . ?
Cl14 C91 H91A 109.2 . . ?
Cl14 C91 H91B 109.2 . . ?
H91A C91 H91B 107.9 . . ?

