# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_ga_ff18_4
_database_code_depnum_ccdc_archive 'CCDC 1815806'
_audit_update_record             
;
2018-01-17 deposited with the CCDC.
2018-02-05 downloaded from the CCDC.
;
_audit_creation_date             2017-02-22

_audit_block_code                ga_ff18
_audit_block_refno               2824
_audit_block_usercomment         'FF371, block, black'


_audit_creation_method           
;
Olex2 1.2
(compiled Aug 10 2017 17:44:14 for OlexSys, GUI svn.r5381)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C37 H29 F3 N2 O Ti, 1.5(C7 H8)'
_chemical_formula_sum            'C47.50 H41 F3 N2 O Ti'
_chemical_properties_physical    air-sensitive
_chemical_formula_weight         760.72
_chemical_melting_point          ?
_exptl_crystal_description       block
_exptl_crystal_colour            black
_diffrn_ambient_temperature      120(1)
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 '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'
_chemical_absolute_configuration .
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.83402(10)
_cell_length_b                   10.87734(15)
_cell_length_c                   19.1786(3)
_cell_angle_alpha                104.5042(12)
_cell_angle_beta                 103.2734(10)
_cell_angle_gamma                91.6813(10)
_cell_volume                     1924.82(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    34531
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      32.1440
_cell_measurement_theta_min      3.3430
_shelx_estimated_absorpt_T_max   0.973
_shelx_estimated_absorpt_T_min   0.973
_exptl_absorpt_coefficient_mu    0.276
_exptl_absorpt_correction_T_max  0.9546
_exptl_absorpt_correction_T_min  0.9322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             794
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 15 -1 0.0647
4 7 16 0.0851
-14 3 8 0.1318
1 -15 2 0.0955
13 -3 -10 0.1314
0 -2 26 0.0789
-6 -13 6 0.1187
0 2 -26 0.0634
0 9 -25 0.0833
4 14 -5 0.0655
2 7 19 0.0717
13 4 -14 0.1248
9 1 15 0.1247
8 -11 -8 0.1254
5 -9 21 0.1244
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.142
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
-0.9971 14.9956 -1.0018 -0.9949 0.0530 -0.0987
4.0001 6.9960 15.9935 -0.5521 -0.3197 -0.7604
-13.9949 3.0015 7.9955 -0.1944 1.0033 -0.1230
0.9971 -14.9957 2.0014 0.9904 -0.0542 0.0596
12.9952 -3.0012 -9.9949 0.2064 -0.9282 0.2170
-0.0000 -2.0010 25.9908 0.0163 -0.0286 -0.9963
-6.0002 -12.9951 5.9992 0.8598 0.4467 -0.0070
0.0000 2.0010 -25.9908 -0.0163 0.0286 0.9963
0.0012 8.9987 -24.9921 -0.4886 0.0177 0.8855
3.9973 14.1147 -4.6101 -0.9348 -0.3044 -0.0272
2.0481 7.3469 18.6745 -0.5818 -0.1815 -0.8381
13.0058 4.0686 -14.3671 -0.2464 -0.9334 0.3154
9.0624 1.3730 14.6098 -0.1853 -0.6781 -0.7284
8.0108 -11.0423 -7.6129 0.7483 -0.5578 0.2847
5.0676 -8.6896 20.8064 0.4715 -0.3814 -0.8048

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            98052
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.443
_diffrn_reflns_theta_min         2.493
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      7.00  96.00   0.50   15.00    --   27.02  57.00-120.00  178
  2  ω    -42.00  48.00   0.50   15.00    --   27.02 -57.00  90.00  180
  3  ω     -3.00  97.00   0.50   15.00    --   27.02  77.00 120.00  200
  4  ω    -20.00  69.00   0.50   15.00    --   27.02 -99.00  30.00  178
  5  ω    -20.00  69.00   0.50   15.00    --   27.02 -99.00-150.00  178
  6  ω    -45.00  53.00   0.50   15.00    --   27.02 -38.00 -30.00  196
  7  ω      2.00  99.00   0.50   15.00    --   27.02  38.00   0.00  194
  8  ω     -3.00  97.00   0.50   15.00    --   27.02  77.00  30.00  200
  9  ω    -43.00  57.00   0.50   15.00    --   27.02 -77.00 -90.00  200
 10  ω     -3.00  97.00   0.50   15.00    --   27.02  77.00-180.00  200
 11  ω      7.00  96.00   0.50   15.00    --   27.02  57.00   0.00  178
 12  ω    -42.00  48.00   0.50   15.00    --   27.02 -57.00 -90.00  180
 13  ω    -20.00  69.00   0.50   15.00    --   27.02 -99.00 150.00  178
 14  ω      2.00  99.00   0.50   15.00    --   27.02  38.00-180.00  194
 15  ω      2.00  99.00   0.50   15.00    --   27.02  38.00 -30.00  194
 16  ω     -3.00  97.00   0.50   15.00    --   27.02  77.00 -90.00  200
 17  φ      0.00 120.00   0.50   15.00  27.02  27.02  40.00    --   240
 18  φ      0.00 120.00   0.50   15.00  27.02  27.02 -60.00    --   240
 19  φ      0.00 120.00   0.50   15.00  27.02  27.02  60.00    --   240
 20  φ    120.00 240.00   0.50   15.00  27.02  27.02 -40.00    --   240
 21  φ    120.00 213.00   0.50   15.00  27.02  27.02  40.00    --   186
 22  φ      0.00 120.00   0.50   15.00  27.02  27.02 -40.00    --   240
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0030290000
_diffrn_orient_matrix_UB_12      -0.0668494000
_diffrn_orient_matrix_UB_13      -0.0045205000
_diffrn_orient_matrix_UB_21      -0.0726730000
_diffrn_orient_matrix_UB_22      -0.0013771000
_diffrn_orient_matrix_UB_23      -0.0012080000
_diffrn_orient_matrix_UB_31      -0.0157585000
_diffrn_orient_matrix_UB_32      -0.0102428000
_diffrn_orient_matrix_UB_33      -0.0391220000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10506
_reflns_number_total             13318
_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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-17); encifer 1.5.2 (CCDC, 2016)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_shelxl_version_number           2018/1
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         13318
_refine_ls_number_restraints     141
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0482
_refine_ls_restrained_S_all      1.012
_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)+(0.0748P)²+0.2469P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1257
_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. Restrained distances
 C51A-C57A \\sim C51B-C57B
 with sigma of 0.02
 C52A-C57A \\sim C56A-C57A \\sim C52B-C57B \\sim C56B-C57B
 with sigma of 0.02
3. Restrained atomic chiral volume
 C51A
 fixed at 0 with sigma of 0.1
 C51B
 fixed at 0 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C51A \\sim C52A \\sim C53A \\sim C54A \\sim C55A \\sim C56A \\sim C57A \\sim
C51B \\sim C52B \\sim C53B \\sim C54B \\sim C55B \\sim C56B \\sim C57B: within
0.5A with sigma of 0.02 and sigma for terminal atoms of 0.04
5. Rigid body (RIGU) restrains
 C51A, C52A, C53A, C54A, C55A, C56A, C57A, C51B, C52B, C53B, C54B, C55B, C56B,
 C57B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C51B)=Sof(C52B)=Sof(H52B)=Sof(C53B)=Sof(H53B)=Sof(C54B)=Sof(H54B)=
 Sof(C55B)=Sof(H55B)=Sof(C56B)=Sof(H56B)=Sof(C57B)=Sof(H57D)=Sof(H57E)=
 Sof(H57F)=1-FVAR(1)
 Sof(C51A)=Sof(C52A)=Sof(H52A)=Sof(C53A)=Sof(H53A)=Sof(C54A)=Sof(H54A)=
 Sof(C55A)=Sof(H55A)=Sof(C56A)=Sof(H56A)=Sof(C57A)=Sof(H57A)=Sof(H57B)=
 Sof(H57C)=FVAR(1)
 Fixed Sof: C61(0.5) C62(0.5) H62(0.5) C63(0.5) H63(0.5) C64(0.5) H64(0.5)
 C65(0.5) H65(0.5) C66(0.5) H66(0.5) C67(0.5) H67A(0.5) H67B(0.5) H67C(0.5)
7.a Ternary CH refined with riding coordinates:
 C35(H35)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C15(H15),
 C16(H16), C19(H19), C20(H20), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27),
  C28(H28), C30(H30), C31(H31), C33(H33), C34(H34), C52A(H52A), C53A(H53A),
 C54A(H54A), C55A(H55A), C56A(H56A), C52B(H52B), C53B(H53B), C54B(H54B),
 C55B(H55B), C56B(H56B), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66)
7.c Fitted hexagon refined as free rotating group:
 C51A(C52A,C53A,C54A,C55A,C56A), C51B(C52B,C53B,C54B,C55B,C56B), C61(C62,C63,
 C64,C65,C66)
7.d Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C57A(H57A,H57B,H57C), C57B(H57D,
 H57E,H57F), C67(H67A,H67B,H67C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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
Ti Ti 0.86061(2) 0.16227(2) 0.26763(2) 0.01435(6) Uani 1 1 d . . . . .
F1 F 0.34935(10) -0.39467(9) 0.22775(5) 0.0332(2) Uani 1 1 d . . . . .
F2 F 0.45675(11) 0.36925(9) -0.02463(5) 0.0332(2) Uani 1 1 d . . . . .
F3 F 1.24216(10) -0.20247(9) 0.41716(5) 0.0324(2) Uani 1 1 d . . . . .
O O 0.94295(10) 0.32067(9) 0.30263(5) 0.0220(2) Uani 1 1 d . . . . .
N1 N 0.88813(11) 0.08117(10) 0.16695(6) 0.0165(2) Uani 1 1 d . . . . .
N2 N 0.70479(11) 0.16523(10) 0.33313(6) 0.0168(2) Uani 1 1 d . . . . .
C1 C 0.79948(12) -0.02492(12) 0.15869(7) 0.0154(2) Uani 1 1 d . . . . .
C2 C 0.83289(14) -0.14910(13) 0.12070(7) 0.0190(2) Uani 1 1 d . . . . .
H2 H 0.777079 -0.223958 0.117621 0.023 Uiso 1 1 calc R . . . .
C3 C 0.94366(14) -0.15771(13) 0.08976(7) 0.0216(3) Uani 1 1 d . . . . .
H3 H 0.964861 -0.239239 0.064855 0.026 Uiso 1 1 calc R . . . .
C4 C 1.03010(13) -0.04631(14) 0.09370(7) 0.0199(3) Uani 1 1 d . . . . .
C5 C 1.14282(14) -0.05031(16) 0.05921(8) 0.0260(3) Uani 1 1 d . . . . .
H5 H 1.165541 -0.129978 0.032668 0.031 Uiso 1 1 calc R . . . .
C6 C 1.21973(15) 0.05971(17) 0.06369(8) 0.0297(3) Uani 1 1 d . . . . .
H6 H 1.295978 0.055593 0.040701 0.036 Uiso 1 1 calc R . . . .
C7 C 1.18708(15) 0.17758(17) 0.10166(8) 0.0285(3) Uani 1 1 d . . . . .
H7 H 1.240550 0.253344 0.104034 0.034 Uiso 1 1 calc R . . . .
C8 C 1.07695(14) 0.18472(15) 0.13597(8) 0.0232(3) Uani 1 1 d . . . . .
H8 H 1.055060 0.265158 0.161982 0.028 Uiso 1 1 calc R . . . .
C9 C 0.99823(12) 0.07326(13) 0.13219(7) 0.0174(2) Uani 1 1 d . . . . .
C10 C 0.68287(12) -0.00034(12) 0.18942(7) 0.0145(2) Uani 1 1 d . . . . .
C11 C 0.59822(12) -0.10389(11) 0.20172(7) 0.0147(2) Uani 1 1 d . . . . .
C12 C 0.45152(13) -0.10364(12) 0.18629(7) 0.0171(2) Uani 1 1 d . . . . .
H12 H 0.409180 -0.035196 0.169853 0.021 Uiso 1 1 calc R . . . .
C13 C 0.36691(14) -0.20077(13) 0.19444(7) 0.0207(3) Uani 1 1 d . . . . .
H13 H 0.267717 -0.200225 0.183168 0.025 Uiso 1 1 calc R . . . .
C14 C 0.43097(15) -0.29819(13) 0.21938(8) 0.0220(3) Uani 1 1 d . . . . .
C15 C 0.57440(15) -0.30203(13) 0.23660(7) 0.0214(3) Uani 1 1 d . . . . .
H15 H 0.615506 -0.370242 0.253854 0.026 Uiso 1 1 calc R . . . .
C16 C 0.65778(13) -0.20380(12) 0.22817(7) 0.0178(2) Uani 1 1 d . . . . .
H16 H 0.756937 -0.204564 0.240602 0.021 Uiso 1 1 calc R . . . .
C17 C 0.64171(12) 0.13331(11) 0.20609(7) 0.0146(2) Uani 1 1 d . . . . .
C18 C 0.59314(12) 0.19655(12) 0.14588(7) 0.0151(2) Uani 1 1 d . . . . .
C19 C 0.55228(14) 0.32140(12) 0.16055(7) 0.0189(2) Uani 1 1 d . . . . .
H19 H 0.556075 0.366704 0.210328 0.023 Uiso 1 1 calc R . . . .
C20 C 0.50628(15) 0.38019(13) 0.10360(8) 0.0231(3) Uani 1 1 d . . . . .
H20 H 0.478025 0.464270 0.114100 0.028 Uiso 1 1 calc R . . . .
C21 C 0.50274(15) 0.31369(13) 0.03185(8) 0.0225(3) Uani 1 1 d . . . . .
C22 C 0.54558(15) 0.19316(13) 0.01475(8) 0.0218(3) Uani 1 1 d . . . . .
H22 H 0.545001 0.150342 -0.035016 0.026 Uiso 1 1 calc R . . . .
C23 C 0.58990(14) 0.13513(12) 0.07201(7) 0.0187(2) Uani 1 1 d . . . . .
H23 H 0.618799 0.051373 0.060605 0.022 Uiso 1 1 calc R . . . .
C24 C 0.59578(13) 0.16941(11) 0.27592(7) 0.0151(2) Uani 1 1 d . . . . .
C25 C 0.46569(14) 0.20246(13) 0.28901(8) 0.0205(3) Uani 1 1 d . . . . .
H25 H 0.390228 0.209316 0.249555 0.025 Uiso 1 1 calc R . . . .
C26 C 0.44963(15) 0.22497(13) 0.36101(8) 0.0235(3) Uani 1 1 d . . . . .
H26 H 0.361367 0.245014 0.370874 0.028 Uiso 1 1 calc R . . . .
C27 C 0.56172(16) 0.21840(13) 0.41884(8) 0.0237(3) Uani 1 1 d . . . . .
H27 H 0.551227 0.233299 0.468210 0.028 Uiso 1 1 calc R . . . .
C28 C 0.68920(15) 0.18956(13) 0.40255(7) 0.0209(3) Uani 1 1 d . . . . .
H28 H 0.767407 0.187015 0.441701 0.025 Uiso 1 1 calc R . . . .
C29 C 0.98049(13) 0.03950(12) 0.32483(7) 0.0182(2) Uani 1 1 d . . . . .
C30 C 1.11510(14) 0.02329(14) 0.31244(7) 0.0224(3) Uani 1 1 d . . . . .
H30 H 1.146965 0.069552 0.282394 0.027 Uiso 1 1 calc R . . . .
C31 C 1.20367(15) -0.05806(15) 0.34254(8) 0.0252(3) Uani 1 1 d . . . . .
H31 H 1.293764 -0.068222 0.332874 0.030 Uiso 1 1 calc R . . . .
C32 C 1.15668(14) -0.12294(13) 0.38654(8) 0.0222(3) Uani 1 1 d . . . . .
C33 C 1.02664(15) -0.11113(13) 0.40174(8) 0.0225(3) Uani 1 1 d . . . . .
H33 H 0.996807 -0.156994 0.432538 0.027 Uiso 1 1 calc R . . . .
C34 C 0.94006(13) -0.02942(13) 0.37033(7) 0.0199(2) Uani 1 1 d . . . . .
H34 H 0.850110 -0.020411 0.380343 0.024 Uiso 1 1 calc R . . . .
C35 C 0.99200(16) 0.45256(14) 0.33104(9) 0.0291(3) Uani 1 1 d . . . . .
H35 H 1.001724 0.475875 0.385927 0.035 Uiso 1 1 calc R . . . .
C36 C 1.1351(2) 0.4737(2) 0.31813(13) 0.0518(5) Uani 1 1 d . . . . .
H36A H 1.198123 0.417401 0.339629 0.078 Uiso 1 1 calc GR . . . .
H36B H 1.172267 0.562711 0.341716 0.078 Uiso 1 1 calc GR . . . .
H36C H 1.127990 0.454630 0.264632 0.078 Uiso 1 1 calc GR . . . .
C37 C 0.8833(3) 0.5299(2) 0.29810(16) 0.0729(9) Uani 1 1 d . . . . .
H37A H 0.873179 0.510282 0.244330 0.109 Uiso 1 1 calc GR . . . .
H37B H 0.912605 0.620848 0.320447 0.109 Uiso 1 1 calc GR . . . .
H37C H 0.793252 0.508850 0.308045 0.109 Uiso 1 1 calc GR . . . .
C51A C 0.6421(10) 0.7740(5) 0.4451(5) 0.0208(12) Uani 0.53(3) 1 d D U P A 1
C52A C 0.7716(10) 0.7771(6) 0.4939(6) 0.0216(12) Uani 0.53(3) 1 d DG U P A 1
H52A H 0.828969 0.855342 0.515702 0.026 Uiso 0.53(3) 1 calc R . P A 1
C53A C 0.8170(12) 0.6658(8) 0.5108(6) 0.045(2) Uani 0.53(3) 1 d G U P A 1
H53A H 0.905488 0.667983 0.544149 0.053 Uiso 0.53(3) 1 calc R . P A 1
C54A C 0.7330(14) 0.5514(6) 0.4789(5) 0.056(2) Uani 0.53(3) 1 d G U P A 1
H54A H 0.764076 0.475347 0.490446 0.067 Uiso 0.53(3) 1 calc R . P A 1
C55A C 0.6036(13) 0.5483(5) 0.4301(5) 0.0405(15) Uani 0.53(3) 1 d G U P A 1
H55A H 0.546144 0.470068 0.408297 0.049 Uiso 0.53(3) 1 calc R . P A 1
C56A C 0.5581(11) 0.6596(6) 0.4132(4) 0.0253(11) Uani 0.53(3) 1 d DG U P A 1
H56A H 0.469622 0.657425 0.379850 0.030 Uiso 0.53(3) 1 calc R . P A 1
C57A C 0.5921(13) 0.8959(7) 0.4281(7) 0.027(2) Uani 0.53(3) 1 d D U P A 1
H57A H 0.647364 0.969332 0.465771 0.041 Uiso 0.53(3) 1 calc GR . P A 1
H57B H 0.492826 0.899350 0.428448 0.041 Uiso 0.53(3) 1 calc GR . P A 1
H57C H 0.603843 0.898031 0.378999 0.041 Uiso 0.53(3) 1 calc GR . P A 1
C51B C 0.6621(11) 0.7741(6) 0.4486(6) 0.0210(13) Uani 0.47(3) 1 d D U P A 2
C52B C 0.7885(11) 0.7823(6) 0.5008(7) 0.0285(16) Uani 0.47(3) 1 d DG U P A 2
H52B H 0.837624 0.863205 0.526914 0.034 Uiso 0.47(3) 1 calc R . P A 2
C53B C 0.8431(13) 0.6719(8) 0.5147(6) 0.0331(14) Uani 0.47(3) 1 d G U P A 2
H53B H 0.929476 0.677487 0.550397 0.040 Uiso 0.47(3) 1 calc R . P A 2
C54B C 0.7712(18) 0.5535(7) 0.4765(5) 0.050(2) Uani 0.47(3) 1 d G U P A 2
H54B H 0.808535 0.478086 0.486061 0.060 Uiso 0.47(3) 1 calc R . P A 2
C55B C 0.6448(19) 0.5454(6) 0.4244(6) 0.047(2) Uani 0.47(3) 1 d G U P A 2
H55B H 0.595743 0.464400 0.398242 0.057 Uiso 0.47(3) 1 calc R . P A 2
C56B C 0.5903(15) 0.6557(7) 0.4104(5) 0.0293(16) Uani 0.47(3) 1 d DG U P A 2
H56B H 0.503889 0.650116 0.374758 0.035 Uiso 0.47(3) 1 calc R . P A 2
C57B C 0.6019(15) 0.8928(10) 0.4327(8) 0.031(3) Uani 0.47(3) 1 d D U P A 2
H57D H 0.523479 0.911474 0.456061 0.046 Uiso 0.47(3) 1 calc GR . P A 2
H57E H 0.568493 0.879408 0.378861 0.046 Uiso 0.47(3) 1 calc GR . P A 2
H57F H 0.674673 0.964594 0.452695 0.046 Uiso 0.47(3) 1 calc GR . P A 2
C61 C 0.9449(2) -0.5147(3) 0.03288(14) 0.0305(6) Uani 0.5 1 d . . P B -3
C62 C 1.0890(3) -0.4857(2) 0.05966(10) 0.0276(9) Uani 0.5 1 d G . P B -3
H62 H 1.132046 -0.480132 0.110188 0.033 Uiso 0.5 1 calc R . P B -3
C63 C 1.17031(18) -0.4648(3) 0.01252(16) 0.0406(8) Uani 0.5 1 d G . P B -3
H63 H 1.268861 -0.444960 0.030819 0.049 Uiso 0.5 1 calc R . P B -3
C64 C 1.1074(3) -0.4729(3) -0.06141(15) 0.0485(12) Uani 0.5 1 d G . P B -3
H64 H 1.162941 -0.458605 -0.093631 0.058 Uiso 0.5 1 calc R . P B -3
C65 C 0.9632(3) -0.5019(3) -0.08819(10) 0.0471(10) Uani 0.5 1 d G . P B -3
H65 H 0.920205 -0.507420 -0.138713 0.056 Uiso 0.5 1 calc R . P B -3
C66 C 0.88193(18) -0.5228(2) -0.04104(15) 0.0307(9) Uani 0.5 1 d G . P B -3
H66 H 0.783386 -0.542592 -0.059345 0.037 Uiso 0.5 1 calc R . P B -3
C67 C 0.8569(5) -0.5364(5) 0.0832(3) 0.0495(11) Uani 0.5 1 d . . P B -3
H67A H 0.768528 -0.497590 0.072146 0.074 Uiso 0.5 1 calc GR . P B -3
H67B H 0.907381 -0.497658 0.134964 0.074 Uiso 0.5 1 calc GR . P B -3
H67C H 0.836986 -0.628242 0.075695 0.074 Uiso 0.5 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
Ti O 1.7788(10) . ?
Ti N1 1.9951(11) . ?
Ti N2 2.1894(11) . ?
Ti C1 2.4685(12) . ?
Ti C10 2.3915(12) . ?
Ti C17 2.1757(12) . ?
Ti C24 2.6476(12) . ?
Ti C29 2.1468(13) . ?
F1 C14 1.3659(15) . ?
F2 C21 1.3646(15) . ?
F3 C32 1.3675(15) . ?
O C35 1.4265(17) . ?
N1 C1 1.3794(16) . ?
N1 C9 1.3901(16) . ?
N2 C24 1.3574(15) . ?
N2 C28 1.3364(17) . ?
C1 C2 1.4513(17) . ?
C1 C10 1.4084(17) . ?
C2 H2 0.9500 . ?
C2 C3 1.3499(18) . ?
C3 H3 0.9500 . ?
C3 C4 1.436(2) . ?
C4 C5 1.4119(18) . ?
C4 C9 1.4085(19) . ?
C5 H5 0.9500 . ?
C5 C6 1.370(2) . ?
C6 H6 0.9500 . ?
C6 C7 1.393(2) . ?
C7 H7 0.9500 . ?
C7 C8 1.385(2) . ?
C8 H8 0.9500 . ?
C8 C9 1.3962(19) . ?
C10 C11 1.4783(17) . ?
C10 C17 1.4970(16) . ?
C11 C12 1.4048(17) . ?
C11 C16 1.3994(17) . ?
C12 H12 0.9500 . ?
C12 C13 1.3869(18) . ?
C13 H13 0.9500 . ?
C13 C14 1.3796(19) . ?
C14 C15 1.377(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.3914(19) . ?
C16 H16 0.9500 . ?
C17 C18 1.4827(17) . ?
C17 C24 1.4754(17) . ?
C18 C19 1.4062(17) . ?
C18 C23 1.3994(18) . ?
C19 H19 0.9500 . ?
C19 C20 1.3951(18) . ?
C20 H20 0.9500 . ?
C20 C21 1.377(2) . ?
C21 C22 1.373(2) . ?
C22 H22 0.9500 . ?
C22 C23 1.3922(18) . ?
C23 H23 0.9500 . ?
C24 C25 1.3993(17) . ?
C25 H25 0.9500 . ?
C25 C26 1.387(2) . ?
C26 H26 0.9500 . ?
C26 C27 1.390(2) . ?
C27 H27 0.9500 . ?
C27 C28 1.3861(19) . ?
C28 H28 0.9500 . ?
C29 C30 1.4061(18) . ?
C29 C34 1.3969(19) . ?
C30 H30 0.9500 . ?
C30 C31 1.3946(19) . ?
C31 H31 0.9500 . ?
C31 C32 1.372(2) . ?
C32 C33 1.378(2) . ?
C33 H33 0.9500 . ?
C33 C34 1.3981(18) . ?
C34 H34 0.9500 . ?
C35 H35 1.0000 . ?
C35 C36 1.504(3) . ?
C35 C37 1.502(2) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C51A C52A 1.3900 . ?
C51A C56A 1.3900 . ?
C51A C57A 1.513(6) . ?
C52A H52A 0.9500 . ?
C52A C53A 1.3900 . ?
C53A H53A 0.9500 . ?
C53A C54A 1.3900 . ?
C54A H54A 0.9500 . ?
C54A C55A 1.3900 . ?
C55A H55A 0.9500 . ?
C55A C56A 1.3900 . ?
C56A H56A 0.9500 . ?
C57A H57A 0.9800 . ?
C57A H57B 0.9800 . ?
C57A H57C 0.9800 . ?
C51B C52B 1.3900 . ?
C51B C56B 1.3900 . ?
C51B C57B 1.506(7) . ?
C52B H52B 0.9500 . ?
C52B C53B 1.3900 . ?
C53B H53B 0.9500 . ?
C53B C54B 1.3900 . ?
C54B H54B 0.9500 . ?
C54B C55B 1.3900 . ?
C55B H55B 0.9500 . ?
C55B C56B 1.3900 . ?
C56B H56B 0.9500 . ?
C57B H57D 0.9800 . ?
C57B H57E 0.9800 . ?
C57B H57F 0.9800 . ?
C61 C62 1.3900 . ?
C61 C66 1.3900 . ?
C61 C67 1.491(5) . ?
C62 H62 0.9500 . ?
C62 C63 1.3900 . ?
C63 H63 0.9500 . ?
C63 C64 1.3900 . ?
C64 H64 0.9500 . ?
C64 C65 1.3900 . ?
C65 H65 0.9500 . ?
C65 C66 1.3900 . ?
C66 H66 0.9500 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 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
O Ti N1 111.32(5) . . ?
O Ti N2 102.01(4) . . ?
O Ti C1 144.93(5) . . ?
O Ti C10 154.71(4) . . ?
O Ti C17 118.52(5) . . ?
O Ti C24 107.91(4) . . ?
O Ti C29 109.47(5) . . ?
N1 Ti N2 140.55(4) . . ?
N1 Ti C1 33.95(4) . . ?
N1 Ti C10 64.11(4) . . ?
N1 Ti C17 81.70(4) . . ?
N1 Ti C24 115.09(4) . . ?
N1 Ti C29 97.09(5) . . ?
N2 Ti C1 109.05(4) . . ?
N2 Ti C10 76.70(4) . . ?
N2 Ti C24 30.78(4) . . ?
C1 Ti C24 91.62(4) . . ?
C10 Ti C1 33.64(4) . . ?
C10 Ti C24 58.47(4) . . ?
C17 Ti N2 63.73(4) . . ?
C17 Ti C1 64.58(4) . . ?
C17 Ti C10 37.89(4) . . ?
C17 Ti C24 33.86(4) . . ?
C29 Ti N2 90.92(5) . . ?
C29 Ti C1 86.29(4) . . ?
C29 Ti C10 95.82(4) . . ?
C29 Ti C17 128.88(5) . . ?
C29 Ti C24 115.64(4) . . ?
C35 O Ti 172.86(10) . . ?
C1 N1 Ti 92.19(7) . . ?
C1 N1 C9 121.24(11) . . ?
C9 N1 Ti 136.67(9) . . ?
C24 N2 Ti 93.61(8) . . ?
C28 N2 Ti 143.32(9) . . ?
C28 N2 C24 120.81(11) . . ?
N1 C1 Ti 53.87(6) . . ?
N1 C1 C2 118.86(11) . . ?
N1 C1 C10 115.07(11) . . ?
C2 C1 Ti 148.35(9) . . ?
C10 C1 Ti 70.18(7) . . ?
C10 C1 C2 126.07(12) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 C1 119.67(13) . . ?
C3 C2 H2 120.2 . . ?
C2 C3 H3 119.3 . . ?
C2 C3 C4 121.41(12) . . ?
C4 C3 H3 119.3 . . ?
C5 C4 C3 123.30(13) . . ?
C9 C4 C3 118.24(11) . . ?
C9 C4 C5 118.44(13) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 C4 120.56(14) . . ?
C6 C5 H5 119.7 . . ?
C5 C6 H6 119.7 . . ?
C5 C6 C7 120.57(13) . . ?
C7 C6 H6 119.7 . . ?
C6 C7 H7 119.9 . . ?
C8 C7 C6 120.25(15) . . ?
C8 C7 H7 119.9 . . ?
C7 C8 H8 120.1 . . ?
C7 C8 C9 119.76(14) . . ?
C9 C8 H8 120.1 . . ?
N1 C9 C4 120.17(12) . . ?
N1 C9 C8 119.42(12) . . ?
C8 C9 C4 120.41(12) . . ?
C1 C10 Ti 76.18(7) . . ?
C1 C10 C11 121.45(11) . . ?
C1 C10 C17 118.20(11) . . ?
C11 C10 Ti 134.59(8) . . ?
C11 C10 C17 120.28(10) . . ?
C17 C10 Ti 63.22(6) . . ?
C12 C11 C10 119.37(11) . . ?
C16 C11 C10 122.83(11) . . ?
C16 C11 C12 117.81(12) . . ?
C11 C12 H12 119.2 . . ?
C13 C12 C11 121.69(12) . . ?
C13 C12 H12 119.2 . . ?
C12 C13 H13 121.0 . . ?
C14 C13 C12 118.08(12) . . ?
C14 C13 H13 121.0 . . ?
F1 C14 C13 118.91(12) . . ?
F1 C14 C15 118.43(12) . . ?
C15 C14 C13 122.66(12) . . ?
C14 C15 H15 120.7 . . ?
C14 C15 C16 118.53(12) . . ?
C16 C15 H15 120.7 . . ?
C11 C16 H16 119.4 . . ?
C15 C16 C11 121.20(12) . . ?
C15 C16 H16 119.4 . . ?
C10 C17 Ti 78.89(7) . . ?
C18 C17 Ti 120.26(8) . . ?
C18 C17 C10 121.09(10) . . ?
C24 C17 Ti 90.89(7) . . ?
C24 C17 C10 112.47(10) . . ?
C24 C17 C18 121.29(10) . . ?
C19 C18 C17 121.74(11) . . ?
C23 C18 C17 121.04(11) . . ?
C23 C18 C19 117.20(11) . . ?
C18 C19 H19 119.3 . . ?
C20 C19 C18 121.44(12) . . ?
C20 C19 H19 119.3 . . ?
C19 C20 H20 120.7 . . ?
C21 C20 C19 118.55(12) . . ?
C21 C20 H20 120.7 . . ?
F2 C21 C20 119.34(12) . . ?
F2 C21 C22 118.29(13) . . ?
C22 C21 C20 122.36(12) . . ?
C21 C22 H22 120.8 . . ?
C21 C22 C23 118.47(13) . . ?
C23 C22 H22 120.8 . . ?
C18 C23 H23 119.0 . . ?
C22 C23 C18 121.93(12) . . ?
C22 C23 H23 119.0 . . ?
N2 C24 Ti 55.62(6) . . ?
N2 C24 C17 108.82(10) . . ?
N2 C24 C25 120.39(11) . . ?
C17 C24 Ti 55.25(6) . . ?
C25 C24 Ti 166.84(9) . . ?
C25 C24 C17 130.79(11) . . ?
C24 C25 H25 120.8 . . ?
C26 C25 C24 118.37(12) . . ?
C26 C25 H25 120.8 . . ?
C25 C26 H26 119.8 . . ?
C25 C26 C27 120.50(13) . . ?
C27 C26 H26 119.8 . . ?
C26 C27 H27 120.9 . . ?
C28 C27 C26 118.25(13) . . ?
C28 C27 H27 120.9 . . ?
N2 C28 C27 121.62(13) . . ?
N2 C28 H28 119.2 . . ?
C27 C28 H28 119.2 . . ?
C30 C29 Ti 115.37(10) . . ?
C34 C29 Ti 128.38(9) . . ?
C34 C29 C30 116.21(12) . . ?
C29 C30 H30 118.7 . . ?
C31 C30 C29 122.57(13) . . ?
C31 C30 H30 118.7 . . ?
C30 C31 H31 121.0 . . ?
C32 C31 C30 117.95(13) . . ?
C32 C31 H31 121.0 . . ?
F3 C32 C31 119.00(12) . . ?
F3 C32 C33 118.19(13) . . ?
C31 C32 C33 122.81(12) . . ?
C32 C33 H33 121.1 . . ?
C32 C33 C34 117.81(13) . . ?
C34 C33 H33 121.1 . . ?
C29 C34 C33 122.64(12) . . ?
C29 C34 H34 118.7 . . ?
C33 C34 H34 118.7 . . ?
O C35 H35 107.7 . . ?
O C35 C36 109.59(13) . . ?
O C35 C37 108.93(13) . . ?
C36 C35 H35 107.7 . . ?
C37 C35 H35 107.7 . . ?
C37 C35 C36 114.86(19) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C52A C51A C56A 120.0 . . ?
C52A C51A C57A 119.7(4) . . ?
C56A C51A C57A 120.3(4) . . ?
C51A C52A H52A 120.0 . . ?
C51A C52A C53A 120.0 . . ?
C53A C52A H52A 120.0 . . ?
C52A C53A H53A 120.0 . . ?
C54A C53A C52A 120.0 . . ?
C54A C53A H53A 120.0 . . ?
C53A C54A H54A 120.0 . . ?
C53A C54A C55A 120.0 . . ?
C55A C54A H54A 120.0 . . ?
C54A C55A H55A 120.0 . . ?
C54A C55A C56A 120.0 . . ?
C56A C55A H55A 120.0 . . ?
C51A C56A H56A 120.0 . . ?
C55A C56A C51A 120.0 . . ?
C55A C56A H56A 120.0 . . ?
C51A C57A H57A 109.5 . . ?
C51A C57A H57B 109.5 . . ?
C51A C57A H57C 109.5 . . ?
H57A C57A H57B 109.5 . . ?
H57A C57A H57C 109.5 . . ?
H57B C57A H57C 109.5 . . ?
C52B C51B C56B 120.0 . . ?
C52B C51B C57B 120.6(5) . . ?
C56B C51B C57B 119.4(5) . . ?
C51B C52B H52B 120.0 . . ?
C51B C52B C53B 120.0 . . ?
C53B C52B H52B 120.0 . . ?
C52B C53B H53B 120.0 . . ?
C54B C53B C52B 120.0 . . ?
C54B C53B H53B 120.0 . . ?
C53B C54B H54B 120.0 . . ?
C55B C54B C53B 120.0 . . ?
C55B C54B H54B 120.0 . . ?
C54B C55B H55B 120.0 . . ?
C54B C55B C56B 120.0 . . ?
C56B C55B H55B 120.0 . . ?
C51B C56B H56B 120.0 . . ?
C55B C56B C51B 120.0 . . ?
C55B C56B H56B 120.0 . . ?
C51B C57B H57D 109.5 . . ?
C51B C57B H57E 109.5 . . ?
C51B C57B H57F 109.5 . . ?
H57D C57B H57E 109.5 . . ?
H57D C57B H57F 109.5 . . ?
H57E C57B H57F 109.5 . . ?
C62 C61 C66 120.0 . . ?
C62 C61 C67 120.3(3) . . ?
C66 C61 C67 119.7(3) . . ?
C61 C62 H62 120.0 . . ?
C61 C62 C63 120.0 . . ?
C63 C62 H62 120.0 . . ?
C62 C63 H63 120.0 . . ?
C64 C63 C62 120.0 . . ?
C64 C63 H63 120.0 . . ?
C63 C64 H64 120.0 . . ?
C63 C64 C65 120.0 . . ?
C65 C64 H64 120.0 . . ?
C64 C65 H65 120.0 . . ?
C64 C65 C66 120.0 . . ?
C66 C65 H65 120.0 . . ?
C61 C66 H66 120.0 . . ?
C65 C66 C61 120.0 . . ?
C65 C66 H66 120.0 . . ?
C61 C67 H67A 109.5 . . ?
C61 C67 H67B 109.5 . . ?
C61 C67 H67C 109.5 . . ?
H67A C67 H67B 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 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
Ti N1 C1 C2 -143.23(10) . . . . ?
Ti N1 C1 C10 36.40(10) . . . . ?
Ti N1 C9 C4 128.65(12) . . . . ?
Ti N1 C9 C8 -51.17(17) . . . . ?
Ti N2 C24 C17 15.69(10) . . . . ?
Ti N2 C24 C25 -165.13(11) . . . . ?
Ti N2 C28 C27 158.17(12) . . . . ?
Ti C1 C2 C3 -71.7(2) . . . . ?
Ti C1 C10 C11 -134.18(11) . . . . ?
Ti C1 C10 C17 48.81(9) . . . . ?
Ti C10 C11 C12 118.15(12) . . . . ?
Ti C10 C11 C16 -62.02(17) . . . . ?
Ti C10 C17 C18 118.77(11) . . . . ?
Ti C10 C17 C24 -86.32(9) . . . . ?
Ti C17 C18 C19 -85.66(13) . . . . ?
Ti C17 C18 C23 92.53(13) . . . . ?
Ti C17 C24 N2 -15.76(10) . . . . ?
Ti C17 C24 C25 165.18(13) . . . . ?
Ti C24 C25 C26 -71.3(4) . . . . ?
Ti C29 C30 C31 -176.86(11) . . . . ?
Ti C29 C34 C33 176.93(10) . . . . ?
F1 C14 C15 C16 -179.95(12) . . . . ?
F2 C21 C22 C23 -178.73(12) . . . . ?
F3 C32 C33 C34 179.87(12) . . . . ?
N1 C1 C2 C3 -4.62(18) . . . . ?
N1 C1 C10 Ti -30.63(9) . . . . ?
N1 C1 C10 C11 -164.81(10) . . . . ?
N1 C1 C10 C17 18.18(16) . . . . ?
N2 C24 C25 C26 -2.86(19) . . . . ?
C1 N1 C9 C4 -6.43(17) . . . . ?
C1 N1 C9 C8 173.74(11) . . . . ?
C1 C2 C3 C4 0.17(19) . . . . ?
C1 C10 C11 C12 -139.75(12) . . . . ?
C1 C10 C11 C16 40.08(18) . . . . ?
C1 C10 C17 Ti -54.94(10) . . . . ?
C1 C10 C17 C18 63.82(15) . . . . ?
C1 C10 C17 C24 -141.26(11) . . . . ?
C2 C1 C10 Ti 148.97(12) . . . . ?
C2 C1 C10 C11 14.79(19) . . . . ?
C2 C1 C10 C17 -162.22(11) . . . . ?
C2 C3 C4 C5 -176.94(13) . . . . ?
C2 C3 C4 C9 1.23(19) . . . . ?
C3 C4 C5 C6 178.63(13) . . . . ?
C3 C4 C9 N1 1.82(17) . . . . ?
C3 C4 C9 C8 -178.37(12) . . . . ?
C4 C5 C6 C7 -0.7(2) . . . . ?
C5 C4 C9 N1 -179.93(11) . . . . ?
C5 C4 C9 C8 -0.11(18) . . . . ?
C5 C6 C7 C8 0.6(2) . . . . ?
C6 C7 C8 C9 -0.2(2) . . . . ?
C7 C8 C9 N1 179.81(12) . . . . ?
C7 C8 C9 C4 -0.01(19) . . . . ?
C9 N1 C1 Ti 151.00(12) . . . . ?
C9 N1 C1 C2 7.77(17) . . . . ?
C9 N1 C1 C10 -172.60(11) . . . . ?
C9 C4 C5 C6 0.47(19) . . . . ?
C10 C1 C2 C3 175.79(12) . . . . ?
C10 C11 C12 C13 177.77(12) . . . . ?
C10 C11 C16 C15 -177.72(12) . . . . ?
C10 C17 C18 C19 179.11(11) . . . . ?
C10 C17 C18 C23 -2.71(18) . . . . ?
C10 C17 C24 Ti 78.34(9) . . . . ?
C10 C17 C24 N2 62.57(13) . . . . ?
C10 C17 C24 C25 -116.49(14) . . . . ?
C11 C10 C17 Ti 128.02(10) . . . . ?
C11 C10 C17 C18 -113.22(13) . . . . ?
C11 C10 C17 C24 41.70(15) . . . . ?
C11 C12 C13 C14 0.9(2) . . . . ?
C12 C11 C16 C15 2.11(19) . . . . ?
C12 C13 C14 F1 180.00(12) . . . . ?
C12 C13 C14 C15 0.3(2) . . . . ?
C13 C14 C15 C16 -0.3(2) . . . . ?
C14 C15 C16 C11 -1.0(2) . . . . ?
C16 C11 C12 C13 -2.07(19) . . . . ?
C17 C10 C11 C12 37.20(17) . . . . ?
C17 C10 C11 C16 -142.98(12) . . . . ?
C17 C18 C19 C20 -179.81(12) . . . . ?
C17 C18 C23 C22 -179.55(12) . . . . ?
C17 C24 C25 C26 176.10(13) . . . . ?
C18 C17 C24 Ti -126.81(12) . . . . ?
C18 C17 C24 N2 -142.57(11) . . . . ?
C18 C17 C24 C25 38.4(2) . . . . ?
C18 C19 C20 C21 -0.6(2) . . . . ?
C19 C18 C23 C22 -1.28(19) . . . . ?
C19 C20 C21 F2 179.37(12) . . . . ?
C19 C20 C21 C22 -1.4(2) . . . . ?
C20 C21 C22 C23 2.1(2) . . . . ?
C21 C22 C23 C18 -0.7(2) . . . . ?
C23 C18 C19 C20 1.94(19) . . . . ?
C24 N2 C28 C27 0.7(2) . . . . ?
C24 C17 C18 C19 26.40(18) . . . . ?
C24 C17 C18 C23 -155.42(12) . . . . ?
C24 C25 C26 C27 1.9(2) . . . . ?
C25 C26 C27 C28 0.3(2) . . . . ?
C26 C27 C28 N2 -1.7(2) . . . . ?
C28 N2 C24 Ti 166.71(14) . . . . ?
C28 N2 C24 C17 -177.59(11) . . . . ?
C28 N2 C24 C25 1.58(19) . . . . ?
C29 C30 C31 C32 -0.8(2) . . . . ?
C30 C29 C34 C33 -0.5(2) . . . . ?
C30 C31 C32 F3 -179.48(13) . . . . ?
C30 C31 C32 C33 0.2(2) . . . . ?
C31 C32 C33 C34 0.2(2) . . . . ?
C32 C33 C34 C29 0.0(2) . . . . ?
C34 C29 C30 C31 0.9(2) . . . . ?
C51A C52A C53A C54A 0.0 . . . . ?
C52A C51A C56A C55A 0.0 . . . . ?
C52A C53A C54A C55A 0.0 . . . . ?
C53A C54A C55A C56A 0.0 . . . . ?
C54A C55A C56A C51A 0.0 . . . . ?
C56A C51A C52A C53A 0.0 . . . . ?
C57A C51A C52A C53A 178.9(8) . . . . ?
C57A C51A C56A C55A -178.9(8) . . . . ?
C51B C52B C53B C54B 0.0 . . . . ?
C52B C51B C56B C55B 0.0 . . . . ?
C52B C53B C54B C55B 0.0 . . . . ?
C53B C54B C55B C56B 0.0 . . . . ?
C54B C55B C56B C51B 0.0 . . . . ?
C56B C51B C52B C53B 0.0 . . . . ?
C57B C51B C52B C53B -179.7(10) . . . . ?
C57B C51B C56B C55B 179.8(9) . . . . ?
C61 C62 C63 C64 0.0 . . . . ?
C62 C61 C66 C65 0.0 . . . . ?
C62 C63 C64 C65 0.0 . . . . ?
C63 C64 C65 C66 0.0 . . . . ?
C64 C65 C66 C61 0.0 . . . . ?
C66 C61 C62 C63 0.0 . . . . ?
C67 C61 C62 C63 -179.6(4) . . . . ?
C67 C61 C66 C65 179.6(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.257
_oxdiff_exptl_absorpt_empirical_full_min 0.812
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.9324 83517 17618 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.0676 0 17617 nmt 1.0030 -0.0006 0.0022 0.0167 1.0063 0.0134 -0.1013 -0.0910
0.9760

_twin_special_details            
;
Component 2 rotated by 3.9300°
 around [-0.68 0.73 0.09] (reciprocal) or [-0.74 0.67 0.03] (direct)
;
_cell_oxdiff_length_a            9.83402(10)
_cell_oxdiff_length_b            10.87734(15)
_cell_oxdiff_length_c            19.1786(3)
_cell_oxdiff_angle_alpha         104.5042(12)
_cell_oxdiff_angle_beta          103.2734(10)
_cell_oxdiff_angle_gamma         91.6813(10)
_cell_oxdiff_volume              1924.83(4)
_cell_oxdiff_measurement_reflns_used 34531
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_ambient_environment      'perfluoro polyether oil / N~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_ga_tro67
_database_code_depnum_ccdc_archive 'CCDC 1817689'
_audit_update_record             
;
2018-01-17 deposited with the CCDC.
2018-02-05 downloaded from the CCDC.
;
_audit_creation_date             
;
'Thu Apr 10 16:53:26 2014'
;

_audit_block_code                ga_tro67
_audit_block_refno               2008
_audit_block_usercomment         'tr1218, needle, colourless'


_audit_creation_method           
;
Olex2 1.2
(compiled Aug 10 2017 17:44:14 for OlexSys, GUI svn.r5381)
;


# start Validation Reply Form
_vrf_RINTA01_ga_tro67            
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: very weak dataset.
;
_vrf_PLAT020_ga_tro67            
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.183 Report
RESPONSE: see _vrf_RINTA01_ga_tro67
;
_vrf_PLAT340_ga_tro67            
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01169 Ang.
RESPONSE: see _vrf_RINTA01_ga_tro67
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C24 H16 F2 N2'
_chemical_formula_sum            'C24 H16 F2 N2'
_chemical_formula_weight         370.39
_space_group_crystal_system      trigonal
_space_group_IT_number           145
_space_group_name_H-M_alt        'P 32'
_space_group_name_Hall           'P 32'
_chemical_absolute_configuration unk
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
_chemical_melting_point          ?
_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_diffrn_ambient_temperature      110(1)
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

_cell_length_a                   28.9605(16)
_cell_length_b                   28.9605(16)
_cell_length_c                   5.6946(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4136.3(5)
_cell_formula_units_Z            9
_cell_measurement_reflns_used    3963
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      19.2960
_cell_measurement_theta_min      3.6490
_shelx_estimated_absorpt_T_max   0.997
_shelx_estimated_absorpt_T_min   0.973
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.291
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.035
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1830
_diffrn_reflns_av_unetI/netI     0.1180
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            76183
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.155
_diffrn_reflns_theta_max         25.155
_diffrn_reflns_theta_min         3.249
_diffrn_detector_area_resol_mean 7.9621
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus X-Ray tube'
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                7376
_reflns_number_total             9873
_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, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-17); encifer 1.5.2 (CCDC, 2016)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_shelxl_version_number           2018/1
_computing_structure_solution    'SHELXD (Sheldrick, 2000-2008)'
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 
;
 Flack x determined using 2389 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.3(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         9873
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1034
_refine_ls_R_factor_gt           0.0742
_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)+(0.0362P)²+0.1453P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1330
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.921(2)
 0.079(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C12(H12), C13(H13),
 C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24),
  C34(H34), C35(H35), C36(H36), C37(H37), C39(H39), C40(H40), C42(H42),
 C43(H43), C45(H45), C46(H46), C47(H47), C48(H48), C50(H50), C51(H51), C53(H53),
  C54(H54), C64(H64), C65(H65), C66(H66), C67(H67), C69(H69), C70(H70),
 C72(H72), C73(H73), C75(H75), C76(H76), C77(H77), C78(H78), C80(H80), C81(H81),
  C83(H83), C84(H84)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
F1 F 0.13586(18) -0.07921(18) -1.1647(8) 0.0463(13) Uani 1 1 d . . . . .
F2 F -0.07745(19) -0.02822(19) -1.3260(9) 0.0485(13) Uani 1 1 d . . . . .
N1 N -0.0686(3) -0.3166(3) -1.0128(11) 0.0356(17) Uani 1 1 d . . . . .
N2 N -0.1955(2) -0.2638(3) -0.7680(10) 0.0298(16) Uani 1 1 d . . . . .
C1 C -0.0753(3) -0.2366(3) -0.9772(11) 0.0184(16) Uani 1 1 d . . . . .
C2 C -0.1157(3) -0.2270(3) -1.0054(11) 0.0181(16) Uani 1 1 d . . . . .
C3 C -0.0835(3) -0.2880(3) -0.8782(12) 0.0207(17) Uani 1 1 d . . . . .
C4 C -0.1051(3) -0.3047(3) -0.6554(12) 0.0253(18) Uani 1 1 d . . . . .
H4 H -0.114114 -0.283239 -0.561915 0.030 Uiso 1 1 calc R . . . .
C5 C -0.1130(3) -0.3527(3) -0.5722(15) 0.039(2) Uani 1 1 d . . . . .
H5 H -0.127842 -0.364725 -0.420390 0.047 Uiso 1 1 calc R . . . .
C6 C -0.0996(4) -0.3834(4) -0.7089(18) 0.048(3) Uani 1 1 d . . . . .
H6 H -0.105437 -0.416910 -0.655068 0.058 Uiso 1 1 calc R . . . .
C7 C -0.0773(4) -0.3639(3) -0.9271(17) 0.046(3) Uani 1 1 d . . . . .
H7 H -0.067590 -0.384778 -1.021448 0.055 Uiso 1 1 calc R . . . .
C8 C -0.0189(3) -0.1966(3) -1.0392(12) 0.0201(17) Uani 1 1 d . . . . .
C9 C 0.0209(3) -0.1848(3) -0.8721(12) 0.0197(16) Uani 1 1 d . . . . .
H9 H 0.011844 -0.203995 -0.728350 0.024 Uiso 1 1 calc R . . . .
C10 C 0.0731(3) -0.1457(3) -0.9128(12) 0.0258(18) Uani 1 1 d . . . . .
H10 H 0.099813 -0.137318 -0.797344 0.031 Uiso 1 1 calc R . . . .
C11 C 0.0854(3) -0.1192(3) -1.1229(13) 0.0223(18) Uani 1 1 d . . . . .
C12 C 0.0477(3) -0.1298(3) -1.2952(13) 0.0244(18) Uani 1 1 d . . . . .
H12 H 0.057406 -0.110761 -1.439324 0.029 Uiso 1 1 calc R . . . .
C13 C -0.0047(3) -0.1693(3) -1.2519(12) 0.0219(17) Uani 1 1 d . . . . .
H13 H -0.031159 -0.177654 -1.368889 0.026 Uiso 1 1 calc R . . . .
C14 C -0.1722(3) -0.2692(3) -0.9593(12) 0.0201(17) Uani 1 1 d . . . . .
C15 C -0.1981(3) -0.3103(3) -1.1155(13) 0.0300(19) Uani 1 1 d . . . . .
H15 H -0.180161 -0.312991 -1.249804 0.036 Uiso 1 1 calc R . . . .
C16 C -0.2519(3) -0.3486(3) -1.0734(14) 0.032(2) Uani 1 1 d . . . . .
H16 H -0.271089 -0.376991 -1.180765 0.039 Uiso 1 1 calc R . . . .
C17 C -0.2759(3) -0.3440(3) -0.8756(13) 0.0306(19) Uani 1 1 d . . . . .
H17 H -0.311907 -0.369607 -0.840333 0.037 Uiso 1 1 calc R . . . .
C18 C -0.2466(3) -0.3012(3) -0.7277(13) 0.0285(19) Uani 1 1 d . . . . .
H18 H -0.263369 -0.298079 -0.590243 0.034 Uiso 1 1 calc R . . . .
C19 C -0.1079(3) -0.1746(3) -1.0837(13) 0.0213(17) Uani 1 1 d . . . . .
C20 C -0.0753(3) -0.1279(3) -0.9573(13) 0.0240(17) Uani 1 1 d . . . . .
H20 H -0.059590 -0.130212 -0.814524 0.029 Uiso 1 1 calc R . . . .
C21 C -0.0655(3) -0.0790(3) -1.0346(14) 0.0295(19) Uani 1 1 d . . . . .
H21 H -0.044011 -0.047734 -0.945337 0.035 Uiso 1 1 calc R . . . .
C22 C -0.0874(3) -0.0763(3) -1.2428(14) 0.031(2) Uani 1 1 d . . . . .
C23 C -0.1201(3) -0.1205(3) -1.3749(13) 0.033(2) Uani 1 1 d . . . . .
H23 H -0.135244 -0.117369 -1.517972 0.040 Uiso 1 1 calc R . . . .
C24 C -0.1305(3) -0.1703(3) -1.2917(12) 0.0246(18) Uani 1 1 d . . . . .
H24 H -0.153333 -0.201501 -1.378694 0.030 Uiso 1 1 calc R . . . .
F31 F -0.57264(17) -0.45920(17) 0.1204(7) 0.0414(12) Uani 1 1 d . . . . .
F32 F -0.64010(18) -0.2527(2) 0.3235(8) 0.0492(14) Uani 1 1 d . . . . .
N31 N -0.3483(2) -0.2439(2) -0.0409(10) 0.0268(15) Uani 1 1 d . . . . .
N32 N -0.4084(2) -0.1229(2) -0.2740(10) 0.0273(15) Uani 1 1 d . . . . .
C31 C -0.4313(3) -0.2435(3) -0.0775(11) 0.0184(16) Uani 1 1 d . . . . .
C32 C -0.4416(3) -0.2035(3) -0.0452(11) 0.0181(16) Uani 1 1 d . . . . .
C33 C -0.3795(3) -0.2330(3) -0.1801(13) 0.0213(17) Uani 1 1 d . . . . .
C34 C -0.3650(3) -0.2153(3) -0.4078(12) 0.0245(18) Uani 1 1 d . . . . .
H34 H -0.387898 -0.208864 -0.504215 0.029 Uiso 1 1 calc R . . . .
C35 C -0.3173(3) -0.2072(3) -0.4944(13) 0.031(2) Uani 1 1 d . . . . .
H35 H -0.307418 -0.195842 -0.652078 0.037 Uiso 1 1 calc R . . . .
C36 C -0.2841(3) -0.2154(3) -0.3540(14) 0.031(2) Uani 1 1 d . . . . .
H36 H -0.250358 -0.208660 -0.409212 0.038 Uiso 1 1 calc R . . . .
C37 C -0.3011(3) -0.2341(3) -0.1271(14) 0.0299(19) Uani 1 1 d . . . . .
H37 H -0.278156 -0.240138 -0.028606 0.036 Uiso 1 1 calc R . . . .
C38 C -0.4691(3) -0.3007(3) -0.0215(12) 0.0174(16) Uani 1 1 d . . . . .
C39 C -0.4776(3) -0.3394(3) -0.1822(12) 0.0202(17) Uani 1 1 d . . . . .
H39 H -0.458845 -0.329367 -0.327061 0.024 Uiso 1 1 calc R . . . .
C40 C -0.5128(3) -0.3927(3) -0.1386(12) 0.0225(17) Uani 1 1 d . . . . .
H40 H -0.518910 -0.419049 -0.253042 0.027 Uiso 1 1 calc R . . . .
C41 C -0.5384(3) -0.4066(3) 0.0713(12) 0.0230(18) Uani 1 1 d . . . . .
C42 C -0.5308(3) -0.3696(3) 0.2421(12) 0.0246(18) Uani 1 1 d . . . . .
H42 H -0.548992 -0.380400 0.388229 0.029 Uiso 1 1 calc R . . . .
C43 C -0.4960(3) -0.3161(3) 0.1945(12) 0.0218(17) Uani 1 1 d . . . . .
H43 H -0.490291 -0.289896 0.308617 0.026 Uiso 1 1 calc R . . . .
C44 C -0.3997(3) -0.1469(3) -0.0888(12) 0.0190(16) Uani 1 1 d . . . . .
C45 C -0.3564(3) -0.1203(3) 0.0546(13) 0.0265(18) Uani 1 1 d . . . . .
H45 H -0.352130 -0.137864 0.186591 0.032 Uiso 1 1 calc R . . . .
C46 C -0.3183(3) -0.0672(3) 0.0077(14) 0.034(2) Uani 1 1 d . . . . .
H46 H -0.287742 -0.048420 0.104439 0.040 Uiso 1 1 calc R . . . .
C47 C -0.3265(3) -0.0431(3) -0.1821(12) 0.0250(18) Uani 1 1 d . . . . .
H47 H -0.301747 -0.006976 -0.218992 0.030 Uiso 1 1 calc R . . . .
C48 C -0.3710(3) -0.0719(3) -0.3179(14) 0.033(2) Uani 1 1 d . . . . .
H48 H -0.375741 -0.054968 -0.451049 0.039 Uiso 1 1 calc R . . . .
C49 C -0.4941(3) -0.2133(3) 0.0427(12) 0.0222(17) Uani 1 1 d . . . . .
C50 C -0.5414(3) -0.2485(3) -0.0731(12) 0.0229(17) Uani 1 1 d . . . . .
H50 H -0.539552 -0.263582 -0.218569 0.028 Uiso 1 1 calc R . . . .
C51 C -0.5903(3) -0.2618(3) 0.0180(13) 0.0292(19) Uani 1 1 d . . . . .
H51 H -0.622252 -0.285706 -0.061962 0.035 Uiso 1 1 calc R . . . .
C52 C -0.5915(3) -0.2392(3) 0.2302(15) 0.034(2) Uani 1 1 d . . . . .
C53 C -0.5464(3) -0.2032(3) 0.3494(13) 0.033(2) Uani 1 1 d . . . . .
H53 H -0.548657 -0.187505 0.492366 0.040 Uiso 1 1 calc R . . . .
C54 C -0.4976(3) -0.1907(3) 0.2522(13) 0.0258(18) Uani 1 1 d . . . . .
H54 H -0.465757 -0.166077 0.331071 0.031 Uiso 1 1 calc R . . . .
F61 F -0.18982(16) -0.45353(17) -0.1997(7) 0.0355(11) Uani 1 1 d . . . . .
F62 F -0.4142(2) -0.71187(18) -0.0194(8) 0.0518(14) Uani 1 1 d . . . . .
N61 N -0.3792(2) -0.4074(2) -0.3574(10) 0.0249(15) Uani 1 1 d . . . . .
N62 N -0.5221(3) -0.5842(3) -0.6022(11) 0.0311(16) Uani 1 1 d . . . . .
C61 C -0.3984(3) -0.4984(3) -0.3950(11) 0.0176(16) Uani 1 1 d . . . . .
C62 C -0.4421(3) -0.5469(3) -0.3665(11) 0.0208(17) Uani 1 1 d . . . . .
C63 C -0.4016(3) -0.4522(3) -0.4937(12) 0.0191(16) Uani 1 1 d . . . . .
C64 C -0.4234(3) -0.4545(3) -0.7119(12) 0.0254(18) Uani 1 1 d . . . . .
H64 H -0.438893 -0.486473 -0.801492 0.030 Uiso 1 1 calc R . . . .
C65 C -0.4220(3) -0.4096(4) -0.7959(13) 0.033(2) Uani 1 1 d . . . . .
H65 H -0.436141 -0.410045 -0.946909 0.040 Uiso 1 1 calc R . . . .
C66 C -0.4001(3) -0.3635(3) -0.6629(15) 0.036(2) Uani 1 1 d . . . . .
H66 H -0.398925 -0.332071 -0.719661 0.043 Uiso 1 1 calc R . . . .
C67 C -0.3801(3) -0.3649(3) -0.4446(15) 0.035(2) Uani 1 1 d . . . . .
H67 H -0.366159 -0.333684 -0.350182 0.043 Uiso 1 1 calc R . . . .
C68 C -0.3429(3) -0.4866(3) -0.3379(11) 0.0192(16) Uani 1 1 d . . . . .
C69 C -0.3021(3) -0.4602(3) -0.5006(12) 0.0190(16) Uani 1 1 d . . . . .
H69 H -0.309963 -0.449210 -0.645316 0.023 Uiso 1 1 calc R . . . .
C70 C -0.2510(3) -0.4494(3) -0.4591(12) 0.0229(17) Uani 1 1 d . . . . .
H70 H -0.223757 -0.432277 -0.573725 0.027 Uiso 1 1 calc R . . . .
C71 C -0.2408(3) -0.4643(3) -0.2448(13) 0.0255(18) Uani 1 1 d . . . . .
C72 C -0.2788(3) -0.4892(3) -0.0752(12) 0.0226(17) Uani 1 1 d . . . . .
H72 H -0.270185 -0.498837 0.070832 0.027 Uiso 1 1 calc R . . . .
C73 C -0.3301(3) -0.4999(3) -0.1214(12) 0.0244(18) Uani 1 1 d . . . . .
H73 H -0.356937 -0.516521 -0.004603 0.029 Uiso 1 1 calc R . . . .
C74 C -0.4968(3) -0.5550(3) -0.4111(12) 0.0195(17) Uani 1 1 d . . . . .
C75 C -0.5187(3) -0.5326(3) -0.2669(13) 0.0281(19) Uani 1 1 d . . . . .
H75 H -0.499927 -0.512618 -0.132359 0.034 Uiso 1 1 calc R . . . .
C76 C -0.5683(3) -0.5396(3) -0.3211(14) 0.034(2) Uani 1 1 d . . . . .
H76 H -0.584124 -0.524907 -0.222456 0.041 Uiso 1 1 calc R . . . .
C77 C -0.5945(3) -0.5678(3) -0.5177(14) 0.032(2) Uani 1 1 d . . . . .
H77 H -0.628013 -0.571944 -0.561415 0.039 Uiso 1 1 calc R . . . .
C78 C -0.5705(3) -0.5899(3) -0.6503(14) 0.037(2) Uani 1 1 d . . . . .
H78 H -0.589152 -0.610472 -0.783741 0.044 Uiso 1 1 calc R . . . .
C79 C -0.4377(3) -0.5936(3) -0.2847(12) 0.0200(17) Uani 1 1 d . . . . .
C80 C -0.4076(3) -0.6102(3) -0.4059(12) 0.0238(18) Uani 1 1 d . . . . .
H80 H -0.392049 -0.593784 -0.551590 0.029 Uiso 1 1 calc R . . . .
C81 C -0.3995(3) -0.6505(3) -0.3195(13) 0.0262(18) Uani 1 1 d . . . . .
H81 H -0.378802 -0.662134 -0.403647 0.031 Uiso 1 1 calc R . . . .
C82 C -0.4224(3) -0.6728(3) -0.1095(14) 0.031(2) Uani 1 1 d . . . . .
C83 C -0.4542(3) -0.6586(3) 0.0152(13) 0.0297(19) Uani 1 1 d . . . . .
H83 H -0.470065 -0.675662 0.159390 0.036 Uiso 1 1 calc R . . . .
C84 C -0.4623(3) -0.6192(3) -0.0743(12) 0.0250(18) Uani 1 1 d . . . . .
H84 H -0.484681 -0.609202 0.006768 0.030 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
F1 C11 1.356(8) . ?
F2 C22 1.358(8) . ?
N1 C3 1.348(9) . ?
N1 C7 1.355(10) . ?
N2 C14 1.330(8) . ?
N2 C18 1.347(9) . ?
C1 C2 1.340(9) . ?
C1 C3 1.495(10) . ?
C1 C8 1.498(9) . ?
C2 C14 1.498(9) . ?
C2 C19 1.487(10) . ?
C3 C4 1.389(9) . ?
C4 H4 0.9500 . ?
C4 C5 1.375(10) . ?
C5 H5 0.9500 . ?
C5 C6 1.375(12) . ?
C6 H6 0.9500 . ?
C6 C7 1.384(12) . ?
C7 H7 0.9500 . ?
C8 C9 1.398(9) . ?
C8 C13 1.391(9) . ?
C9 H9 0.9500 . ?
C9 C10 1.383(9) . ?
C10 H10 0.9500 . ?
C10 C11 1.369(10) . ?
C11 C12 1.383(10) . ?
C12 H12 0.9500 . ?
C12 C13 1.393(9) . ?
C13 H13 0.9500 . ?
C14 C15 1.370(10) . ?
C15 H15 0.9500 . ?
C15 C16 1.409(10) . ?
C16 H16 0.9500 . ?
C16 C17 1.364(10) . ?
C17 H17 0.9500 . ?
C17 C18 1.384(10) . ?
C18 H18 0.9500 . ?
C19 C20 1.400(10) . ?
C19 C24 1.390(9) . ?
C20 H20 0.9500 . ?
C20 C21 1.371(10) . ?
C21 H21 0.9500 . ?
C21 C22 1.365(10) . ?
C22 C23 1.375(11) . ?
C23 H23 0.9500 . ?
C23 C24 1.400(10) . ?
C24 H24 0.9500 . ?
F31 C41 1.369(8) . ?
F32 C52 1.367(8) . ?
N31 C33 1.352(9) . ?
N31 C37 1.343(9) . ?
N32 C44 1.354(8) . ?
N32 C48 1.348(9) . ?
C31 C32 1.346(9) . ?
C31 C33 1.493(9) . ?
C31 C38 1.492(10) . ?
C32 C44 1.494(9) . ?
C32 C49 1.488(9) . ?
C33 C34 1.380(9) . ?
C34 H34 0.9500 . ?
C34 C35 1.371(10) . ?
C35 H35 0.9500 . ?
C35 C36 1.358(11) . ?
C36 H36 0.9500 . ?
C36 C37 1.392(10) . ?
C37 H37 0.9500 . ?
C38 C39 1.372(9) . ?
C38 C43 1.404(9) . ?
C39 H39 0.9500 . ?
C39 C40 1.382(10) . ?
C40 H40 0.9500 . ?
C40 C41 1.357(9) . ?
C41 C42 1.382(10) . ?
C42 H42 0.9500 . ?
C42 C43 1.387(9) . ?
C43 H43 0.9500 . ?
C44 C45 1.367(9) . ?
C45 H45 0.9500 . ?
C45 C46 1.398(10) . ?
C46 H46 0.9500 . ?
C46 C47 1.370(10) . ?
C47 H47 0.9500 . ?
C47 C48 1.371(10) . ?
C48 H48 0.9500 . ?
C49 C50 1.398(9) . ?
C49 C54 1.389(9) . ?
C50 H50 0.9500 . ?
C50 C51 1.371(10) . ?
C51 H51 0.9500 . ?
C51 C52 1.383(11) . ?
C52 C53 1.375(11) . ?
C53 H53 0.9500 . ?
C53 C54 1.388(10) . ?
C54 H54 0.9500 . ?
F61 C71 1.372(8) . ?
F62 C82 1.367(8) . ?
N61 C63 1.366(9) . ?
N61 C67 1.341(9) . ?
N62 C74 1.348(9) . ?
N62 C78 1.355(9) . ?
C61 C62 1.350(9) . ?
C61 C63 1.497(9) . ?
C61 C68 1.501(9) . ?
C62 C74 1.502(10) . ?
C62 C79 1.494(9) . ?
C63 C64 1.380(9) . ?
C64 H64 0.9500 . ?
C64 C65 1.368(10) . ?
C65 H65 0.9500 . ?
C65 C66 1.382(11) . ?
C66 H66 0.9500 . ?
C66 C67 1.380(11) . ?
C67 H67 0.9500 . ?
C68 C69 1.392(9) . ?
C68 C73 1.396(9) . ?
C69 H69 0.9500 . ?
C69 C70 1.373(9) . ?
C70 H70 0.9500 . ?
C70 C71 1.375(9) . ?
C71 C72 1.368(10) . ?
C72 H72 0.9500 . ?
C72 C73 1.382(10) . ?
C73 H73 0.9500 . ?
C74 C75 1.384(10) . ?
C75 H75 0.9500 . ?
C75 C76 1.380(11) . ?
C76 H76 0.9500 . ?
C76 C77 1.370(11) . ?
C77 H77 0.9500 . ?
C77 C78 1.382(10) . ?
C78 H78 0.9500 . ?
C79 C80 1.373(10) . ?
C79 C84 1.402(9) . ?
C80 H80 0.9500 . ?
C80 C81 1.393(9) . ?
C81 H81 0.9500 . ?
C81 C82 1.362(10) . ?
C82 C83 1.379(11) . ?
C83 H83 0.9500 . ?
C83 C84 1.375(10) . ?
C84 H84 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
C3 N1 C7 117.5(7) . . ?
C14 N2 C18 117.5(6) . . ?
C2 C1 C3 122.0(6) . . ?
C2 C1 C8 122.5(6) . . ?
C3 C1 C8 115.4(6) . . ?
C1 C2 C14 121.4(6) . . ?
C1 C2 C19 123.0(6) . . ?
C19 C2 C14 115.6(6) . . ?
N1 C3 C1 117.1(6) . . ?
N1 C3 C4 122.1(7) . . ?
C4 C3 C1 120.7(7) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 C3 119.1(8) . . ?
C5 C4 H4 120.5 . . ?
C4 C5 H5 120.1 . . ?
C6 C5 C4 119.9(8) . . ?
C6 C5 H5 120.1 . . ?
C5 C6 H6 120.9 . . ?
C5 C6 C7 118.1(9) . . ?
C7 C6 H6 120.9 . . ?
N1 C7 C6 123.2(8) . . ?
N1 C7 H7 118.4 . . ?
C6 C7 H7 118.4 . . ?
C9 C8 C1 118.3(6) . . ?
C13 C8 C1 122.9(6) . . ?
C13 C8 C9 118.8(7) . . ?
C8 C9 H9 119.5 . . ?
C10 C9 C8 121.1(7) . . ?
C10 C9 H9 119.5 . . ?
C9 C10 H10 120.7 . . ?
C11 C10 C9 118.5(7) . . ?
C11 C10 H10 120.7 . . ?
F1 C11 C10 120.0(6) . . ?
F1 C11 C12 117.3(7) . . ?
C10 C11 C12 122.6(7) . . ?
C11 C12 H12 120.9 . . ?
C11 C12 C13 118.2(7) . . ?
C13 C12 H12 120.9 . . ?
C8 C13 C12 120.7(7) . . ?
C8 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
N2 C14 C2 117.3(6) . . ?
N2 C14 C15 123.0(7) . . ?
C15 C14 C2 119.7(6) . . ?
C14 C15 H15 120.6 . . ?
C14 C15 C16 118.9(7) . . ?
C16 C15 H15 120.6 . . ?
C15 C16 H16 120.6 . . ?
C17 C16 C15 118.8(7) . . ?
C17 C16 H16 120.6 . . ?
C16 C17 H17 120.9 . . ?
C16 C17 C18 118.3(7) . . ?
C18 C17 H17 120.9 . . ?
N2 C18 C17 123.6(7) . . ?
N2 C18 H18 118.2 . . ?
C17 C18 H18 118.2 . . ?
C20 C19 C2 121.1(7) . . ?
C24 C19 C2 120.7(6) . . ?
C24 C19 C20 118.1(7) . . ?
C19 C20 H20 119.2 . . ?
C21 C20 C19 121.6(7) . . ?
C21 C20 H20 119.2 . . ?
C20 C21 H21 120.8 . . ?
C22 C21 C20 118.5(7) . . ?
C22 C21 H21 120.8 . . ?
F2 C22 C21 119.7(7) . . ?
F2 C22 C23 117.3(7) . . ?
C21 C22 C23 123.1(7) . . ?
C22 C23 H23 121.1 . . ?
C22 C23 C24 117.8(7) . . ?
C24 C23 H23 121.1 . . ?
C19 C24 C23 120.9(7) . . ?
C19 C24 H24 119.5 . . ?
C23 C24 H24 119.5 . . ?
C37 N31 C33 117.7(6) . . ?
C48 N32 C44 116.9(6) . . ?
C32 C31 C33 120.6(6) . . ?
C32 C31 C38 124.8(6) . . ?
C38 C31 C33 114.6(6) . . ?
C31 C32 C44 121.0(6) . . ?
C31 C32 C49 121.8(6) . . ?
C49 C32 C44 117.2(6) . . ?
N31 C33 C31 116.3(6) . . ?
N31 C33 C34 121.5(7) . . ?
C34 C33 C31 122.2(7) . . ?
C33 C34 H34 120.1 . . ?
C35 C34 C33 119.7(7) . . ?
C35 C34 H34 120.1 . . ?
C34 C35 H35 120.1 . . ?
C36 C35 C34 119.8(7) . . ?
C36 C35 H35 120.1 . . ?
C35 C36 H36 120.9 . . ?
C35 C36 C37 118.1(7) . . ?
C37 C36 H36 120.9 . . ?
N31 C37 C36 123.0(7) . . ?
N31 C37 H37 118.5 . . ?
C36 C37 H37 118.5 . . ?
C39 C38 C31 119.8(6) . . ?
C39 C38 C43 118.6(7) . . ?
C43 C38 C31 121.6(6) . . ?
C38 C39 H39 119.2 . . ?
C38 C39 C40 121.7(6) . . ?
C40 C39 H39 119.2 . . ?
C39 C40 H40 120.7 . . ?
C41 C40 C39 118.5(7) . . ?
C41 C40 H40 120.7 . . ?
F31 C41 C42 117.7(6) . . ?
C40 C41 F31 119.6(7) . . ?
C40 C41 C42 122.6(7) . . ?
C41 C42 H42 120.9 . . ?
C41 C42 C43 118.2(7) . . ?
C43 C42 H42 120.9 . . ?
C38 C43 H43 119.8 . . ?
C42 C43 C38 120.4(7) . . ?
C42 C43 H43 119.8 . . ?
N32 C44 C32 115.8(6) . . ?
N32 C44 C45 122.0(7) . . ?
C45 C44 C32 122.2(6) . . ?
C44 C45 H45 119.9 . . ?
C44 C45 C46 120.2(7) . . ?
C46 C45 H45 119.9 . . ?
C45 C46 H46 121.0 . . ?
C47 C46 C45 118.0(7) . . ?
C47 C46 H46 121.0 . . ?
C46 C47 H47 120.5 . . ?
C46 C47 C48 118.9(7) . . ?
C48 C47 H47 120.5 . . ?
N32 C48 C47 123.9(7) . . ?
N32 C48 H48 118.0 . . ?
C47 C48 H48 118.0 . . ?
C50 C49 C32 121.0(6) . . ?
C54 C49 C32 120.6(6) . . ?
C54 C49 C50 118.2(7) . . ?
C49 C50 H50 119.2 . . ?
C51 C50 C49 121.6(7) . . ?
C51 C50 H50 119.2 . . ?
C50 C51 H51 121.2 . . ?
C50 C51 C52 117.7(7) . . ?
C52 C51 H51 121.2 . . ?
F32 C52 C51 118.1(8) . . ?
F32 C52 C53 118.4(8) . . ?
C53 C52 C51 123.5(7) . . ?
C52 C53 H53 121.4 . . ?
C52 C53 C54 117.2(7) . . ?
C54 C53 H53 121.4 . . ?
C49 C54 H54 119.2 . . ?
C53 C54 C49 121.7(7) . . ?
C53 C54 H54 119.2 . . ?
C67 N61 C63 116.3(6) . . ?
C74 N62 C78 116.4(7) . . ?
C62 C61 C63 122.0(6) . . ?
C62 C61 C68 123.4(6) . . ?
C63 C61 C68 114.6(6) . . ?
C61 C62 C74 120.6(6) . . ?
C61 C62 C79 121.3(7) . . ?
C79 C62 C74 118.0(6) . . ?
N61 C63 C61 115.0(6) . . ?
N61 C63 C64 123.2(7) . . ?
C64 C63 C61 121.7(6) . . ?
C63 C64 H64 120.9 . . ?
C65 C64 C63 118.2(7) . . ?
C65 C64 H64 120.9 . . ?
C64 C65 H65 119.7 . . ?
C64 C65 C66 120.6(7) . . ?
C66 C65 H65 119.7 . . ?
C65 C66 H66 121.2 . . ?
C67 C66 C65 117.5(7) . . ?
C67 C66 H66 121.2 . . ?
N61 C67 C66 124.1(8) . . ?
N61 C67 H67 117.9 . . ?
C66 C67 H67 117.9 . . ?
C69 C68 C61 119.8(6) . . ?
C69 C68 C73 118.1(6) . . ?
C73 C68 C61 122.0(6) . . ?
C68 C69 H69 118.9 . . ?
C70 C69 C68 122.2(6) . . ?
C70 C69 H69 118.9 . . ?
C69 C70 H70 121.4 . . ?
C69 C70 C71 117.3(7) . . ?
C71 C70 H70 121.4 . . ?
F61 C71 C70 118.1(7) . . ?
C72 C71 F61 118.6(6) . . ?
C72 C71 C70 123.3(7) . . ?
C71 C72 H72 120.8 . . ?
C71 C72 C73 118.4(7) . . ?
C73 C72 H72 120.8 . . ?
C68 C73 H73 119.7 . . ?
C72 C73 C68 120.6(7) . . ?
C72 C73 H73 119.7 . . ?
N62 C74 C62 115.8(6) . . ?
N62 C74 C75 122.7(7) . . ?
C75 C74 C62 121.5(6) . . ?
C74 C75 H75 120.5 . . ?
C76 C75 C74 119.1(7) . . ?
C76 C75 H75 120.5 . . ?
C75 C76 H76 120.1 . . ?
C77 C76 C75 119.7(7) . . ?
C77 C76 H76 120.1 . . ?
C76 C77 H77 121.1 . . ?
C76 C77 C78 117.8(7) . . ?
C78 C77 H77 121.1 . . ?
N62 C78 C77 124.3(7) . . ?
N62 C78 H78 117.9 . . ?
C77 C78 H78 117.9 . . ?
C80 C79 C62 121.0(6) . . ?
C80 C79 C84 119.2(7) . . ?
C84 C79 C62 119.6(6) . . ?
C79 C80 H80 119.4 . . ?
C79 C80 C81 121.3(7) . . ?
C81 C80 H80 119.4 . . ?
C80 C81 H81 121.3 . . ?
C82 C81 C80 117.4(7) . . ?
C82 C81 H81 121.3 . . ?
F62 C82 C83 118.1(7) . . ?
C81 C82 F62 118.4(8) . . ?
C81 C82 C83 123.4(7) . . ?
C82 C83 H83 120.8 . . ?
C84 C83 C82 118.3(7) . . ?
C84 C83 H83 120.8 . . ?
C79 C84 H84 119.9 . . ?
C83 C84 C79 120.2(7) . . ?
C83 C84 H84 119.9 . . ?

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
F1 C11 C12 C13 -177.4(6) . . . . ?
F2 C22 C23 C24 179.7(6) . . . . ?
N1 C3 C4 C5 -2.2(10) . . . . ?
N2 C14 C15 C16 0.4(12) . . . . ?
C1 C2 C14 N2 107.9(8) . . . . ?
C1 C2 C14 C15 -73.9(9) . . . . ?
C1 C2 C19 C20 -58.1(10) . . . . ?
C1 C2 C19 C24 118.4(8) . . . . ?
C1 C3 C4 C5 178.7(6) . . . . ?
C1 C8 C9 C10 -175.7(7) . . . . ?
C1 C8 C13 C12 175.7(6) . . . . ?
C2 C1 C3 N1 121.9(7) . . . . ?
C2 C1 C3 C4 -59.0(9) . . . . ?
C2 C1 C8 C9 129.6(7) . . . . ?
C2 C1 C8 C13 -48.0(10) . . . . ?
C2 C14 C15 C16 -177.7(7) . . . . ?
C2 C19 C20 C21 176.4(6) . . . . ?
C2 C19 C24 C23 -175.3(6) . . . . ?
C3 N1 C7 C6 -1.2(12) . . . . ?
C3 C1 C2 C14 -5.6(10) . . . . ?
C3 C1 C2 C19 174.5(6) . . . . ?
C3 C1 C8 C9 -49.5(9) . . . . ?
C3 C1 C8 C13 132.8(7) . . . . ?
C3 C4 C5 C6 0.2(11) . . . . ?
C4 C5 C6 C7 1.1(12) . . . . ?
C5 C6 C7 N1 -0.6(13) . . . . ?
C7 N1 C3 C1 -178.2(6) . . . . ?
C7 N1 C3 C4 2.7(11) . . . . ?
C8 C1 C2 C14 175.3(6) . . . . ?
C8 C1 C2 C19 -4.6(10) . . . . ?
C8 C1 C3 N1 -58.9(8) . . . . ?
C8 C1 C3 C4 120.2(7) . . . . ?
C8 C9 C10 C11 -1.3(11) . . . . ?
C9 C8 C13 C12 -1.9(10) . . . . ?
C9 C10 C11 F1 177.5(6) . . . . ?
C9 C10 C11 C12 0.4(11) . . . . ?
C10 C11 C12 C13 -0.2(11) . . . . ?
C11 C12 C13 C8 1.0(10) . . . . ?
C13 C8 C9 C10 2.1(10) . . . . ?
C14 N2 C18 C17 -1.0(11) . . . . ?
C14 C2 C19 C20 122.0(7) . . . . ?
C14 C2 C19 C24 -61.6(9) . . . . ?
C14 C15 C16 C17 -1.5(11) . . . . ?
C15 C16 C17 C18 1.4(11) . . . . ?
C16 C17 C18 N2 -0.1(12) . . . . ?
C18 N2 C14 C2 179.0(6) . . . . ?
C18 N2 C14 C15 0.9(11) . . . . ?
C19 C2 C14 N2 -72.2(8) . . . . ?
C19 C2 C14 C15 106.0(8) . . . . ?
C19 C20 C21 C22 -1.5(11) . . . . ?
C20 C19 C24 C23 1.3(10) . . . . ?
C20 C21 C22 F2 -178.6(6) . . . . ?
C20 C21 C22 C23 2.1(12) . . . . ?
C21 C22 C23 C24 -1.0(11) . . . . ?
C22 C23 C24 C19 -0.7(11) . . . . ?
C24 C19 C20 C21 -0.1(10) . . . . ?
F31 C41 C42 C43 179.7(6) . . . . ?
F32 C52 C53 C54 179.3(6) . . . . ?
N31 C33 C34 C35 -1.8(11) . . . . ?
N32 C44 C45 C46 -2.4(11) . . . . ?
C31 C32 C44 N32 112.1(7) . . . . ?
C31 C32 C44 C45 -70.5(9) . . . . ?
C31 C32 C49 C50 -56.0(10) . . . . ?
C31 C32 C49 C54 119.0(8) . . . . ?
C31 C33 C34 C35 -178.8(7) . . . . ?
C31 C38 C39 C40 -179.2(6) . . . . ?
C31 C38 C43 C42 -179.8(6) . . . . ?
C32 C31 C33 N31 117.6(7) . . . . ?
C32 C31 C33 C34 -65.3(9) . . . . ?
C32 C31 C38 C39 133.0(7) . . . . ?
C32 C31 C38 C43 -47.9(10) . . . . ?
C32 C44 C45 C46 -179.6(7) . . . . ?
C32 C49 C50 C51 173.6(7) . . . . ?
C32 C49 C54 C53 -173.8(7) . . . . ?
C33 N31 C37 C36 -2.7(11) . . . . ?
C33 C31 C32 C44 -6.1(10) . . . . ?
C33 C31 C32 C49 176.1(6) . . . . ?
C33 C31 C38 C39 -45.9(9) . . . . ?
C33 C31 C38 C43 133.3(7) . . . . ?
C33 C34 C35 C36 -1.4(11) . . . . ?
C34 C35 C36 C37 2.5(11) . . . . ?
C35 C36 C37 N31 -0.4(12) . . . . ?
C37 N31 C33 C31 -179.1(6) . . . . ?
C37 N31 C33 C34 3.8(10) . . . . ?
C38 C31 C32 C44 175.2(6) . . . . ?
C38 C31 C32 C49 -2.6(10) . . . . ?
C38 C31 C33 N31 -63.5(8) . . . . ?
C38 C31 C33 C34 113.6(7) . . . . ?
C38 C39 C40 C41 -1.5(11) . . . . ?
C39 C38 C43 C42 -0.7(10) . . . . ?
C39 C40 C41 F31 -178.7(6) . . . . ?
C39 C40 C41 C42 0.3(11) . . . . ?
C40 C41 C42 C43 0.6(11) . . . . ?
C41 C42 C43 C38 -0.4(10) . . . . ?
C43 C38 C39 C40 1.7(10) . . . . ?
C44 N32 C48 C47 -2.5(11) . . . . ?
C44 C32 C49 C50 126.0(7) . . . . ?
C44 C32 C49 C54 -58.9(9) . . . . ?
C44 C45 C46 C47 1.1(11) . . . . ?
C45 C46 C47 C48 -0.6(11) . . . . ?
C46 C47 C48 N32 1.4(12) . . . . ?
C48 N32 C44 C32 -179.6(6) . . . . ?
C48 N32 C44 C45 3.0(10) . . . . ?
C49 C32 C44 N32 -70.0(8) . . . . ?
C49 C32 C44 C45 107.4(8) . . . . ?
C49 C50 C51 C52 -0.2(11) . . . . ?
C50 C49 C54 C53 1.4(11) . . . . ?
C50 C51 C52 F32 -179.4(6) . . . . ?
C50 C51 C52 C53 2.1(12) . . . . ?
C51 C52 C53 C54 -2.2(12) . . . . ?
C52 C53 C54 C49 0.4(11) . . . . ?
C54 C49 C50 C51 -1.5(10) . . . . ?
F61 C71 C72 C73 180.0(6) . . . . ?
F62 C82 C83 C84 179.7(6) . . . . ?
N61 C63 C64 C65 0.5(10) . . . . ?
N62 C74 C75 C76 -0.8(11) . . . . ?
C61 C62 C74 N62 110.1(7) . . . . ?
C61 C62 C74 C75 -68.3(9) . . . . ?
C61 C62 C79 C80 -57.5(9) . . . . ?
C61 C62 C79 C84 119.0(8) . . . . ?
C61 C63 C64 C65 -176.1(6) . . . . ?
C61 C68 C69 C70 -178.7(6) . . . . ?
C61 C68 C73 C72 179.2(6) . . . . ?
C62 C61 C63 N61 125.7(7) . . . . ?
C62 C61 C63 C64 -57.4(9) . . . . ?
C62 C61 C68 C69 131.0(7) . . . . ?
C62 C61 C68 C73 -51.1(10) . . . . ?
C62 C74 C75 C76 177.5(7) . . . . ?
C62 C79 C80 C81 174.2(6) . . . . ?
C62 C79 C84 C83 -173.4(7) . . . . ?
C63 N61 C67 C66 -2.6(11) . . . . ?
C63 C61 C62 C74 -6.1(10) . . . . ?
C63 C61 C62 C79 175.4(6) . . . . ?
C63 C61 C68 C69 -47.3(9) . . . . ?
C63 C61 C68 C73 130.6(7) . . . . ?
C63 C64 C65 C66 -1.1(11) . . . . ?
C64 C65 C66 C67 -0.1(11) . . . . ?
C65 C66 C67 N61 2.1(12) . . . . ?
C67 N61 C63 C61 178.1(6) . . . . ?
C67 N61 C63 C64 1.3(10) . . . . ?
C68 C61 C62 C74 175.7(6) . . . . ?
C68 C61 C62 C79 -2.9(10) . . . . ?
C68 C61 C63 N61 -55.9(8) . . . . ?
C68 C61 C63 C64 121.0(7) . . . . ?
C68 C69 C70 C71 -2.0(11) . . . . ?
C69 C68 C73 C72 -2.9(10) . . . . ?
C69 C70 C71 F61 -179.6(6) . . . . ?
C69 C70 C71 C72 0.3(11) . . . . ?
C70 C71 C72 C73 0.1(11) . . . . ?
C71 C72 C73 C68 1.3(11) . . . . ?
C73 C68 C69 C70 3.3(10) . . . . ?
C74 N62 C78 C77 0.3(12) . . . . ?
C74 C62 C79 C80 123.9(7) . . . . ?
C74 C62 C79 C84 -59.6(9) . . . . ?
C74 C75 C76 C77 -1.0(11) . . . . ?
C75 C76 C77 C78 2.3(12) . . . . ?
C76 C77 C78 N62 -2.0(13) . . . . ?
C78 N62 C74 C62 -177.2(7) . . . . ?
C78 N62 C74 C75 1.2(10) . . . . ?
C79 C62 C74 N62 -71.3(8) . . . . ?
C79 C62 C74 C75 110.3(8) . . . . ?
C79 C80 C81 C82 -0.3(10) . . . . ?
C80 C79 C84 C83 3.2(11) . . . . ?
C80 C81 C82 F62 -178.9(6) . . . . ?
C80 C81 C82 C83 2.3(11) . . . . ?
C81 C82 C83 C84 -1.5(12) . . . . ?
C82 C83 C84 C79 -1.3(11) . . . . ?
C84 C79 C80 C81 -2.4(10) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.921(2)
2 0.079(2)

_cell_oxdiff_length_a            28.9472(11)
_cell_oxdiff_length_b            28.9603(13)
_cell_oxdiff_length_c            5.6949(2)
_cell_oxdiff_angle_alpha         90.001(4)
_cell_oxdiff_angle_beta          90.001(3)
_cell_oxdiff_angle_gamma         119.958(4)
_cell_oxdiff_volume              4136.3(3)
_cell_oxdiff_measurement_reflns_used 3963
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_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
36 -4 -2 0.0279 36.0114 -4.0126 -1.9988 0.0759 -0.9845 -0.1473
17 -41 0 0.0177 16.9969 -40.9863 0.0019 -1.0053 -0.0820 0.0001
-17 41 0 0.0177 -16.9969 40.9863 -0.0019 1.0053 0.0820 -0.0001
-36 4 2 0.0279 -36.0114 4.0126 1.9988 -0.0759 0.9845 0.1473
-9 1 -8 0.1615 -8.9851 0.9897 -7.9984 -0.0102 0.1363 -1.0159
7 -1 8 0.1271 6.9846 -0.9891 7.9984 0.0002 -0.0810 1.0100
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_orient_matrix_UB_11      0.0050120000
_diffrn_orient_matrix_UB_12      0.0266052000
_diffrn_orient_matrix_UB_13      -0.0010607000
_diffrn_orient_matrix_UB_21      -0.0276806000
_diffrn_orient_matrix_UB_22      -0.0094778000
_diffrn_orient_matrix_UB_23      0.0128754000
_diffrn_orient_matrix_UB_31      0.0029207000
_diffrn_orient_matrix_UB_32      0.0012136000
_diffrn_orient_matrix_UB_33      0.1238788000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -49.00    1.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5380   77.0000 -120.0000 100

#__ type_ start__ end____ width___ exp.time_
  2 omega  -78.00   10.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5380  -77.0000   30.0000 176

#__ type_ start__ end____ width___ exp.time_
  3 omega  -49.00  -23.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5380   77.0000   60.0000 52

#__ type_ start__ end____ width___ exp.time_
  4 omega  -50.00   11.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5380   79.0000  109.9258 122

#__ type_ start__ end____ width___ exp.time_
  5 omega    8.00   51.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5380   77.0000   60.0000 86

#__ type_ start__ end____ width___ exp.time_
  6 omega   24.00   49.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6161  -77.0000 -150.0000 50

#__ type_ start__ end____ width___ exp.time_
  7 omega  -23.00   49.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6161  -77.0000  -60.0000 144

#__ type_ start__ end____ width___ exp.time_
  8 omega   -3.00   84.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6161   57.0000  -30.0000 174

#__ type_ start__ end____ width___ exp.time_
  9 omega  -50.00   12.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6161  -77.0000 -180.0000 124

#__ type_ start__ end____ width___ exp.time_
 10 omega  -52.00   49.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6161  -77.0000   30.0000 202

#__ type_ start__ end____ width___ exp.time_
 11 omega   -1.00   80.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6161   57.0000 -180.0000 162

#__ type_ start__ end____ width___ exp.time_
 12 omega    2.00   59.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6161   77.0000 -120.0000 114

#__ type_ start__ end____ width___ exp.time_
 13 omega  -25.00   74.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6161   19.0000  150.0000 198

#__ type_ start__ end____ width___ exp.time_
 14 omega   24.00   49.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6161  -77.0000  -30.0000 50

#__ type_ start__ end____ width___ exp.time_
 15 omega   21.00   50.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6161  -79.0000  155.8710 58

#__ type_ start__ end____ width___ exp.time_
 16 omega  -50.00    4.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6161  -57.0000  -90.0000 108

#__ type_ start__ end____ width___ exp.time_
 17 omega  -25.00   92.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6161   19.0000  -30.0000 234

;
_reflns_odcompleteness_completeness 87.99
_reflns_odcompleteness_theta     26.32
_reflns_odcompleteness_iscentric 1
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_ambient_environment      'perfluoro polyether oil / N~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_ga_tro59
_database_code_depnum_ccdc_archive 'CCDC 1817688'
_audit_update_record             
;
2018-01-17 deposited with the CCDC.
2018-02-05 downloaded from the CCDC.
;
_audit_creation_date             2018-01-15

_audit_block_code                ga_tro59
_audit_block_refno               1961
_audit_block_usercomment         'tr1209, needle, colourless'


_audit_creation_method           
;
Olex2 1.2
(compiled Aug 10 2017 17:44:14 for OlexSys, GUI svn.r5381)
;

# start Validation Reply Form
_vrf_PLAT340_ga_tro59            
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01476 Ang.
RESPONSE: weak and noisy dataset.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C24 H18 F2 N2'
_chemical_formula_sum            'C24 H18 F2 N2'
_chemical_formula_weight         372.40
_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'
_chemical_absolute_configuration unk
loop_
_symmetry_equiv_pos_as_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'
_chemical_melting_point          ?
_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_diffrn_ambient_temperature      110(1)
_chemical_oxdiff_formula         'C24 H18 F2 N2'
_chemical_oxdiff_usercomment     'tr1209, needle, colourless'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

_cell_length_a                   14.1238(3)
_cell_length_b                   8.54517(18)
_cell_length_c                   15.8226(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1909.64(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    15217
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      66.9260
_cell_measurement_theta_min      5.5790
_shelx_estimated_absorpt_T_max   0.944
_shelx_estimated_absorpt_T_min   0.837
_exptl_absorpt_coefficient_mu    0.736
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.646
_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 (Busing & Levy, 1957).
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             776
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 5 1 0.0677
5 -5 -1 0.0010
9 1 -1 0.0680
-9 -1 1 0.0680
3 -1 10 0.1026
-3 1 -10 0.1026
4 -5 -1 0.0044
5 5 0 0.0739
_exptl_crystal_size_max          0.243
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.069
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
-5.0117 4.9966 1.0094 1.0569 0.0502 -0.0195
5.0117 -4.9966 -1.0094 -1.0569 -0.0502 0.0195
8.9981 1.0003 -1.0050 -0.3454 -0.0215 0.9413
-8.9981 -1.0003 1.0050 0.3454 0.0215 -0.9413
2.9980 -1.0038 9.9985 -0.2780 0.9972 0.1259
-2.9980 1.0038 -9.9985 0.2780 -0.9972 -0.1259
4.0117 -4.9966 -1.0087 -1.0017 -0.0587 -0.0743
4.9886 4.9975 0.0026 0.5010 0.0381 0.9245

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1686
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            56245
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.373
_diffrn_reflns_theta_max         67.373
_diffrn_reflns_theta_min         5.592
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -12.00  20.00   1.00    5.00    --    0.00 -38.00 -30.00   32
  2  ω    -43.00 -17.00   1.00    5.00    --    0.00  19.00-180.00   26
  3  ω    -40.00 -14.00   1.00    5.00    --    0.00 -38.00 -30.00   26
  4  ω    -69.00 -16.00   1.00    5.00    --    0.00 -38.00-120.00   53
  5  ω     12.00  70.00   1.00    5.00    --    0.00  19.00-180.00   58
  6  ω    -26.00  24.00   1.00    5.00    --    0.00  77.00-120.00   50
  7  ω     28.00  70.00   1.00    5.00    --    0.00  77.00-120.00   42
  8  ω     -9.00  42.00   1.00    5.00    --   14.00  80.00 -41.72   51
  9  ω     -6.00  19.00   1.00    5.00    --   26.00  80.00 125.49   25
 10  ω     -1.00  34.00   1.00   15.00    --   30.00  78.00-156.59   35
 11  ω      2.00  27.00   1.00   15.00    --   34.00  80.00 -62.41   25
 12  ω      6.00  31.00   1.00   15.00    --   38.00  80.00 166.44   25
 13  ω     11.00  37.00   1.00   15.00    --   42.00  80.00  -3.51   26
 14  ω     11.00  36.00   1.00   15.00    --   42.00  79.00 152.46   25
 15  ω     10.00  46.00   1.00   15.00    --   42.00  80.00  68.67   36
 16  ω     17.00  44.00   1.00   15.00    --   46.00  77.00 -72.62   27
 17  ω     90.00 116.00   1.00   15.00    --   46.00  75.00 -19.91   26
 18  ω     19.00  45.00   1.00   15.00    --   46.00  75.00 -19.91   26
 19  ω     19.00  44.00   1.00   15.00    --   50.00  78.00 154.71   25
 20  ω     19.00  44.00   1.00   15.00    --   50.00  79.00  55.32   25
 21  ω     19.00  44.00   1.00   15.00    --   50.00  79.00 113.58   25
 22  ω     24.00  50.00   1.00   15.00    --   54.00  77.00-180.00   26
 23  ω     26.00  53.00   1.00   15.00    --   54.00  77.00-150.00   27
 24  ω     24.00  50.00   1.00   15.00    --   54.00  77.00-123.76   26
 25  ω     24.00  51.00   1.00   15.00    --   54.00  77.00  90.00   27
 26  ω     23.00  48.00   1.00   15.00    --   54.00  78.00-162.46   25
 27  ω     31.00  57.00   1.00   15.00    --   54.00  77.00 -30.00   26
 28  ω     18.00  83.00   1.00   15.00    --   54.00 -77.00 -60.00   65
 29  ω     24.00  53.00   1.00   15.00    --   54.00  77.00  30.00   29
 30  ω     24.00  52.00   1.00   15.00    --   54.00  77.00   0.00   28
 31  ω     55.00  82.00   1.00   15.00    --   54.00  77.00-123.76   27
 32  ω    -16.00  82.00   1.00   15.00    --   54.00 -78.00 -90.26   98
 33  ω     29.00  56.00   1.00   15.00    --   54.00  77.00  60.00   27
 34  ω    -17.00  84.00   1.00   15.00    --   54.00 -79.00  53.20  101
 35  ω     23.00  48.00   1.00   15.00    --   54.00  78.00 -75.57   25
 36  ω     73.00 123.00   1.00   15.00    --   54.00  77.00  90.00   50
 37  ω     35.00  62.00   1.00   15.00    --   58.00  71.00 156.00   27
 38  ω     37.00  64.00   1.00   15.00    --   58.00  77.00 -74.03   27
 39  ω     40.00  67.00   1.00   15.00    --   58.00  59.00 124.85   27
 40  ω     31.00  57.00   1.00   15.00    --   58.00  75.00   8.55   26
 41  ω     78.00 104.00   1.00   15.00    --   58.00  74.00 133.05   26
 42  ω     34.00  61.00   1.00   15.00    --   58.00  70.00  37.82   27
 43  ω     31.00  56.00   1.00   15.00    --   58.00  74.00 133.05   25
 44  ω     35.00  61.00   1.00   15.00    --   62.00  76.00-110.63   26
 45  ω     40.00  67.00   1.00   15.00    --   62.00  71.00  43.26   27
 46  ω     33.00  58.00   1.00   15.00    --   62.00  77.00 -90.53   25
 47  ω     39.00  65.00   1.00   15.00    --   66.00  73.00-140.41   26
 48  ω     43.00 120.00   1.00   15.00    --   66.00  69.00 -41.74   77
 49  ω     43.00  69.00   1.00   15.00    --   66.00  64.00 134.09   26
 50  ω     38.00  65.00   1.00   15.00    --   66.00  75.00  48.33   27
 51  ω     40.00  67.00   1.00   15.00    --   66.00  77.00 143.92   27
 52  ω     42.00 103.00   1.00   15.00    --   70.00  73.00-162.67   61
 53  ω     44.00  85.00   1.00   15.00    --   70.00  70.00 172.27   41
 54  ω     52.00  78.00   1.00   15.00    --   70.00  59.00 -94.61   26
 55  ω     41.00  66.00   1.00   15.00    --   70.00  75.00  14.79   25
 56  ω     45.00  91.00   1.00   15.00    --   70.00  75.00 -80.55   46
 57  ω     53.00  80.00   1.00   15.00    --   74.00 -80.00  96.46   27
 58  ω     52.00  83.00   1.00   15.00    --   74.00  66.00  24.43   31
 59  ω     49.00 108.00   1.00   15.00    --   74.00  72.00  34.24   59
 60  ω     49.00  75.00   1.00   15.00    --   74.00  70.00 135.48   26
 61  ω     57.00  86.00   1.00   15.00    --   74.00  66.00  78.67   29
 62  ω     45.00  80.00   1.00   15.00    --   74.00  76.00  59.16   35
 63  ω     47.00  90.00   1.00   15.00    --   74.00  73.00-145.41   43
 64  ω      4.00 106.00   1.00   15.00    --   74.00 -80.00 150.50  102
 65  ω     53.00  80.00   1.00   15.00    --   78.00  76.00 -28.96   27
 66  ω     57.00  85.00   1.00   15.00    --   78.00  63.00  46.48   28
 67  ω     51.00  77.00   1.00   15.00    --   78.00  72.00 -93.87   26
 68  ω     54.00  80.00   1.00   15.00    --   78.00  72.00 141.28   26
 69  ω     53.00  81.00   1.00   15.00    --   78.00  69.00 -32.50   28
 70  ω     52.00 145.00   1.00   15.00    --   78.00  72.00  -9.95   93
 71  ω     57.00  83.00   1.00   15.00    --   78.00  65.00 103.45   26
 72  ω     60.00 109.00   1.00   30.00    --   82.00  63.00 150.96   49
 73  ω     63.00  88.00   1.00   30.00    --   82.00  47.00 135.07   25
 74  ω     57.00 145.00   1.00   30.00    --   82.00  70.00 -94.14   88
 75  ω     57.00  83.00   1.00   30.00    --   82.00  70.00  59.71   26
 76  ω     55.00 107.00   1.00   30.00    --   82.00  71.00-174.97   52
 77  ω     57.00  84.00   1.00   30.00    --   82.00  70.00 -27.20   27
 78  ω     67.00  94.00   1.00   30.00    --   86.00 -80.00  31.85   27
 79  ω     87.00 120.00   1.00   30.00    --   86.00  77.00 151.06   33
 80  ω     57.00  82.00   1.00   30.00    --   86.00  77.00 151.06   25
 81  ω     62.00  99.00   1.00   30.00    --   86.00  69.00-153.15   37
 82  ω     65.00 103.00   1.00   30.00    --   94.00  75.00  56.99   38
 83  ω     73.00 123.00   1.00   30.00    --   94.00  58.00-120.08   50
 84  ω     69.00 103.00   1.00   30.00    --   98.00  76.00 -58.52   34
 85  ω     79.00 106.00   1.00   30.00    --   98.00  57.00  94.57   27
 86  ω     72.00  98.00   1.00   30.00    --   98.00  72.00 115.04   26
 87  ω     73.00 101.00   1.00   30.00    --   98.00  72.00  20.58   28
 88  ω     75.00 148.00   1.00   30.00    --  102.00  75.00 150.13   73
 89  ω     84.00 157.00   1.00   30.00    --  108.00  38.00 -60.00   73
 90  ω     82.00 142.00   1.00   30.00    --  108.00  38.00-150.00   60
 91  ω     85.00 174.00   1.00   30.00    --  108.00  64.00 -60.00   89
 92  ω     59.00  85.00   1.00   30.00    --  108.00 -38.00 -60.00   26
 93  ω    109.00 170.00   1.00   30.00    --  108.00  77.00   0.00   61
 94  ω     79.00 104.00   1.00   30.00    --  108.00  77.00   0.00   25
 95  ω     83.00 110.00   1.00   30.00    --  108.00  77.00 150.00   27
 96  ω     38.00 140.00   1.00   30.00    --  108.00 -80.00 -69.56  102
 97  ω     85.00 137.00   1.00   30.00    --  108.00  64.00-150.00   52
 98  ω     78.00 104.00   1.00   30.00    --  108.00  77.00  60.00   26
 99  ω     81.00 106.00   1.00   30.00    --  108.00  77.00  30.00   25
100  ω    115.00 140.00   1.00   30.00    --  108.00 -80.00  28.26   25
101  ω     65.00 108.00   1.00   30.00    --  108.00 -80.00  28.26   43
102  ω     78.00 105.00   1.00   30.00    --  108.00  77.00-180.00   27
103  ω     84.00 134.00   1.00   30.00    --  108.00 -77.00 150.00   50
104  ω    115.00 140.00   1.00   30.00    --  108.00 -80.00-126.13   25
105  ω    136.00 166.00   1.00   30.00    --  108.00  77.00 -90.00   30
106  ω     78.00 104.00   1.00   30.00    --  108.00  77.00 -90.00   26
107  ω     79.00 178.00   1.00   30.00    --  108.00  77.00  90.00   99
108  ω    112.00 176.00   1.00   30.00    --  108.00  77.00-150.00   64
109  ω     79.00 104.00   1.00   30.00    --  108.00  77.00-150.00   25
110  ω     86.00 113.00   1.00   30.00    --  108.00  64.00-120.00   27
111  ω     76.00 107.00   1.00   30.00    --  108.00 -79.00-153.19   31
112  ω     86.00 175.00   1.00   30.00    --  108.00  64.00-180.00   89
113  ω     71.00 100.00   1.00   30.00    --  108.00 -80.00-126.13   29
114  ω    151.00 177.00   1.00   30.00    --  108.00  77.00 -60.00   26
115  ω     78.00 104.00   1.00   30.00    --  108.00  77.00 -60.00   26
116  ω     86.00 174.00   1.00   30.00    --  108.00  64.00  60.00   88
117  ω     85.00 111.00   1.00   30.00    --  108.00  64.00   0.00   26
118  ω     79.00 177.00   1.00   30.00    --  108.00  77.00 120.00   98
119  ω    112.00 177.00   1.00   30.00    --  108.00  77.00-120.00   65
120  ω     47.00 139.00   1.00   30.00    --  108.00 -80.00  91.34   92
121  ω     78.00 104.00   1.00   30.00    --  108.00  77.00-120.00   26
122  ω     78.00 177.00   1.00   30.00    --  108.00  77.00 -30.00   99
123  ω     85.00 114.00   1.00   30.00    --  108.00  64.00 -90.00   29
124  ω     84.00 111.00   1.00   30.00    --  108.00 -80.00 -37.07   27
125  ω     80.00 178.00   1.00   30.00    --  108.00  76.00  18.92   98
126  ω     79.00 104.00   1.00   30.00    --  108.00  77.00  74.92   25
127  ω    -70.00  30.00   1.00    5.00    --    0.00 -77.00 120.00  100
128  ω    -21.00  69.00   1.00    5.00    --    0.00  57.00   0.00   90
129  ω    -26.00  72.00   1.00    5.00    --    0.00  38.00  90.00   98
130  ω    -21.00  69.00   1.00    5.00    --    0.00  57.00 150.00   90
131  ω     -6.00  91.00   1.00    5.00    --   22.00  73.00-166.69   97
132  ω     -9.00  47.00   1.00    5.00    --   22.00  79.00-132.18   56
133  ω     -6.00  46.00   1.00    5.00    --   26.00  80.00 125.49   52
134  ω      7.00  49.00   1.00   15.00    --   38.00  78.00 -54.74   42
135  ω     11.00  47.00   1.00   15.00    --   42.00  79.00 152.46   36
136  ω     19.00  47.00   1.00   15.00    --   50.00  79.00  55.32   28
137  ω     19.00  49.00   1.00   15.00    --   50.00  78.00 154.71   30
138  ω     23.00  49.00   1.00   15.00    --   54.00  78.00 -75.57   26
139  ω     23.00  49.00   1.00   15.00    --   54.00  78.00-162.46   26
140  ω    -15.00  75.00   1.00   15.00    --   54.00 -57.00-180.00   90
141  ω    -18.00  80.00   1.00   15.00    --   54.00 -38.00  30.00   98
142  ω     30.00 128.00   1.00   15.00    --   58.00  74.00 133.05   98
143  ω     -5.00  98.00   1.00   15.00    --   66.00 -80.00  57.13  103
144  ω     41.00 134.00   1.00   15.00    --   66.00  69.00 -41.74   93
145  ω     42.00 139.00   1.00   15.00    --   70.00  73.00-162.67   97
146  ω     44.00 139.00   1.00   15.00    --   70.00  70.00 172.27   95
147  ω     41.00 140.00   1.00   15.00    --   70.00  75.00 -80.55   99
148  ω      4.00 105.00   1.00   15.00    --   74.00 -78.00 -82.57  101
149  ω     47.00 143.00   1.00   15.00    --   74.00  72.00  34.24   96
150  ω      3.00 106.00   1.00   15.00    --   74.00 -80.00  96.46  103
151  ω     48.00 143.00   1.00   15.00    --   74.00  70.00 135.48   95
152  ω      3.00 106.00   1.00   15.00    --   74.00 -80.00 150.50  103
153  ω     45.00 135.00   1.00   15.00    --   74.00  76.00  59.16   90
154  ω     46.00 143.00   1.00   15.00    --   74.00  73.00-145.41   97
155  ω     56.00 148.00   1.00   15.00    --   78.00  50.00 -82.22   92
156  ω     51.00 147.00   1.00   15.00    --   78.00  72.00 141.28   96
157  ω     56.00 146.00   1.00   15.00    --   78.00  63.00  46.48   90
158  ω     51.00 147.00   1.00   15.00    --   78.00  72.00  -9.95   96
159  ω     53.00 146.00   1.00   15.00    --   78.00  69.00 -32.50   93
160  ω     55.00 146.00   1.00   15.00    --   78.00  65.00 103.45   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0551686000
_diffrn_orient_matrix_UB_12      0.1553099000
_diffrn_orient_matrix_UB_13      0.0043282000
_diffrn_orient_matrix_UB_21      0.0085647000
_diffrn_orient_matrix_UB_22      -0.0009746000
_diffrn_orient_matrix_UB_23      0.0970682000
_diffrn_orient_matrix_UB_31      0.0937449000
_diffrn_orient_matrix_UB_32      0.0914091000
_diffrn_orient_matrix_UB_33      -0.0063390000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.922
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                2778
_reflns_number_total             3420
_reflns_odcompleteness_completeness 99.85
_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 1.171.38.46 (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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-17); encifer 1.5.2 (CCDC, 2016)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_shelxl_version_number           2018/1
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 
;
 Flack x determined using 981 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.3(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.226
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3420
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1151
_refine_ls_R_factor_gt           0.0928
_refine_ls_restrained_S_all      1.225
_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)+(0.1589P)²+1.2955P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2666
_refine_ls_wR_factor_ref         0.3170
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12), C13(H13),
 C15(H15), C16(H16), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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
F1 F -0.9845(4) -0.3075(7) -0.2565(5) 0.0962(19) Uani 1 1 d . . . . .
F2 F -0.6520(6) -1.0057(9) -0.1826(6) 0.132(3) Uani 1 1 d . . . . .
N1 N -0.6052(5) -0.1928(8) -0.4798(5) 0.0716(19) Uani 1 1 d . . . . .
N2 N -0.5113(6) -0.6692(8) -0.5196(6) 0.077(2) Uani 1 1 d . . . . .
C1 C -0.6668(6) -0.4574(10) -0.4575(6) 0.071(2) Uani 1 1 d . . . . .
H1 H -0.685849 -0.546645 -0.494650 0.085 Uiso 1 1 calc R . . . .
C2 C -0.5799(6) -0.5081(10) -0.4064(7) 0.073(2) Uani 1 1 d . . . . .
H2 H -0.558782 -0.416513 -0.371831 0.087 Uiso 1 1 calc R . . . .
C3 C -0.7505(6) -0.4189(10) -0.3992(6) 0.071(2) Uani 1 1 d . . . . .
C4 C -0.8359(7) -0.4905(12) -0.4127(8) 0.079(2) Uani 1 1 d . . . . .
H4 H -0.841029 -0.567218 -0.455872 0.095 Uiso 1 1 calc R . . . .
C5 C -0.9157(7) -0.4533(12) -0.3645(7) 0.080(3) Uani 1 1 d . . . . .
H5 H -0.974907 -0.502489 -0.374692 0.096 Uiso 1 1 calc R . . . .
C6 C -0.9058(7) -0.3461(11) -0.3034(7) 0.076(2) Uani 1 1 d . . . . .
C7 C -0.8217(7) -0.2738(10) -0.2840(6) 0.076(2) Uani 1 1 d . . . . .
H7 H -0.817109 -0.201204 -0.238714 0.091 Uiso 1 1 calc R . . . .
C8 C -0.7429(7) -0.3116(9) -0.3339(7) 0.073(2) Uani 1 1 d . . . . .
H8 H -0.683698 -0.263142 -0.322857 0.088 Uiso 1 1 calc R . . . .
C9 C -0.6442(6) -0.3183(9) -0.5136(6) 0.0659(19) Uani 1 1 d . . . . .
C10 C -0.6693(7) -0.3237(12) -0.6005(8) 0.083(3) Uani 1 1 d . . . . .
H10 H -0.696916 -0.415206 -0.623962 0.100 Uiso 1 1 calc R . . . .
C11 C -0.6527(8) -0.1922(13) -0.6507(7) 0.085(3) Uani 1 1 d . . . . .
H11 H -0.669116 -0.191035 -0.708974 0.102 Uiso 1 1 calc R . . . .
C12 C -0.6122(7) -0.0657(12) -0.6130(7) 0.079(2) Uani 1 1 d . . . . .
H12 H -0.600735 0.026756 -0.644707 0.095 Uiso 1 1 calc R . . . .
C13 C -0.5877(7) -0.0719(11) -0.5283(7) 0.076(2) Uani 1 1 d . . . . .
H13 H -0.556702 0.016029 -0.504076 0.091 Uiso 1 1 calc R . . . .
C14 C -0.6019(6) -0.6418(10) -0.3461(6) 0.070(2) Uani 1 1 d . . . . .
C15 C -0.5714(7) -0.6314(12) -0.2622(7) 0.082(3) Uani 1 1 d . . . . .
H15 H -0.539431 -0.540434 -0.242720 0.098 Uiso 1 1 calc R . . . .
C16 C -0.5884(9) -0.7551(17) -0.2077(8) 0.101(4) Uani 1 1 d . . . . .
H16 H -0.567520 -0.750721 -0.150704 0.121 Uiso 1 1 calc R . . . .
C17 C -0.6356(9) -0.8836(13) -0.2371(10) 0.099(4) Uani 1 1 d . . . . .
C18 C -0.6669(9) -0.8947(13) -0.3167(10) 0.097(4) Uani 1 1 d . . . . .
H18 H -0.700071 -0.985397 -0.334853 0.116 Uiso 1 1 calc R . . . .
C19 C -0.6508(7) -0.7740(10) -0.3717(7) 0.079(3) Uani 1 1 d . . . . .
H19 H -0.673414 -0.781049 -0.428117 0.095 Uiso 1 1 calc R . . . .
C20 C -0.4999(6) -0.5501(9) -0.4666(6) 0.068(2) Uani 1 1 d . . . . .
C21 C -0.4172(7) -0.4661(11) -0.4645(7) 0.079(2) Uani 1 1 d . . . . .
H21 H -0.410193 -0.382557 -0.425370 0.095 Uiso 1 1 calc R . . . .
C22 C -0.3436(7) -0.5028(13) -0.5195(9) 0.088(3) Uani 1 1 d . . . . .
H22 H -0.286946 -0.442965 -0.519895 0.105 Uiso 1 1 calc R . . . .
C23 C -0.3549(7) -0.6273(12) -0.5731(7) 0.079(2) Uani 1 1 d . . . . .
H23 H -0.305598 -0.658375 -0.610354 0.095 Uiso 1 1 calc R . . . .
C24 C -0.4402(8) -0.7063(10) -0.5713(6) 0.076(2) Uani 1 1 d . . . . .
H24 H -0.448656 -0.791825 -0.608918 0.092 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
F1 C6 1.377(11) . ?
F2 C17 1.373(12) . ?
N1 C9 1.319(11) . ?
N1 C13 1.310(12) . ?
N2 C20 1.329(11) . ?
N2 C24 1.334(13) . ?
C1 H1 1.0000 . ?
C1 C2 1.533(12) . ?
C1 C3 1.534(13) . ?
C1 C9 1.518(12) . ?
C2 H2 1.0000 . ?
C2 C14 1.520(13) . ?
C2 C20 1.521(13) . ?
C3 C4 1.369(14) . ?
C3 C8 1.385(15) . ?
C4 H4 0.9500 . ?
C4 C5 1.397(15) . ?
C5 H5 0.9500 . ?
C5 C6 1.339(15) . ?
C6 C7 1.373(14) . ?
C7 H7 0.9500 . ?
C7 C8 1.402(14) . ?
C8 H8 0.9500 . ?
C9 C10 1.421(16) . ?
C10 H10 0.9500 . ?
C10 C11 1.397(15) . ?
C11 H11 0.9500 . ?
C11 C12 1.361(16) . ?
C12 H12 0.9500 . ?
C12 C13 1.386(15) . ?
C13 H13 0.9500 . ?
C14 C15 1.399(15) . ?
C14 C19 1.385(14) . ?
C15 H15 0.9500 . ?
C15 C16 1.385(17) . ?
C16 H16 0.9500 . ?
C16 C17 1.37(2) . ?
C17 C18 1.34(2) . ?
C18 H18 0.9500 . ?
C18 C19 1.368(16) . ?
C19 H19 0.9500 . ?
C20 C21 1.371(14) . ?
C21 H21 0.9500 . ?
C21 C22 1.392(15) . ?
C22 H22 0.9500 . ?
C22 C23 1.370(15) . ?
C23 H23 0.9500 . ?
C23 C24 1.381(15) . ?
C24 H24 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
C13 N1 C9 118.9(9) . . ?
C20 N2 C24 118.5(8) . . ?
C2 C1 H1 108.1 . . ?
C2 C1 C3 111.1(8) . . ?
C3 C1 H1 108.1 . . ?
C9 C1 H1 108.1 . . ?
C9 C1 C2 111.2(7) . . ?
C9 C1 C3 110.2(7) . . ?
C1 C2 H2 107.8 . . ?
C14 C2 C1 112.3(7) . . ?
C14 C2 H2 107.8 . . ?
C14 C2 C20 111.5(7) . . ?
C20 C2 C1 109.4(8) . . ?
C20 C2 H2 107.8 . . ?
C4 C3 C1 119.3(9) . . ?
C4 C3 C8 118.6(9) . . ?
C8 C3 C1 122.1(8) . . ?
C3 C4 H4 119.2 . . ?
C3 C4 C5 121.6(11) . . ?
C5 C4 H4 119.2 . . ?
C4 C5 H5 121.1 . . ?
C6 C5 C4 117.7(10) . . ?
C6 C5 H5 121.1 . . ?
C5 C6 F1 117.9(9) . . ?
C5 C6 C7 124.0(9) . . ?
C7 C6 F1 118.1(9) . . ?
C6 C7 H7 121.4 . . ?
C6 C7 C8 117.1(9) . . ?
C8 C7 H7 121.4 . . ?
C3 C8 C7 120.8(9) . . ?
C3 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
N1 C9 C1 119.2(8) . . ?
N1 C9 C10 121.5(8) . . ?
C10 C9 C1 119.2(8) . . ?
C9 C10 H10 120.5 . . ?
C11 C10 C9 118.9(9) . . ?
C11 C10 H10 120.5 . . ?
C10 C11 H11 121.3 . . ?
C12 C11 C10 117.3(10) . . ?
C12 C11 H11 121.3 . . ?
C11 C12 H12 120.0 . . ?
C11 C12 C13 120.0(10) . . ?
C13 C12 H12 120.0 . . ?
N1 C13 C12 123.3(10) . . ?
N1 C13 H13 118.3 . . ?
C12 C13 H13 118.3 . . ?
C15 C14 C2 119.0(9) . . ?
C19 C14 C2 122.1(9) . . ?
C19 C14 C15 118.9(9) . . ?
C14 C15 H15 120.4 . . ?
C16 C15 C14 119.3(11) . . ?
C16 C15 H15 120.4 . . ?
C15 C16 H16 120.4 . . ?
C17 C16 C15 119.1(12) . . ?
C17 C16 H16 120.4 . . ?
C16 C17 F2 118.7(15) . . ?
C18 C17 F2 118.7(14) . . ?
C18 C17 C16 122.6(10) . . ?
C17 C18 H18 120.3 . . ?
C17 C18 C19 119.3(12) . . ?
C19 C18 H18 120.3 . . ?
C14 C19 H19 119.6 . . ?
C18 C19 C14 120.8(11) . . ?
C18 C19 H19 119.6 . . ?
N2 C20 C2 119.1(8) . . ?
N2 C20 C21 121.3(8) . . ?
C21 C20 C2 119.6(8) . . ?
C20 C21 H21 119.9 . . ?
C20 C21 C22 120.2(9) . . ?
C22 C21 H21 119.9 . . ?
C21 C22 H22 120.8 . . ?
C23 C22 C21 118.4(9) . . ?
C23 C22 H22 120.8 . . ?
C22 C23 H23 121.0 . . ?
C22 C23 C24 117.9(9) . . ?
C24 C23 H23 121.0 . . ?
N2 C24 C23 123.6(9) . . ?
N2 C24 H24 118.2 . . ?
C23 C24 H24 118.2 . . ?

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
F1 C6 C7 C8 -178.3(7) . . . . ?
F2 C17 C18 C19 -179.8(9) . . . . ?
N1 C9 C10 C11 -0.5(15) . . . . ?
N2 C20 C21 C22 1.1(16) . . . . ?
C1 C2 C14 C15 -132.4(9) . . . . ?
C1 C2 C14 C19 47.9(11) . . . . ?
C1 C2 C20 N2 -63.0(10) . . . . ?
C1 C2 C20 C21 117.9(10) . . . . ?
C1 C3 C4 C5 -176.4(9) . . . . ?
C1 C3 C8 C7 177.2(8) . . . . ?
C1 C9 C10 C11 176.7(9) . . . . ?
C2 C1 C3 C4 -126.6(9) . . . . ?
C2 C1 C3 C8 54.5(11) . . . . ?
C2 C1 C9 N1 -52.6(10) . . . . ?
C2 C1 C9 C10 130.2(9) . . . . ?
C2 C14 C15 C16 -177.8(8) . . . . ?
C2 C14 C19 C18 177.9(9) . . . . ?
C2 C20 C21 C22 -179.7(10) . . . . ?
C3 C1 C2 C14 53.8(10) . . . . ?
C3 C1 C2 C20 178.2(7) . . . . ?
C3 C1 C9 N1 71.1(10) . . . . ?
C3 C1 C9 C10 -106.1(10) . . . . ?
C3 C4 C5 C6 -0.8(15) . . . . ?
C4 C3 C8 C7 -1.7(13) . . . . ?
C4 C5 C6 F1 179.1(8) . . . . ?
C4 C5 C6 C7 -1.7(14) . . . . ?
C5 C6 C7 C8 2.5(14) . . . . ?
C6 C7 C8 C3 -0.7(13) . . . . ?
C8 C3 C4 C5 2.5(15) . . . . ?
C9 N1 C13 C12 3.1(14) . . . . ?
C9 C1 C2 C14 176.9(8) . . . . ?
C9 C1 C2 C20 -58.7(9) . . . . ?
C9 C1 C3 C4 109.7(9) . . . . ?
C9 C1 C3 C8 -69.2(11) . . . . ?
C9 C10 C11 C12 0.6(16) . . . . ?
C10 C11 C12 C13 1.1(16) . . . . ?
C11 C12 C13 N1 -3.1(15) . . . . ?
C13 N1 C9 C1 -178.5(8) . . . . ?
C13 N1 C9 C10 -1.3(13) . . . . ?
C14 C2 C20 N2 61.9(11) . . . . ?
C14 C2 C20 C21 -117.3(10) . . . . ?
C14 C15 C16 C17 -0.8(15) . . . . ?
C15 C14 C19 C18 -1.8(14) . . . . ?
C15 C16 C17 F2 179.9(9) . . . . ?
C15 C16 C17 C18 -0.5(17) . . . . ?
C16 C17 C18 C19 0.6(17) . . . . ?
C17 C18 C19 C14 0.6(16) . . . . ?
C19 C14 C15 C16 1.9(14) . . . . ?
C20 N2 C24 C23 -0.2(15) . . . . ?
C20 C2 C14 C15 104.5(10) . . . . ?
C20 C2 C14 C19 -75.3(11) . . . . ?
C20 C21 C22 C23 -2.2(17) . . . . ?
C21 C22 C23 C24 2.1(17) . . . . ?
C22 C23 C24 N2 -0.9(16) . . . . ?
C24 N2 C20 C2 -179.1(8) . . . . ?
C24 N2 C20 C21 0.1(14) . . . . ?

_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 14.959
_oxdiff_exptl_absorpt_empirical_full_min 0.092
_cell_oxdiff_length_a            14.1194(3)
_cell_oxdiff_length_b            8.5484(2)
_cell_oxdiff_length_c            15.8215(3)
_cell_oxdiff_angle_alpha         89.9940(16)
_cell_oxdiff_angle_beta          89.9910(15)
_cell_oxdiff_angle_gamma         89.9786(18)
_cell_oxdiff_volume              1909.64(7)
_cell_oxdiff_measurement_reflns_used 15217
_diffrn_measurement_specimen_support 'polyimid foil'
####################################################################### 
# 
# 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_ga_ff22
_database_code_depnum_ccdc_archive 'CCDC 1817692'
_audit_update_record             
;
2018-01-17 deposited with the CCDC.
2018-02-05 downloaded from the CCDC.
;
_audit_creation_date             2017-11-22

_audit_block_code                ga_ff22
_audit_block_refno               2982
_audit_block_usercomment         'FF465, plate, colourless'


_audit_creation_method           
;
Olex2 1.2
(compiled Aug 10 2017 17:44:14 for OlexSys, GUI svn.r5381)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C45 H33 N, 0.5(C5 H12)'
_chemical_formula_sum            'C47.50 H39 N'
_chemical_formula_weight         623.79
_chemical_melting_point          ?
_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_diffrn_ambient_temperature      120(1)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'
_chemical_absolute_configuration .
loop_
_symmetry_equiv_pos_as_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                   17.51974(11)
_cell_length_b                   9.24966(5)
_cell_length_c                   22.74222(19)
_cell_angle_alpha                90
_cell_angle_beta                 107.3819(8)
_cell_angle_gamma                90
_cell_volume                     3517.12(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    56452
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      70.8480
_cell_measurement_theta_min      3.7810
_shelx_estimated_absorpt_T_max   0.951
_shelx_estimated_absorpt_T_min   0.951
_exptl_absorpt_coefficient_mu    0.508
_exptl_absorpt_correction_T_max  1.155
_exptl_absorpt_correction_T_min  0.924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1324
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 0 12 0.0547
-3 0 -12 0.0547
-2 6 0 0.0644
1 -6 0 0.0766
-11 -1 9 0.0122
11 1 -9 0.0052
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.017
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
3.0000 0.0000 12.0000 -0.0169 0.1108 0.9643
-3.0000 -0.0000 -12.0000 0.0169 -0.1108 -0.9643
-2.0000 6.0000 -0.0000 0.1178 -1.0090 0.0168
1.0000 -6.0000 0.0000 -0.0398 1.0005 -0.0652
-11.0000 -1.0000 8.9999 1.0269 0.1356 0.0635
11.0000 1.0000 -8.9999 -1.0269 -0.1356 -0.0635

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_unetI/netI     0.0134
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            175052
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.926
_diffrn_reflns_theta_min         3.789
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -72.00  26.00   1.00    1.00    --    0.00 -38.00  90.00   98
  2  ω    -21.00  69.00   1.00    1.00    --    0.00  57.00 120.00   90
  3  ω    -26.00  72.00   1.00    1.00    --    0.00  38.00 -60.00   98
  4  ω    -69.00  21.00   1.00    1.00    --    0.00 -57.00 -30.00   90
  5  ω    -42.00   5.00   1.00    1.00    --   10.00 117.00  -7.56   47
  6  ω    -35.00  -1.00   1.00    1.00    --   22.00 124.00 -84.15   34
  7  ω    -22.00   5.00   1.00    4.00    --   30.00 117.00  93.35   27
  8  ω      5.00  32.00   1.00    4.00    --   42.00  90.00 178.70   27
  9  ω      5.00  32.00   1.00    4.00    --   42.00  90.00  26.50   27
 10  ω      5.00  32.00   1.00    4.00    --   42.00  90.00 -82.97   27
 11  ω     13.00  45.00   1.00    4.00    --   46.00  82.00-134.42   32
 12  ω     12.00  38.00   1.00    4.00    --   46.00  84.00 -36.66   26
 13  ω     13.00  40.00   1.00    4.00    --   46.00  83.00  83.48   27
 14  ω     12.00  38.00   1.00    4.00    --   46.00  84.00 137.07   26
 15  ω     12.00  38.00   1.00    4.00    --   46.00  84.00 -84.40   26
 16  ω     13.00  40.00   1.00    4.00    --   46.00  83.00  27.55   27
 17  ω     21.00 120.00   1.00    4.00    --   50.00  76.00  68.75   99
 18  ω     17.00  45.00   1.00    4.00    --   50.00  82.00 -13.42   28
 19  ω     18.00  46.00   1.00    4.00    --   50.00  81.00 119.50   28
 20  ω     17.00  45.00   1.00    4.00    --   50.00  82.00-177.85   28
 21  ω     17.00  45.00   1.00    4.00    --   50.00  82.00  34.00   28
 22  ω     24.00 124.00   1.00    4.00    --   54.00  77.00 -30.00  100
 23  ω     24.00 124.00   1.00    4.00    --   54.00  77.00-120.00  100
 24  ω     24.00 124.00   1.00    4.00    --   54.00  77.00  90.00  100
 25  ω     24.00 124.00   1.00    4.00    --   54.00  77.00   0.00  100
 26  ω     24.00 124.00   1.00    4.00    --   54.00  77.00 -90.00  100
 27  ω     24.00 124.00   1.00    4.00    --   54.00  77.00 120.00  100
 28  ω    -15.00  75.00   1.00    4.00    --   54.00 -57.00  30.00   90
 29  ω     24.00 124.00   1.00    4.00    --   54.00  77.00-150.00  100
 30  ω     23.00 111.00   1.00    4.00    --   54.00-125.00-150.00   88
 31  ω    -15.00  75.00   1.00    4.00    --   54.00 -57.00 -60.00   90
 32  ω     25.00 124.00   1.00    4.00    --   54.00  75.00 145.70   99
 33  ω      1.00  96.00   1.00    4.00    --   54.00 -99.00-150.00   95
 34  ω     24.00 124.00   1.00    4.00    --   54.00  77.00  30.00  100
 35  ω     24.00 124.00   1.00    4.00    --   54.00  77.00 -60.00  100
 36  ω     35.00 125.00   1.00    4.00    --   58.00  64.00 -35.86   90
 37  ω     34.00 126.00   1.00    4.00    --   58.00  68.00 144.39   92
 38  ω     29.00 128.00   1.00    4.00    --   58.00  75.00  29.59   99
 39  ω     31.00 127.00   1.00    4.00    --   58.00  71.00  61.73   96
 40  ω     35.00 126.00   1.00    4.00    --   58.00  66.00  85.44   91
 41  ω     28.00 128.00   1.00    4.00    --   58.00  77.00 167.92  100
 42  ω     35.00 131.00   1.00    4.00    --   62.00  72.00  -3.57   96
 43  ω     37.00 130.00   1.00    4.00    --   62.00  69.00-129.42   93
 44  ω     39.00 130.00   1.00    4.00    --   62.00  65.00-170.05   91
 45  ω     41.00 131.00   1.00    4.00    --   62.00  54.00 -57.75   90
 46  ω     33.00 132.00   1.00    4.00    --   62.00  76.00 150.25   99
 47  ω     37.00 136.00   1.00    4.00    --   66.00  76.00  24.37   99
 48  ω     41.00 134.00   1.00    4.00    --   66.00  69.00  55.28   93
 49  ω     37.00 136.00   1.00    4.00    --   66.00  76.00  91.35   99
 50  ω     39.00 135.00   1.00    4.00    --   66.00  71.00-154.18   96
 51  ω     44.00 134.00   1.00    4.00    --   66.00  63.00 -68.49   90
 52  ω     45.00 135.00   1.00    4.00    --   66.00  56.00-176.36   90
 53  ω     46.00 138.00   1.00    4.00    --   70.00  67.00  70.46   92
 54  ω     48.00 138.00   1.00    4.00    --   70.00  61.00 -96.93   90
 55  ω     45.00 142.00   1.00    4.00    --   70.00  41.00   5.88   97
 56  ω     42.00 140.00   1.00    4.00    --   70.00  74.00-146.12   98
 57  ω     44.00 144.00   1.00    4.00    --   74.00  77.00-143.80  100
 58  ω     53.00 143.00   1.00    4.00    --   74.00  55.00 179.59   90
 59  ω     46.00 144.00   1.00    4.00    --   74.00  74.00-177.70   98
 60  ω     49.00 142.00   1.00    4.00    --   74.00  69.00 -86.32   93
 61  ω     55.00 146.00   1.00    4.00    --   78.00  65.00 127.83   91
 62  ω     57.00 147.00   1.00    4.00    --   78.00  58.00 -29.71   90
 63  ω     49.00 148.00   1.00    4.00    --   78.00  75.00  71.58   99
 64  ω     48.00 148.00   1.00    4.00    --   78.00  77.00  -4.02  100
 65  ω     48.00 148.00   1.00    4.00    --   78.00  77.00 166.80  100
 66  ω     49.00 148.00   1.00    4.00    --   78.00  75.00 129.00   99
 67  ω     60.00 150.00   1.00   10.00    --   82.00  61.00-175.37   90
 68  ω     59.00 153.00   1.00   10.00    --   82.00  48.00  38.56   94
 69  ω     55.00 151.00   1.00   10.00    --   82.00  71.00-140.33   96
 70  ω     55.00 151.00   1.00   10.00    --   82.00  71.00  47.28   96
 71  ω     54.00 152.00   1.00   10.00    --   82.00  74.00  87.96   98
 72  ω     58.00 156.00   1.00   10.00    --   86.00  74.00-155.58   98
 73  ω     56.00 156.00   1.00   10.00    --   86.00  77.00  17.57  100
 74  ω     59.00 155.00   1.00   10.00    --   86.00  72.00 -38.82   96
 75  ω     57.00 156.00   1.00   10.00    --   86.00  75.00 -90.21   99
 76  ω     57.00 156.00   1.00   10.00    --   86.00  76.00 -45.91   99
 77  ω     61.00 160.00   1.00   10.00    --   90.00  75.00   8.45   99
 78  ω     61.00 160.00   1.00   10.00    --   90.00  76.00 157.31   99
 79  ω     62.00 159.00   1.00   10.00    --   90.00  73.00-139.41   97
 80  ω     61.00 160.00   1.00   10.00    --   90.00  76.00 -25.36   99
 81  ω     65.00 164.00   1.00   10.00    --   94.00  75.00-111.25   99
 82  ω     76.00 166.00   1.00   10.00    --   98.00  61.00 146.63   90
 83  ω     77.00 167.00   1.00   10.00    --   98.00  55.00 143.70   90
 84  ω     75.00 171.00   1.00   10.00    --  102.00  71.00  60.88   96
 85  ω     79.00 173.00   1.00   10.00    --  102.00  48.00 -29.19   94
 86  ω     80.00 177.00   1.00   10.00    --  108.00  73.00 145.96   97
 87  ω     85.00 176.00   1.00   10.00    --  108.00  65.00-100.72   91
 88  ω     81.00 177.00   1.00   10.00    --  108.00  71.00 -67.83   96
 89  ω     36.00 116.00   1.00   10.00    --  108.00-111.00-180.00   80
 90  ω     82.00 178.00   1.00   10.00    --  108.00  38.00 150.00   96
 91  ω     36.00 116.00   1.00   10.00    --  108.00-111.00  30.00   80
 92  ω     85.00 175.00   1.00   10.00    --  108.00  64.00-180.00   90
 93  ω     85.00 175.00   1.00   10.00    --  108.00  64.00  90.00   90
 94  ω     85.00 175.00   1.00   10.00    --  108.00  64.00 -30.00   90
 95  ω     78.00 178.00   1.00   10.00    --  108.00  77.00 150.00  100
 96  ω     78.00 178.00   1.00   10.00    --  108.00  77.00-150.00  100
 97  ω     78.00 178.00   1.00   10.00    --  108.00  77.00 -60.00  100
 98  ω     78.00 178.00   1.00   10.00    --  108.00  77.00  60.00  100
 99  ω     78.00 178.00   1.00   10.00    --  108.00  77.00  30.00  100
100  ω     78.00 178.00   1.00   10.00    --  108.00  77.00-120.00  100
101  ω     78.00 178.00   1.00   10.00    --  108.00  77.00 -90.00  100
102  ω     78.00 178.00   1.00   10.00    --  108.00  77.00   0.00  100
103  ω     78.00 178.00   1.00   10.00    --  108.00  77.00 120.00  100
104  ω     78.00 178.00   1.00   10.00    --  108.00  77.00-180.00  100
105  ω     36.00 116.00   1.00   10.00    --  108.00-111.00 120.00   80
106  ω    100.00 178.00   1.00   10.00    --  108.00 111.00 150.00   78
107  ω     36.00 146.00   1.00   10.00    --  108.00 -92.00-180.00  110
108  ω     85.00 175.00   1.00   10.00    --  108.00  64.00  30.00   90
109  ω     85.00 175.00   1.00   10.00    --  108.00  64.00-150.00   90
110  ω     85.00 175.00   1.00   10.00    --  108.00  64.00   0.00   90
111  ω     85.00 175.00   1.00   10.00    --  108.00  64.00 120.00   90
112  ω     78.00 178.00   1.00   10.00    --  108.00  77.00  90.00  100
113  ω    100.00 178.00   1.00   10.00    --  108.00 111.00  30.00   78
114  ω     78.00 178.00   1.00   10.00    --  108.00  77.00 -30.00  100
115  ω    100.00 178.00   1.00   10.00    --  108.00 111.00-180.00   78
116  ω     36.00 146.00   1.00   10.00    --  108.00 -92.00 120.00  110
117  ω     82.00 178.00   1.00   10.00    --  108.00  38.00 120.00   96
118  ω     36.00 116.00   1.00   10.00    --  108.00-111.00   0.00   80
119  ω     82.00 178.00   1.00   10.00    --  108.00  38.00  60.00   96
120  ω     82.00 178.00   1.00   10.00    --  108.00  38.00 -30.00   96
121  ω     82.00 178.00   1.00   10.00    --  108.00  38.00-120.00   96
122  ω     85.00 175.00   1.00   10.00    --  108.00  64.00-120.00   90
123  ω    100.00 178.00   1.00   10.00    --  108.00 111.00 -30.00   78
124  ω     80.00 178.00   1.00   10.00    --  108.00  74.00 -19.83   98
125  φ      0.00  97.00   1.00    1.00   0.00   0.00 -40.00    --    97
126  φ      0.00 270.00   1.00    0.20   0.00   0.00   0.00    --   270
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0779749000
_diffrn_orient_matrix_UB_12      -0.0063661000
_diffrn_orient_matrix_UB_13      0.0180867000
_diffrn_orient_matrix_UB_21      0.0085173000
_diffrn_orient_matrix_UB_22      -0.1653256000
_diffrn_orient_matrix_UB_23      0.0071041000
_diffrn_orient_matrix_UB_31      0.0483596000
_diffrn_orient_matrix_UB_32      0.0189206000
_diffrn_orient_matrix_UB_33      0.0682671000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6216
_reflns_number_total             6766
_reflns_odcompleteness_completeness 99.96
_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 1.171.38.46 (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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-17); encifer 1.5.2 (CCDC, 2016)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_shelxl_version_number           2017/1
_computing_structure_solution    'SIR2014 (Giacovazzo et al., 2014)'
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         6766
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0497
_refine_ls_restrained_S_all      1.073
_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)+(0.0468P)²+2.4013P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1185
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C81-C82 = C84-C85
 1.5 with sigma of 0.01
 C82-C83 = C83-C84
 1.5 with sigma of 0.01
 C81-C83 = C82-C84 = C83-C85
 2.53 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C81, C82, C83, C84
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C81(0.5) H81A(0.5) H81B(0.5) H81C(0.5) C82(0.5) H82A(0.5)
 H82B(0.5) C83(0.5) H83A(0.5) H83B(0.5) C84(0.5) H84A(0.5) H84B(0.5) C85(0.5)
 H85A(0.5) H85B(0.5) H85C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B)
5.b Me refined with riding coordinates:
 C81(H81A,H81B,H81C), C85(H85A,H85B,H85C)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13),
 C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23),
  C24(H24), C25(H25), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33),
 C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C41(H41), C42(H42), C43(H43),
  C44(H44), C45(H45)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.01532(7) 0.19098(13) 0.65620(5) 0.0195(2) Uani 1 1 d . . . . .
C1 C -0.04006(8) 0.25118(15) 0.67849(6) 0.0201(3) Uani 1 1 d . . . . .
C2 C -0.03258(9) 0.39076(16) 0.70254(7) 0.0239(3) Uani 1 1 d . . . . .
H2 H -0.072827 0.429996 0.718065 0.029 Uiso 1 1 calc R . . . .
C3 C 0.03419(9) 0.47139(16) 0.70350(7) 0.0248(3) Uani 1 1 d . . . . .
H3 H 0.040286 0.567174 0.719296 0.030 Uiso 1 1 calc R . . . .
C4 C 0.09202(8) 0.41032(16) 0.68107(7) 0.0226(3) Uani 1 1 d . . . . .
H4 H 0.138731 0.462946 0.681462 0.027 Uiso 1 1 calc R . . . .
C5 C 0.08026(8) 0.27022(15) 0.65796(6) 0.0190(3) Uani 1 1 d . . . . .
C6 C -0.10977(8) 0.15543(15) 0.67663(6) 0.0202(3) Uani 1 1 d . . . . .
C7 C -0.18624(9) 0.19517(16) 0.64836(7) 0.0221(3) Uani 1 1 d . . . . .
C8 C -0.08703(8) 0.01481(16) 0.70918(7) 0.0219(3) Uani 1 1 d . . . . .
C9 C -0.03024(10) 0.01336(18) 0.76735(8) 0.0312(4) Uani 1 1 d . . . . .
H9 H -0.004662 0.100837 0.784441 0.037 Uiso 1 1 calc R . . . .
C10 C -0.01082(11) -0.1143(2) 0.80039(9) 0.0405(4) Uani 1 1 d . . . . .
H10 H 0.027686 -0.113753 0.839969 0.049 Uiso 1 1 calc R . . . .
C11 C -0.04739(11) -0.24277(19) 0.77589(9) 0.0396(4) Uani 1 1 d . . . . .
H11 H -0.035180 -0.329822 0.798968 0.048 Uiso 1 1 calc R . . . .
C12 C -0.10184(10) -0.24329(18) 0.71753(9) 0.0344(4) Uani 1 1 d . . . . .
H12 H -0.126296 -0.331395 0.700177 0.041 Uiso 1 1 calc R . . . .
C13 C -0.12081(9) -0.11622(16) 0.68436(7) 0.0259(3) Uani 1 1 d . . . . .
H13 H -0.157461 -0.118345 0.644016 0.031 Uiso 1 1 calc R . . . .
C14 C -0.20721(9) 0.33636(17) 0.61587(7) 0.0290(3) Uani 1 1 d . . . . .
C15 C -0.17063(11) 0.3853(2) 0.57301(9) 0.0441(5) Uani 1 1 d . . . . .
H15 H -0.133955 0.324879 0.561087 0.053 Uiso 1 1 calc R . . . .
C16 C -0.18796(15) 0.5231(3) 0.54761(11) 0.0675(8) Uani 1 1 d . . . . .
H16 H -0.162931 0.556212 0.518360 0.081 Uiso 1 1 calc R . . . .
C17 C -0.24091(17) 0.6116(2) 0.56451(13) 0.0761(10) Uani 1 1 d . . . . .
H17 H -0.250837 0.706594 0.548157 0.091 Uiso 1 1 calc R . . . .
C18 C -0.27954(15) 0.5622(2) 0.60519(12) 0.0647(7) Uani 1 1 d . . . . .
H18 H -0.317018 0.622542 0.616150 0.078 Uiso 1 1 calc R . . . .
C19 C -0.26391(11) 0.42466(19) 0.63021(9) 0.0413(4) Uani 1 1 d . . . . .
H19 H -0.291950 0.390228 0.657281 0.050 Uiso 1 1 calc R . . . .
C20 C -0.25557(8) 0.10084(16) 0.64837(7) 0.0234(3) Uani 1 1 d . . . . .
C21 C -0.31056(9) 0.06198(19) 0.59246(8) 0.0318(4) Uani 1 1 d . . . . .
H21 H -0.306003 0.101504 0.555098 0.038 Uiso 1 1 calc R . . . .
C22 C -0.37196(10) -0.0342(2) 0.59102(9) 0.0382(4) Uani 1 1 d . . . . .
H22 H -0.408944 -0.060571 0.552669 0.046 Uiso 1 1 calc R . . . .
C23 C -0.37956(10) -0.0916(2) 0.64502(9) 0.0382(4) Uani 1 1 d . . . . .
H23 H -0.421278 -0.158138 0.643889 0.046 Uiso 1 1 calc R . . . .
C24 C -0.32606(10) -0.0517(2) 0.70079(9) 0.0360(4) Uani 1 1 d . . . . .
H24 H -0.331048 -0.091085 0.738042 0.043 Uiso 1 1 calc R . . . .
C25 C -0.26516(9) 0.04563(18) 0.70257(8) 0.0292(3) Uani 1 1 d . . . . .
H25 H -0.229712 0.074764 0.741146 0.035 Uiso 1 1 calc R . . . .
C26 C 0.13946(8) 0.20430(15) 0.63009(6) 0.0198(3) Uani 1 1 d . . . . .
C27 C 0.21493(8) 0.17635(15) 0.66531(7) 0.0201(3) Uani 1 1 d . . . . .
C28 C 0.10720(8) 0.18046(16) 0.56247(7) 0.0219(3) Uani 1 1 d . . . . .
C29 C 0.12646(9) 0.05743(18) 0.53440(7) 0.0279(3) Uani 1 1 d . . . . .
H29 H 0.163217 -0.010966 0.558382 0.034 Uiso 1 1 calc R . . . .
C30 C 0.09239(10) 0.0341(2) 0.47175(8) 0.0348(4) Uani 1 1 d . . . . .
H30 H 0.105820 -0.050345 0.453221 0.042 Uiso 1 1 calc R . . . .
C31 C 0.03909(9) 0.1327(2) 0.43608(8) 0.0365(4) Uani 1 1 d . . . . .
H31 H 0.016056 0.116273 0.393181 0.044 Uiso 1 1 calc R . . . .
C32 C 0.01946(10) 0.2553(2) 0.46318(7) 0.0340(4) Uani 1 1 d . . . . .
H32 H -0.016705 0.323984 0.438768 0.041 Uiso 1 1 calc R . . . .
C33 C 0.05255(9) 0.27836(18) 0.52606(7) 0.0270(3) Uani 1 1 d . . . . .
H33 H 0.037799 0.361764 0.544501 0.032 Uiso 1 1 calc R . . . .
C34 C 0.23870(8) 0.18449(15) 0.73394(7) 0.0211(3) Uani 1 1 d . . . . .
C35 C 0.30930(9) 0.25456(16) 0.76665(7) 0.0244(3) Uani 1 1 d . . . . .
H35 H 0.342450 0.296591 0.744979 0.029 Uiso 1 1 calc R . . . .
C36 C 0.33150(10) 0.26341(17) 0.83046(7) 0.0306(4) Uani 1 1 d . . . . .
H36 H 0.378645 0.314361 0.851988 0.037 Uiso 1 1 calc R . . . .
C37 C 0.28533(11) 0.19841(19) 0.86292(8) 0.0344(4) Uani 1 1 d . . . . .
H37 H 0.301062 0.203426 0.906624 0.041 Uiso 1 1 calc R . . . .
C38 C 0.21603(10) 0.12597(18) 0.83119(7) 0.0310(4) Uani 1 1 d . . . . .
H38 H 0.184536 0.080152 0.853297 0.037 Uiso 1 1 calc R . . . .
C39 C 0.19237(9) 0.12001(16) 0.76730(7) 0.0251(3) Uani 1 1 d . . . . .
H39 H 0.144217 0.071641 0.745998 0.030 Uiso 1 1 calc R . . . .
C40 C 0.28044(8) 0.13727(16) 0.63867(7) 0.0215(3) Uani 1 1 d . . . . .
C41 C 0.29811(9) 0.22502(18) 0.59464(7) 0.0269(3) Uani 1 1 d . . . . .
H41 H 0.267770 0.310230 0.580862 0.032 Uiso 1 1 calc R . . . .
C42 C 0.35988(9) 0.1884(2) 0.57081(8) 0.0349(4) Uani 1 1 d . . . . .
H42 H 0.371668 0.248942 0.540901 0.042 Uiso 1 1 calc R . . . .
C43 C 0.40434(10) 0.0644(2) 0.59040(8) 0.0391(4) Uani 1 1 d . . . . .
H43 H 0.446211 0.039241 0.573724 0.047 Uiso 1 1 calc R . . . .
C44 C 0.38758(10) -0.0226(2) 0.63428(8) 0.0353(4) Uani 1 1 d . . . . .
H44 H 0.418036 -0.107857 0.647812 0.042 Uiso 1 1 calc R . . . .
C45 C 0.32642(9) 0.01384(18) 0.65871(7) 0.0270(3) Uani 1 1 d . . . . .
H45 H 0.315825 -0.045864 0.689358 0.032 Uiso 1 1 calc R . . . .
C81 C 0.5708(8) 0.3065(10) 0.4633(6) 0.148(5) Uani 0.5 1 d D U P A -1
H81A H 0.589601 0.289526 0.427374 0.222 Uiso 0.5 1 calc R . P A -1
H81B H 0.616818 0.311056 0.500530 0.222 Uiso 0.5 1 calc R . P A -1
H81C H 0.535451 0.227376 0.467141 0.222 Uiso 0.5 1 calc R . P A -1
C82 C 0.5265(6) 0.4447(9) 0.4555(4) 0.129(3) Uani 0.5 1 d D U P A -1
H82A H 0.479535 0.442105 0.418216 0.154 Uiso 0.5 1 calc R . P A -1
H82B H 0.561410 0.526308 0.451813 0.154 Uiso 0.5 1 calc R . P A -1
C83 C 0.5003(5) 0.4600(8) 0.5138(5) 0.159(5) Uani 0.5 1 d D U P A -1
H83A H 0.545269 0.447749 0.551995 0.191 Uiso 0.5 1 calc R . P A -1
H83B H 0.456159 0.393319 0.513970 0.191 Uiso 0.5 1 calc R . P A -1
C84 C 0.4722(4) 0.6196(6) 0.5025(2) 0.094(3) Uani 0.5 1 d D U P A -1
H84A H 0.517735 0.686429 0.518917 0.113 Uiso 0.5 1 calc R . P A -1
H84B H 0.448400 0.638420 0.457942 0.113 Uiso 0.5 1 calc R . P A -1
C85 C 0.4111(7) 0.6394(9) 0.5358(4) 0.231(11) Uani 0.5 1 d D . P A -1
H85A H 0.391080 0.738955 0.530334 0.346 Uiso 0.5 1 calc R . P A -1
H85B H 0.366616 0.572238 0.519180 0.346 Uiso 0.5 1 calc R . P A -1
H85C H 0.435572 0.619985 0.579822 0.346 Uiso 0.5 1 calc R . 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
N1 C1 1.3426(18) . ?
N1 C5 1.3438(18) . ?
C1 C2 1.393(2) . ?
C1 C6 1.4990(19) . ?
C2 H2 0.9500 . ?
C2 C3 1.382(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.384(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.390(2) . ?
C5 C26 1.4974(19) . ?
C6 C7 1.352(2) . ?
C6 C8 1.491(2) . ?
C7 C14 1.491(2) . ?
C7 C20 1.496(2) . ?
C8 C9 1.398(2) . ?
C8 C13 1.392(2) . ?
C9 H9 0.9500 . ?
C9 C10 1.387(2) . ?
C10 H10 0.9500 . ?
C10 C11 1.385(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.384(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.382(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.392(3) . ?
C14 C19 1.398(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.396(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.375(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.377(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.387(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.394(2) . ?
C20 C25 1.390(2) . ?
C21 H21 0.9500 . ?
C21 C22 1.389(2) . ?
C22 H22 0.9500 . ?
C22 C23 1.381(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.383(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.387(2) . ?
C25 H25 0.9500 . ?
C26 C27 1.350(2) . ?
C26 C28 1.488(2) . ?
C27 C34 1.492(2) . ?
C27 C40 1.4935(19) . ?
C28 C29 1.395(2) . ?
C28 C33 1.396(2) . ?
C29 H29 0.9500 . ?
C29 C30 1.387(2) . ?
C30 H30 0.9500 . ?
C30 C31 1.382(3) . ?
C31 H31 0.9500 . ?
C31 C32 1.383(3) . ?
C32 H32 0.9500 . ?
C32 C33 1.390(2) . ?
C33 H33 0.9500 . ?
C34 C35 1.398(2) . ?
C34 C39 1.399(2) . ?
C35 H35 0.9500 . ?
C35 C36 1.388(2) . ?
C36 H36 0.9500 . ?
C36 C37 1.385(3) . ?
C37 H37 0.9500 . ?
C37 C38 1.386(3) . ?
C38 H38 0.9500 . ?
C38 C39 1.388(2) . ?
C39 H39 0.9500 . ?
C40 C41 1.394(2) . ?
C40 C45 1.393(2) . ?
C41 H41 0.9500 . ?
C41 C42 1.389(2) . ?
C42 H42 0.9500 . ?
C42 C43 1.384(3) . ?
C43 H43 0.9500 . ?
C43 C44 1.380(3) . ?
C44 H44 0.9500 . ?
C44 C45 1.388(2) . ?
C45 H45 0.9500 . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
C81 C82 1.478(8) . ?
C82 H82A 0.9900 . ?
C82 H82B 0.9900 . ?
C82 C83 1.534(8) . ?
C83 H83A 0.9900 . ?
C83 H83B 0.9900 . ?
C83 C84 1.553(8) . ?
C84 H84A 0.9900 . ?
C84 H84B 0.9900 . ?
C84 C85 1.496(9) . ?
C85 H85A 0.9800 . ?
C85 H85B 0.9800 . ?
C85 H85C 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
C1 N1 C5 117.61(12) . . ?
N1 C1 C2 122.60(13) . . ?
N1 C1 C6 114.77(12) . . ?
C2 C1 C6 122.62(12) . . ?
C1 C2 H2 120.4 . . ?
C3 C2 C1 119.11(13) . . ?
C3 C2 H2 120.4 . . ?
C2 C3 H3 120.5 . . ?
C2 C3 C4 118.91(14) . . ?
C4 C3 H3 120.5 . . ?
C3 C4 H4 120.7 . . ?
C3 C4 C5 118.54(13) . . ?
C5 C4 H4 120.7 . . ?
N1 C5 C4 123.24(13) . . ?
N1 C5 C26 116.91(12) . . ?
C4 C5 C26 119.76(12) . . ?
C7 C6 C1 122.41(13) . . ?
C7 C6 C8 123.58(13) . . ?
C8 C6 C1 114.01(12) . . ?
C6 C7 C14 122.41(13) . . ?
C6 C7 C20 122.05(13) . . ?
C14 C7 C20 115.54(12) . . ?
C9 C8 C6 119.17(13) . . ?
C13 C8 C6 122.69(13) . . ?
C13 C8 C9 118.13(14) . . ?
C8 C9 H9 119.6 . . ?
C10 C9 C8 120.73(15) . . ?
C10 C9 H9 119.6 . . ?
C9 C10 H10 119.9 . . ?
C11 C10 C9 120.22(16) . . ?
C11 C10 H10 119.9 . . ?
C10 C11 H11 120.3 . . ?
C12 C11 C10 119.49(16) . . ?
C12 C11 H11 120.3 . . ?
C11 C12 H12 119.8 . . ?
C13 C12 C11 120.32(16) . . ?
C13 C12 H12 119.8 . . ?
C8 C13 H13 119.5 . . ?
C12 C13 C8 121.01(15) . . ?
C12 C13 H13 119.5 . . ?
C15 C14 C7 122.31(16) . . ?
C15 C14 C19 118.77(17) . . ?
C19 C14 C7 118.89(15) . . ?
C14 C15 H15 120.1 . . ?
C14 C15 C16 119.9(2) . . ?
C16 C15 H15 120.1 . . ?
C15 C16 H16 119.7 . . ?
C17 C16 C15 120.6(2) . . ?
C17 C16 H16 119.7 . . ?
C16 C17 H17 120.0 . . ?
C16 C17 C18 119.9(2) . . ?
C18 C17 H17 120.0 . . ?
C17 C18 H18 119.9 . . ?
C17 C18 C19 120.2(2) . . ?
C19 C18 H18 119.9 . . ?
C14 C19 H19 119.8 . . ?
C18 C19 C14 120.5(2) . . ?
C18 C19 H19 119.8 . . ?
C21 C20 C7 119.36(14) . . ?
C25 C20 C7 121.86(14) . . ?
C25 C20 C21 118.73(14) . . ?
C20 C21 H21 119.8 . . ?
C22 C21 C20 120.41(16) . . ?
C22 C21 H21 119.8 . . ?
C21 C22 H22 119.8 . . ?
C23 C22 C21 120.35(17) . . ?
C23 C22 H22 119.8 . . ?
C22 C23 H23 120.2 . . ?
C22 C23 C24 119.61(15) . . ?
C24 C23 H23 120.2 . . ?
C23 C24 H24 119.8 . . ?
C23 C24 C25 120.30(16) . . ?
C25 C24 H24 119.8 . . ?
C20 C25 H25 119.7 . . ?
C24 C25 C20 120.54(16) . . ?
C24 C25 H25 119.7 . . ?
C27 C26 C5 120.41(13) . . ?
C27 C26 C28 125.94(13) . . ?
C28 C26 C5 113.61(12) . . ?
C26 C27 C34 121.91(13) . . ?
C26 C27 C40 122.73(13) . . ?
C34 C27 C40 115.36(12) . . ?
C29 C28 C26 121.65(14) . . ?
C29 C28 C33 118.34(14) . . ?
C33 C28 C26 119.89(13) . . ?
C28 C29 H29 119.7 . . ?
C30 C29 C28 120.54(15) . . ?
C30 C29 H29 119.7 . . ?
C29 C30 H30 119.7 . . ?
C31 C30 C29 120.56(16) . . ?
C31 C30 H30 119.7 . . ?
C30 C31 H31 120.2 . . ?
C30 C31 C32 119.62(15) . . ?
C32 C31 H31 120.2 . . ?
C31 C32 H32 120.0 . . ?
C31 C32 C33 120.10(16) . . ?
C33 C32 H32 120.0 . . ?
C28 C33 H33 119.6 . . ?
C32 C33 C28 120.82(15) . . ?
C32 C33 H33 119.6 . . ?
C35 C34 C27 120.41(13) . . ?
C35 C34 C39 118.25(14) . . ?
C39 C34 C27 121.32(13) . . ?
C34 C35 H35 119.6 . . ?
C36 C35 C34 120.72(15) . . ?
C36 C35 H35 119.6 . . ?
C35 C36 H36 119.8 . . ?
C37 C36 C35 120.39(15) . . ?
C37 C36 H36 119.8 . . ?
C36 C37 H37 120.2 . . ?
C36 C37 C38 119.53(15) . . ?
C38 C37 H37 120.2 . . ?
C37 C38 H38 119.8 . . ?
C37 C38 C39 120.36(15) . . ?
C39 C38 H38 119.8 . . ?
C34 C39 H39 119.6 . . ?
C38 C39 C34 120.70(15) . . ?
C38 C39 H39 119.6 . . ?
C41 C40 C27 120.87(13) . . ?
C45 C40 C27 120.33(13) . . ?
C45 C40 C41 118.78(14) . . ?
C40 C41 H41 119.8 . . ?
C42 C41 C40 120.30(15) . . ?
C42 C41 H41 119.8 . . ?
C41 C42 H42 119.8 . . ?
C43 C42 C41 120.37(16) . . ?
C43 C42 H42 119.8 . . ?
C42 C43 H43 120.1 . . ?
C44 C43 C42 119.72(15) . . ?
C44 C43 H43 120.1 . . ?
C43 C44 H44 119.9 . . ?
C43 C44 C45 120.26(16) . . ?
C45 C44 H44 119.9 . . ?
C40 C45 H45 119.7 . . ?
C44 C45 C40 120.56(15) . . ?
C44 C45 H45 119.7 . . ?
H81A C81 H81B 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
C82 C81 H81A 109.5 . . ?
C82 C81 H81B 109.5 . . ?
C82 C81 H81C 109.5 . . ?
C81 C82 H82A 110.8 . . ?
C81 C82 H82B 110.8 . . ?
C81 C82 C83 104.9(8) . . ?
H82A C82 H82B 108.8 . . ?
C83 C82 H82A 110.8 . . ?
C83 C82 H82B 110.8 . . ?
C82 C83 H83A 112.5 . . ?
C82 C83 H83B 112.5 . . ?
C82 C83 C84 96.2(7) . . ?
H83A C83 H83B 110.0 . . ?
C84 C83 H83A 112.5 . . ?
C84 C83 H83B 112.5 . . ?
C83 C84 H84A 110.6 . . ?
C83 C84 H84B 110.6 . . ?
H84A C84 H84B 108.7 . . ?
C85 C84 C83 105.8(5) . . ?
C85 C84 H84A 110.6 . . ?
C85 C84 H84B 110.6 . . ?
C84 C85 H85A 109.5 . . ?
C84 C85 H85B 109.5 . . ?
C84 C85 H85C 109.5 . . ?
H85A C85 H85B 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 0.2(2) . . . . ?
N1 C1 C6 C7 -124.46(15) . . . . ?
N1 C1 C6 C8 56.24(16) . . . . ?
N1 C5 C26 C27 -117.44(15) . . . . ?
N1 C5 C26 C28 64.67(16) . . . . ?
C1 N1 C5 C4 -0.6(2) . . . . ?
C1 N1 C5 C26 -177.07(12) . . . . ?
C1 C2 C3 C4 -0.6(2) . . . . ?
C1 C6 C7 C14 1.1(2) . . . . ?
C1 C6 C7 C20 -178.10(13) . . . . ?
C1 C6 C8 C9 45.11(18) . . . . ?
C1 C6 C8 C13 -135.69(14) . . . . ?
C2 C1 C6 C7 56.7(2) . . . . ?
C2 C1 C6 C8 -122.61(15) . . . . ?
C2 C3 C4 C5 0.5(2) . . . . ?
C3 C4 C5 N1 0.1(2) . . . . ?
C3 C4 C5 C26 176.53(13) . . . . ?
C4 C5 C26 C27 65.92(19) . . . . ?
C4 C5 C26 C28 -111.97(15) . . . . ?
C5 N1 C1 C2 0.4(2) . . . . ?
C5 N1 C1 C6 -178.45(12) . . . . ?
C5 C26 C27 C34 11.0(2) . . . . ?
C5 C26 C27 C40 -168.15(13) . . . . ?
C5 C26 C28 C29 -141.30(14) . . . . ?
C5 C26 C28 C33 34.85(18) . . . . ?
C6 C1 C2 C3 178.95(14) . . . . ?
C6 C7 C14 C15 49.5(2) . . . . ?
C6 C7 C14 C19 -128.60(16) . . . . ?
C6 C7 C20 C21 -124.66(16) . . . . ?
C6 C7 C20 C25 52.7(2) . . . . ?
C6 C8 C9 C10 176.49(15) . . . . ?
C6 C8 C13 C12 -175.98(14) . . . . ?
C7 C6 C8 C9 -134.18(16) . . . . ?
C7 C6 C8 C13 45.0(2) . . . . ?
C7 C14 C15 C16 -174.95(16) . . . . ?
C7 C14 C19 C18 174.05(16) . . . . ?
C7 C20 C21 C22 175.13(15) . . . . ?
C7 C20 C25 C24 -174.30(14) . . . . ?
C8 C6 C7 C14 -179.70(14) . . . . ?
C8 C6 C7 C20 1.1(2) . . . . ?
C8 C9 C10 C11 0.3(3) . . . . ?
C9 C8 C13 C12 3.2(2) . . . . ?
C9 C10 C11 C12 1.7(3) . . . . ?
C10 C11 C12 C13 -1.2(3) . . . . ?
C11 C12 C13 C8 -1.3(2) . . . . ?
C13 C8 C9 C10 -2.7(2) . . . . ?
C14 C7 C20 C21 56.13(19) . . . . ?
C14 C7 C20 C25 -126.55(16) . . . . ?
C14 C15 C16 C17 0.0(3) . . . . ?
C15 C14 C19 C18 -4.1(3) . . . . ?
C15 C16 C17 C18 -2.4(3) . . . . ?
C16 C17 C18 C19 1.4(3) . . . . ?
C17 C18 C19 C14 1.9(3) . . . . ?
C19 C14 C15 C16 3.2(3) . . . . ?
C20 C7 C14 C15 -131.26(16) . . . . ?
C20 C7 C14 C19 50.61(19) . . . . ?
C20 C21 C22 C23 0.4(3) . . . . ?
C21 C20 C25 C24 3.0(2) . . . . ?
C21 C22 C23 C24 0.7(3) . . . . ?
C22 C23 C24 C25 0.1(3) . . . . ?
C23 C24 C25 C20 -2.0(2) . . . . ?
C25 C20 C21 C22 -2.3(2) . . . . ?
C26 C27 C34 C35 -134.52(15) . . . . ?
C26 C27 C34 C39 46.9(2) . . . . ?
C26 C27 C40 C41 53.8(2) . . . . ?
C26 C27 C40 C45 -127.88(16) . . . . ?
C26 C28 C29 C30 176.68(14) . . . . ?
C26 C28 C33 C32 -177.62(14) . . . . ?
C27 C26 C28 C29 40.9(2) . . . . ?
C27 C26 C28 C33 -142.91(15) . . . . ?
C27 C34 C35 C36 179.55(13) . . . . ?
C27 C34 C39 C38 178.72(14) . . . . ?
C27 C40 C41 C42 179.15(14) . . . . ?
C27 C40 C45 C44 -179.74(14) . . . . ?
C28 C26 C27 C34 -171.35(13) . . . . ?
C28 C26 C27 C40 9.5(2) . . . . ?
C28 C29 C30 C31 0.3(2) . . . . ?
C29 C28 C33 C32 -1.3(2) . . . . ?
C29 C30 C31 C32 -0.2(3) . . . . ?
C30 C31 C32 C33 -0.7(3) . . . . ?
C31 C32 C33 C28 1.5(2) . . . . ?
C33 C28 C29 C30 0.5(2) . . . . ?
C34 C27 C40 C41 -125.45(15) . . . . ?
C34 C27 C40 C45 52.89(18) . . . . ?
C34 C35 C36 C37 2.3(2) . . . . ?
C35 C34 C39 C38 0.1(2) . . . . ?
C35 C36 C37 C38 -0.9(2) . . . . ?
C36 C37 C38 C39 -0.8(2) . . . . ?
C37 C38 C39 C34 1.2(2) . . . . ?
C39 C34 C35 C36 -1.8(2) . . . . ?
C40 C27 C34 C35 44.72(18) . . . . ?
C40 C27 C34 C39 -133.84(14) . . . . ?
C40 C41 C42 C43 0.2(2) . . . . ?
C41 C40 C45 C44 -1.4(2) . . . . ?
C41 C42 C43 C44 -0.6(3) . . . . ?
C42 C43 C44 C45 0.0(3) . . . . ?
C43 C44 C45 C40 1.0(3) . . . . ?
C45 C40 C41 C42 0.8(2) . . . . ?
C81 C82 C83 C84 169.1(7) . . . . ?
C82 C83 C84 C85 154.6(7) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_cell_oxdiff_length_a            17.5162(3)
_cell_oxdiff_length_b            9.25115(10)
_cell_oxdiff_length_c            22.7404(4)
_cell_oxdiff_angle_alpha         90.0065(11)
_cell_oxdiff_angle_beta          107.3603(14)
_cell_oxdiff_angle_gamma         90.0097(11)
_cell_oxdiff_volume              3517.12(9)
_cell_oxdiff_measurement_reflns_used 56452
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_ambient_environment      'perfluoro polyether oil / N~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_ga_tro55
_database_code_depnum_ccdc_archive 'CCDC 1817687'
_audit_update_record             
;
2018-01-17 deposited with the CCDC.
2018-02-05 downloaded from the CCDC.
;
_audit_creation_date             
;
'Thu Jan 23 17:11:22 2014'
;

_audit_block_code                ga_tro55
_audit_block_refno               1947
_audit_block_usercomment         'tr1186, needle, colourless'


_audit_creation_method           
;
Olex2 1.2
(compiled Aug 10 2017 17:44:14 for OlexSys, GUI svn.r5381)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C24 H15 F3 N2'
_chemical_formula_sum            'C24 H15 F3 N2'
_chemical_formula_weight         388.38
_chemical_melting_point          ?
_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_diffrn_ambient_temperature      110(1)
_chemical_oxdiff_formula         'C24 H15 F3 N2'
_chemical_oxdiff_usercomment     'tr1186, needle, colourless'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'
_chemical_absolute_configuration .
loop_
_symmetry_equiv_pos_as_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                   9.06788(17)
_cell_length_b                   5.50360(16)
_cell_length_c                   37.4304(11)
_cell_angle_alpha                90
_cell_angle_beta                 96.012(2)
_cell_angle_gamma                90
_cell_volume                     1857.73(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    16733
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      70.3550
_cell_measurement_theta_min      4.7350
_shelx_estimated_absorpt_T_max   0.919
_shelx_estimated_absorpt_T_min   0.919
_exptl_absorpt_coefficient_mu    0.863
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_correction_T_min  0.833
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
 a multifaceted crystal model (Busing & Levy, 1957).
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.043
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1176
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            53581
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.874
_diffrn_reflns_theta_min         4.752
_diffrn_detector_area_resol_mean 7.9621
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.1659480000
_diffrn_orient_matrix_UB_12      -0.0049345000
_diffrn_orient_matrix_UB_13      -0.0055029000
_diffrn_orient_matrix_UB_21      -0.0135777000
_diffrn_orient_matrix_UB_22      -0.2698338000
_diffrn_orient_matrix_UB_23      -0.0107817000
_diffrn_orient_matrix_UB_31      -0.0381943000
_diffrn_orient_matrix_UB_32      0.0741857000
_diffrn_orient_matrix_UB_33      -0.0395844000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_source                   'microfocus 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                3027
_reflns_number_total             3543
_reflns_odcompleteness_completeness 99.95
_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, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-17); encifer 1.5.2 (CCDC, 2016)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_shelxl_version_number           2018/1
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         3543
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0398
_refine_ls_restrained_S_all      1.064
_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)+(0.0522P)²+0.6680P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1090
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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
F1 F -0.27046(9) 1.31876(19) 0.30484(3) 0.0376(3) Uani 1 1 d . . . . .
F2 F 0.85842(9) 0.48417(18) 0.44962(3) 0.0328(2) Uani 1 1 d . . . . .
F3 F 0.47308(11) 1.05937(19) 0.22628(2) 0.0358(3) Uani 1 1 d . . . . .
N1 N 0.33553(14) 1.1365(3) 0.44663(4) 0.0280(3) Uani 1 1 d . . . . .
N2 N 0.14492(13) 0.8395(3) 0.43603(3) 0.0277(3) Uani 1 1 d . . . . .
C1 C 0.25258(15) 1.0116(3) 0.38560(4) 0.0208(3) Uani 1 1 d . . . . .
C2 C 0.37912(14) 0.9533(3) 0.37122(4) 0.0200(3) Uani 1 1 d . . . . .
C3 C 0.24512(14) 0.9943(3) 0.42512(4) 0.0209(3) Uani 1 1 d . . . . .
C4 C 0.32479(17) 1.1179(3) 0.48188(4) 0.0303(4) Uani 1 1 d . . . . .
H4 H 0.393(2) 1.227(4) 0.4976(5) 0.036 Uiso 1 1 d R . . . .
C5 C 0.22891(16) 0.9600(3) 0.49599(4) 0.0276(4) Uani 1 1 d . . . . .
H5 H 0.2222(19) 0.942(3) 0.5216(5) 0.033 Uiso 1 1 d R . . . .
C6 C 0.13981(16) 0.8231(3) 0.47149(4) 0.0305(4) Uani 1 1 d . . . . .
H6 H 0.070(2) 0.708(4) 0.4793(5) 0.037 Uiso 1 1 d R . . . .
C7 C 0.11199(14) 1.0902(3) 0.36453(4) 0.0204(3) Uani 1 1 d . . . . .
C8 C 0.03963(15) 1.3010(3) 0.37385(4) 0.0237(3) Uani 1 1 d . . . . .
H8 H 0.0793(19) 1.400(3) 0.3942(5) 0.028 Uiso 1 1 d R . . . .
C9 C -0.08952(15) 1.3780(3) 0.35382(4) 0.0261(3) Uani 1 1 d . . . . .
H9 H -0.138(2) 1.529(4) 0.3584(5) 0.031 Uiso 1 1 d R . . . .
C10 C -0.14538(14) 1.2405(3) 0.32491(4) 0.0254(3) Uani 1 1 d . . . . .
C11 C -0.08060(15) 1.0281(3) 0.31534(4) 0.0253(3) Uani 1 1 d . . . . .
H11 H -0.1237(19) 0.936(3) 0.2958(5) 0.030 Uiso 1 1 d R . . . .
C12 C 0.04951(14) 0.9539(3) 0.33529(4) 0.0215(3) Uani 1 1 d . . . . .
H12 H 0.0960(19) 0.803(3) 0.3296(5) 0.026 Uiso 1 1 d R . . . .
C13 C 0.50561(14) 0.8363(3) 0.39360(4) 0.0197(3) Uani 1 1 d . . . . .
C14 C 0.64990(15) 0.9281(3) 0.39380(4) 0.0212(3) Uani 1 1 d . . . . .
H14 H 0.6659(18) 1.081(3) 0.3806(5) 0.025 Uiso 1 1 d R . . . .
C15 C 0.76924(14) 0.8127(3) 0.41290(4) 0.0229(3) Uani 1 1 d . . . . .
H15 H 0.8692(19) 0.873(3) 0.4132(5) 0.027 Uiso 1 1 d R . . . .
C16 C 0.74201(14) 0.6031(3) 0.43124(4) 0.0230(3) Uani 1 1 d . . . . .
C17 C 0.60233(15) 0.5047(3) 0.43172(4) 0.0226(3) Uani 1 1 d . . . . .
H17 H 0.5875(19) 0.357(3) 0.4445(5) 0.027 Uiso 1 1 d R . . . .
C18 C 0.48404(14) 0.6239(3) 0.41253(4) 0.0218(3) Uani 1 1 d . . . . .
H18 H 0.3834(19) 0.558(3) 0.4118(5) 0.026 Uiso 1 1 d R . . . .
C19 C 0.40171(14) 0.9859(3) 0.33262(4) 0.0200(3) Uani 1 1 d . . . . .
C20 C 0.35004(14) 1.1901(3) 0.31287(4) 0.0220(3) Uani 1 1 d . . . . .
H20 H 0.3004(19) 1.317(3) 0.3240(5) 0.026 Uiso 1 1 d R . . . .
C21 C 0.37413(15) 1.2159(3) 0.27714(4) 0.0241(3) Uani 1 1 d . . . . .
H21 H 0.3405(19) 1.356(3) 0.2640(5) 0.029 Uiso 1 1 d R . . . .
C22 C 0.45056(15) 1.0356(3) 0.26134(4) 0.0241(3) Uani 1 1 d . . . . .
C23 C 0.50507(16) 0.8328(3) 0.27969(4) 0.0248(3) Uani 1 1 d . . . . .
H23 H 0.5588(19) 0.710(3) 0.2680(5) 0.030 Uiso 1 1 d R . . . .
C24 C 0.48050(15) 0.8096(3) 0.31556(4) 0.0221(3) Uani 1 1 d . . . . .
H24 H 0.5195(19) 0.666(3) 0.3287(5) 0.027 Uiso 1 1 d 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
F1 C10 1.3629(17) . ?
F2 C16 1.3653(17) . ?
F3 C22 1.3557(17) . ?
N1 C3 1.3400(19) . ?
N1 C4 1.337(2) . ?
N2 C3 1.3399(19) . ?
N2 C6 1.336(2) . ?
C1 C2 1.3559(19) . ?
C1 C3 1.491(2) . ?
C1 C7 1.4913(19) . ?
C2 C13 1.494(2) . ?
C2 C19 1.491(2) . ?
C4 H4 1.01(2) . ?
C4 C5 1.373(2) . ?
C5 H5 0.971(19) . ?
C5 C6 1.381(2) . ?
C6 H6 0.96(2) . ?
C7 C8 1.395(2) . ?
C7 C12 1.397(2) . ?
C8 H8 0.975(19) . ?
C8 C9 1.389(2) . ?
C9 H9 0.965(19) . ?
C9 C10 1.373(2) . ?
C10 C11 1.373(2) . ?
C11 H11 0.942(19) . ?
C11 C12 1.390(2) . ?
C12 H12 0.966(18) . ?
C13 C14 1.4020(19) . ?
C13 C18 1.391(2) . ?
C14 H14 0.992(18) . ?
C14 C15 1.387(2) . ?
C15 H15 0.964(18) . ?
C15 C16 1.378(2) . ?
C16 C17 1.380(2) . ?
C17 H17 0.960(19) . ?
C17 C18 1.391(2) . ?
C18 H18 0.979(17) . ?
C19 C20 1.399(2) . ?
C19 C24 1.398(2) . ?
C20 H20 0.951(18) . ?
C20 C21 1.384(2) . ?
C21 H21 0.951(19) . ?
C21 C22 1.379(2) . ?
C22 C23 1.375(2) . ?
C23 H23 0.964(19) . ?
C23 C24 1.390(2) . ?
C24 H24 0.975(19) . ?

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
C4 N1 C3 116.42(13) . . ?
C6 N2 C3 116.19(13) . . ?
C2 C1 C3 120.46(13) . . ?
C2 C1 C7 124.81(14) . . ?
C3 C1 C7 114.72(11) . . ?
C1 C2 C13 120.76(13) . . ?
C1 C2 C19 124.33(13) . . ?
C19 C2 C13 114.82(11) . . ?
N1 C3 C1 118.07(12) . . ?
N2 C3 N1 125.44(14) . . ?
N2 C3 C1 116.48(13) . . ?
N1 C4 H4 115.3(11) . . ?
N1 C4 C5 122.86(15) . . ?
C5 C4 H4 121.8(11) . . ?
C4 C5 H5 123.4(11) . . ?
C4 C5 C6 116.10(15) . . ?
C6 C5 H5 120.5(11) . . ?
N2 C6 C5 122.95(14) . . ?
N2 C6 H6 116.1(12) . . ?
C5 C6 H6 120.9(12) . . ?
C8 C7 C1 120.49(13) . . ?
C8 C7 C12 118.67(13) . . ?
C12 C7 C1 120.84(13) . . ?
C7 C8 H8 121.0(10) . . ?
C9 C8 C7 120.71(15) . . ?
C9 C8 H8 118.3(10) . . ?
C8 C9 H9 122.8(11) . . ?
C10 C9 C8 118.56(15) . . ?
C10 C9 H9 118.5(11) . . ?
F1 C10 C9 118.51(14) . . ?
F1 C10 C11 118.65(14) . . ?
C11 C10 C9 122.84(14) . . ?
C10 C11 H11 120.6(11) . . ?
C10 C11 C12 118.18(15) . . ?
C12 C11 H11 121.2(11) . . ?
C7 C12 H12 119.0(11) . . ?
C11 C12 C7 121.01(14) . . ?
C11 C12 H12 120.0(11) . . ?
C14 C13 C2 120.60(13) . . ?
C18 C13 C2 120.49(12) . . ?
C18 C13 C14 118.75(13) . . ?
C13 C14 H14 119.2(10) . . ?
C15 C14 C13 121.01(14) . . ?
C15 C14 H14 119.8(10) . . ?
C14 C15 H15 122.0(11) . . ?
C16 C15 C14 117.99(13) . . ?
C16 C15 H15 120.0(10) . . ?
F2 C16 C15 118.89(12) . . ?
F2 C16 C17 117.87(14) . . ?
C15 C16 C17 123.24(14) . . ?
C16 C17 H17 121.1(10) . . ?
C16 C17 C18 117.86(14) . . ?
C18 C17 H17 121.1(11) . . ?
C13 C18 H18 118.4(10) . . ?
C17 C18 C13 121.15(13) . . ?
C17 C18 H18 120.5(10) . . ?
C20 C19 C2 122.43(13) . . ?
C24 C19 C2 119.17(13) . . ?
C24 C19 C20 118.38(14) . . ?
C19 C20 H20 120.5(11) . . ?
C21 C20 C19 120.97(14) . . ?
C21 C20 H20 118.5(11) . . ?
C20 C21 H21 120.7(11) . . ?
C22 C21 C20 118.55(14) . . ?
C22 C21 H21 120.8(11) . . ?
F3 C22 C21 118.64(14) . . ?
F3 C22 C23 118.63(14) . . ?
C23 C22 C21 122.73(14) . . ?
C22 C23 H23 121.1(11) . . ?
C22 C23 C24 118.12(14) . . ?
C24 C23 H23 120.8(11) . . ?
C19 C24 H24 120.5(10) . . ?
C23 C24 C19 121.24(14) . . ?
C23 C24 H24 118.3(10) . . ?

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
F1 C10 C11 C12 177.99(13) . . . . ?
F2 C16 C17 C18 -179.02(13) . . . . ?
F3 C22 C23 C24 -179.61(12) . . . . ?
N1 C4 C5 C6 -1.6(2) . . . . ?
C1 C2 C13 C14 -130.49(15) . . . . ?
C1 C2 C13 C18 54.2(2) . . . . ?
C1 C2 C19 C20 40.1(2) . . . . ?
C1 C2 C19 C24 -141.52(15) . . . . ?
C1 C7 C8 C9 178.53(13) . . . . ?
C1 C7 C12 C11 -179.27(13) . . . . ?
C2 C1 C3 N1 62.5(2) . . . . ?
C2 C1 C3 N2 -118.98(16) . . . . ?
C2 C1 C7 C8 -129.08(16) . . . . ?
C2 C1 C7 C12 51.4(2) . . . . ?
C2 C13 C14 C15 -176.35(13) . . . . ?
C2 C13 C18 C17 176.05(13) . . . . ?
C2 C19 C20 C21 179.38(13) . . . . ?
C2 C19 C24 C23 -179.64(12) . . . . ?
C3 N1 C4 C5 1.0(2) . . . . ?
C3 N2 C6 C5 1.5(2) . . . . ?
C3 C1 C2 C13 9.2(2) . . . . ?
C3 C1 C2 C19 -174.25(13) . . . . ?
C3 C1 C7 C8 52.30(18) . . . . ?
C3 C1 C7 C12 -127.21(14) . . . . ?
C4 N1 C3 N2 0.9(2) . . . . ?
C4 N1 C3 C1 179.37(14) . . . . ?
C4 C5 C6 N2 0.2(2) . . . . ?
C6 N2 C3 N1 -2.2(2) . . . . ?
C6 N2 C3 C1 179.35(14) . . . . ?
C7 C1 C2 C13 -169.39(13) . . . . ?
C7 C1 C2 C19 7.2(2) . . . . ?
C7 C1 C3 N1 -118.86(15) . . . . ?
C7 C1 C3 N2 59.71(18) . . . . ?
C7 C8 C9 C10 0.8(2) . . . . ?
C8 C7 C12 C11 1.2(2) . . . . ?
C8 C9 C10 F1 -178.71(13) . . . . ?
C8 C9 C10 C11 1.2(2) . . . . ?
C9 C10 C11 C12 -1.9(2) . . . . ?
C10 C11 C12 C7 0.7(2) . . . . ?
C12 C7 C8 C9 -1.9(2) . . . . ?
C13 C2 C19 C20 -143.13(14) . . . . ?
C13 C2 C19 C24 35.25(18) . . . . ?
C13 C14 C15 C16 0.9(2) . . . . ?
C14 C13 C18 C17 0.7(2) . . . . ?
C14 C15 C16 F2 178.72(13) . . . . ?
C14 C15 C16 C17 -0.6(2) . . . . ?
C15 C16 C17 C18 0.3(2) . . . . ?
C16 C17 C18 C13 -0.3(2) . . . . ?
C18 C13 C14 C15 -1.0(2) . . . . ?
C19 C2 C13 C14 52.60(18) . . . . ?
C19 C2 C13 C18 -122.70(14) . . . . ?
C19 C20 C21 C22 -0.1(2) . . . . ?
C20 C19 C24 C23 -1.2(2) . . . . ?
C20 C21 C22 F3 179.41(12) . . . . ?
C20 C21 C22 C23 -0.7(2) . . . . ?
C21 C22 C23 C24 0.5(2) . . . . ?
C22 C23 C24 C19 0.5(2) . . . . ?
C24 C19 C20 C21 1.0(2) . . . . ?
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_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 2 -21 0.0488 -0.4883 1.9981 -20.5179 0.0220 -0.3113 0.9791
-6 0 5 0.0122 -6.0056 0.4982 4.9802 -1.0265 -0.1066 0.0692
6 0 -5 0.0311 6.0056 -0.4982 -4.9802 1.0265 0.1066 -0.0692
2 3 13 0.1314 1.5033 2.7518 12.5229 0.1670 -0.8980 -0.3490
-2 -3 -13 0.1314 -1.5033 -2.7518 -12.5229 -0.1670 0.8980 0.3490
0 -2 21 0.0488 0.4883 -1.9981 20.5179 -0.0220 0.3113 -0.9791

_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            9.0687(2)
_cell_oxdiff_length_b            5.50418(15)
_cell_oxdiff_length_c            37.4255(9)
_cell_oxdiff_angle_alpha         89.998(2)
_cell_oxdiff_angle_beta          96.049(2)
_cell_oxdiff_angle_gamma         90.014(2)
_cell_oxdiff_volume              1857.73(8)
_cell_oxdiff_measurement_reflns_used 16733
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   43.00   68.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 25

#__ type_ start__ end____ width___ exp.time_
  2 omega   11.00   65.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -90.0000 54

#__ type_ start__ end____ width___ exp.time_
  3 omega  -21.00   33.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 54

#__ type_ start__ end____ width___ exp.time_
  4 omega  -25.00    4.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -90.0000 29

#__ type_ start__ end____ width___ exp.time_
  5 omega   15.00   43.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -19.0000  -60.0000 28

#__ type_ start__ end____ width___ exp.time_
  6 omega  -38.00  -10.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -19.0000  -60.0000 28

#__ type_ start__ end____ width___ exp.time_
  7 omega  -70.00    8.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -19.0000   90.0000 78

#__ type_ start__ end____ width___ exp.time_
  8 omega  -18.00    9.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0000   78.0000  -36.7725 27

#__ type_ start__ end____ width___ exp.time_
  9 omega   33.00   84.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       14.0000   74.0000   45.8711 51

#__ type_ start__ end____ width___ exp.time_
 10 omega  -14.00   30.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       14.0000   74.0000   45.8711 44

#__ type_ start__ end____ width___ exp.time_
 11 omega    6.00   35.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   80.0000   -4.7506 29

#__ type_ start__ end____ width___ exp.time_
 12 omega    6.00   31.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   80.0000 -143.4453 25

#__ type_ start__ end____ width___ exp.time_
 13 omega   10.00   35.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  -96.7895 25

#__ type_ start__ end____ width___ exp.time_
 14 omega   10.00   35.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000   69.3420 25

#__ type_ start__ end____ width___ exp.time_
 15 omega   15.00   40.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000  107.8577 25

#__ type_ start__ end____ width___ exp.time_
 16 omega   14.00   39.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000 -158.1460 25

#__ type_ start__ end____ width___ exp.time_
 17 omega   15.00   40.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000  155.1236 25

#__ type_ start__ end____ width___ exp.time_
 18 omega   15.00   40.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000   18.9777 25

#__ type_ start__ end____ width___ exp.time_
 19 omega   20.00   46.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000  -17.9530 26

#__ type_ start__ end____ width___ exp.time_
 20 omega   93.00  120.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000   18.9330 27

#__ type_ start__ end____ width___ exp.time_
 21 omega   20.00   46.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  151.7550 26

#__ type_ start__ end____ width___ exp.time_
 22 omega   21.00   47.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000   18.9330 26

#__ type_ start__ end____ width___ exp.time_
 23 omega   19.00   44.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000 -121.7016 25

#__ type_ start__ end____ width___ exp.time_
 24 omega   19.00   44.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  -57.0658 25

#__ type_ start__ end____ width___ exp.time_
 25 omega   19.00   44.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  -89.5757 25

#__ type_ start__ end____ width___ exp.time_
 26 omega   23.00   48.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  179.9186 25

#__ type_ start__ end____ width___ exp.time_
 27 omega   24.00   50.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  120.0000 26

#__ type_ start__ end____ width___ exp.time_
 28 omega   89.00  124.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -150.0000 35

#__ type_ start__ end____ width___ exp.time_
 29 omega   29.00   55.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
 30 omega   23.00   48.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   80.3497 25

#__ type_ start__ end____ width___ exp.time_
 31 omega  -16.00   84.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000  -90.0000 100

#__ type_ start__ end____ width___ exp.time_
 32 omega   23.00   48.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   52.5445 25

#__ type_ start__ end____ width___ exp.time_
 33 omega   24.00   50.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
 34 omega   25.00   51.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -90.0000 26

#__ type_ start__ end____ width___ exp.time_
 35 omega   25.00   50.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -30.0000 25

#__ type_ start__ end____ width___ exp.time_
 36 omega   23.00   48.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   20.5820 25

#__ type_ start__ end____ width___ exp.time_
 37 omega   29.00   55.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
 38 omega   33.00   59.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   71.0000   60.6661 26

#__ type_ start__ end____ width___ exp.time_
 39 omega   28.00   53.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -23.8749 25

#__ type_ start__ end____ width___ exp.time_
 40 omega   29.00   55.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   23.4717 26

#__ type_ start__ end____ width___ exp.time_
 41 omega   28.00   57.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  146.0684 29

#__ type_ start__ end____ width___ exp.time_
 42 omega   36.00   61.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   68.0000  112.1175 25

#__ type_ start__ end____ width___ exp.time_
 43 omega   31.00   57.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   74.0000  -74.7545 26

#__ type_ start__ end____ width___ exp.time_
 44 omega   35.00   61.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   71.0000 -125.2225 26

#__ type_ start__ end____ width___ exp.time_
 45 omega   40.00   66.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   68.0000   49.3742 26

#__ type_ start__ end____ width___ exp.time_
 46 omega   33.00   59.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000  126.4113 26

#__ type_ start__ end____ width___ exp.time_
 47 omega   -9.00   94.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -80.0000  104.0746 103

#__ type_ start__ end____ width___ exp.time_
 48 omega  109.00  134.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   68.0000   80.4749 25

#__ type_ start__ end____ width___ exp.time_
 49 omega   43.00   93.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   68.0000   80.4749 50

#__ type_ start__ end____ width___ exp.time_
 50 omega  105.00  131.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   68.0000 -141.4815 26

#__ type_ start__ end____ width___ exp.time_
 51 omega   48.00   74.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   68.0000 -141.4815 26

#__ type_ start__ end____ width___ exp.time_
 52 omega   37.00   63.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   76.0000 -177.1426 26

#__ type_ start__ end____ width___ exp.time_
 53 omega   52.00   78.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000 -153.7299 26

#__ type_ start__ end____ width___ exp.time_
 54 omega   37.00   83.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   75.0000   47.1184 46

#__ type_ start__ end____ width___ exp.time_
 55 omega  110.00  136.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   74.0000 -166.5222 26

#__ type_ start__ end____ width___ exp.time_
 56 omega   38.00   64.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   74.0000 -166.5222 26

#__ type_ start__ end____ width___ exp.time_
 57 omega   70.00   95.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000  132.3742 25

#__ type_ start__ end____ width___ exp.time_
 58 omega   50.00   76.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   67.0000 -151.2040 26

#__ type_ start__ end____ width___ exp.time_
 59 omega   51.00  119.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   67.0000  -44.3505 68

#__ type_ start__ end____ width___ exp.time_
 60 omega   41.00   71.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000 -113.5183 30

#__ type_ start__ end____ width___ exp.time_
 61 omega   42.00   68.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   76.0000  106.9193 26

#__ type_ start__ end____ width___ exp.time_
 62 omega   49.00   85.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   60.0000   29.7574 36

#__ type_ start__ end____ width___ exp.time_
 63 omega   44.00   93.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   73.0000  127.2491 49

#__ type_ start__ end____ width___ exp.time_
 64 omega   42.00   68.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   73.0000  101.0961 26

#__ type_ start__ end____ width___ exp.time_
 65 omega   41.00   81.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000  -69.6152 40

#__ type_ start__ end____ width___ exp.time_
 66 omega   41.00   90.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   76.0000  -14.5020 49

#__ type_ start__ end____ width___ exp.time_
 67 omega   50.00  106.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   59.0000 -177.9111 56

#__ type_ start__ end____ width___ exp.time_
 68 omega   46.00   72.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   72.0000  -93.2224 26

#__ type_ start__ end____ width___ exp.time_
 69 omega   47.00   72.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   71.0000 -171.2837 25

#__ type_ start__ end____ width___ exp.time_
 70 omega   51.00   77.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   64.0000 -105.8325 26

#__ type_ start__ end____ width___ exp.time_
 71 omega   50.00   89.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   68.0000   86.0036 39

#__ type_ start__ end____ width___ exp.time_
 72 omega   57.00   83.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   74.0000  -23.1273 26

#__ type_ start__ end____ width___ exp.time_
 73 omega   52.00   90.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   62.0000  -72.5554 38

#__ type_ start__ end____ width___ exp.time_
 74 omega   49.00   76.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   75.0000   30.7817 27

#__ type_ start__ end____ width___ exp.time_
 75 omega   84.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   70.0000   48.7141 25

#__ type_ start__ end____ width___ exp.time_
 76 omega   52.00   78.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   70.0000   48.7141 26

#__ type_ start__ end____ width___ exp.time_
 77 omega   57.00  103.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   53.0000  -85.0892 46

#__ type_ start__ end____ width___ exp.time_
 78 omega   49.00  147.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   76.0000  176.9435 98

#__ type_ start__ end____ width___ exp.time_
 79 omega   51.00   81.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   72.0000   94.2292 30

#__ type_ start__ end____ width___ exp.time_
 80 omega   49.00   75.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   75.0000  -31.2709 26

#__ type_ start__ end____ width___ exp.time_
 81 omega   63.00   89.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   72.0000   60.7497 26

#__ type_ start__ end____ width___ exp.time_
 82 omega   56.00   82.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   70.0000  -92.4924 26

#__ type_ start__ end____ width___ exp.time_
 83 omega   62.00  149.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   63.0000  -10.1707 87

#__ type_ start__ end____ width___ exp.time_
 84 omega   54.00   80.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   74.0000  -77.7744 26

#__ type_ start__ end____ width___ exp.time_
 85 omega   57.00   86.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   75.0000  -75.3469 29

#__ type_ start__ end____ width___ exp.time_
 86 omega   58.00   83.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   73.0000   50.8238 25

#__ type_ start__ end____ width___ exp.time_
 87 omega   60.00   86.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   70.0000    6.2915 26

#__ type_ start__ end____ width___ exp.time_
 88 omega   63.00   95.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   68.0000  150.1476 32

#__ type_ start__ end____ width___ exp.time_
 89 omega   63.00   93.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   66.0000  -26.3335 30

#__ type_ start__ end____ width___ exp.time_
 90 omega   64.00   91.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   35.0000  130.0871 27

#__ type_ start__ end____ width___ exp.time_
 91 omega   60.00   86.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   70.0000   99.5368 26

#__ type_ start__ end____ width___ exp.time_
 92 omega   58.00  144.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   75.0000  116.1103 86

#__ type_ start__ end____ width___ exp.time_
 93 omega   64.00   90.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   45.0000  -98.2342 26

#__ type_ start__ end____ width___ exp.time_
 94 omega   18.00   87.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000  -80.0000  -27.3800 69

#__ type_ start__ end____ width___ exp.time_
 95 omega   61.00   87.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   76.0000   95.1330 26

#__ type_ start__ end____ width___ exp.time_
 96 omega   70.00   96.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   48.0000 -154.1602 26

#__ type_ start__ end____ width___ exp.time_
 97 omega   79.00  106.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   63.0000   59.1814 27

#__ type_ start__ end____ width___ exp.time_
 98 omega   66.00   97.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   73.0000  133.3236 31

#__ type_ start__ end____ width___ exp.time_
 99 omega   70.00   97.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   67.0000   21.9161 27

#__ type_ start__ end____ width___ exp.time_
100 omega   65.00  156.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   75.0000  -64.4721 91

#__ type_ start__ end____ width___ exp.time_
101 omega   71.00   97.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   65.0000 -172.4761 26

#__ type_ start__ end____ width___ exp.time_
102 omega   70.00   95.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   74.0000  -86.9515 25

#__ type_ start__ end____ width___ exp.time_
103 omega   71.00  103.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   71.0000  149.5549 32

#__ type_ start__ end____ width___ exp.time_
104 omega   81.00  108.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      102.0000   52.0000  -10.5839 27

#__ type_ start__ end____ width___ exp.time_
105 omega   74.00  114.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      102.0000   73.0000   29.7923 40

#__ type_ start__ end____ width___ exp.time_
106 omega   78.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 99

#__ type_ start__ end____ width___ exp.time_
107 omega  151.00  176.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 25

#__ type_ start__ end____ width___ exp.time_
108 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 26

#__ type_ start__ end____ width___ exp.time_
109 omega  110.00  166.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 56

#__ type_ start__ end____ width___ exp.time_
110 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 26

#__ type_ start__ end____ width___ exp.time_
111 omega  150.00  176.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 26

#__ type_ start__ end____ width___ exp.time_
112 omega   78.00  103.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 25

#__ type_ start__ end____ width___ exp.time_
113 omega   78.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 99

#__ type_ start__ end____ width___ exp.time_
114 omega  108.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 69

#__ type_ start__ end____ width___ exp.time_
115 omega   79.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
116 omega  130.00  175.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000    0.0000 45

#__ type_ start__ end____ width___ exp.time_
117 omega   86.00  127.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000    0.0000 41

#__ type_ start__ end____ width___ exp.time_
118 omega   78.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 99

#__ type_ start__ end____ width___ exp.time_
119 omega  135.00  166.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 31

#__ type_ start__ end____ width___ exp.time_
120 omega   78.00  115.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 37

#__ type_ start__ end____ width___ exp.time_
121 omega  126.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   90.0000 48

#__ type_ start__ end____ width___ exp.time_
122 omega   85.00  122.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   90.0000 37

#__ type_ start__ end____ width___ exp.time_
123 omega   83.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   72.0000 -100.2567 26

#__ type_ start__ end____ width___ exp.time_
124 omega   77.00  103.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  114.1098 26

#__ type_ start__ end____ width___ exp.time_
125 omega   78.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  167.3419 100

#__ type_ start__ end____ width___ exp.time_
126 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
127 omega   80.00  106.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   76.0000 -141.8702 26

#__ type_ start__ end____ width___ exp.time_
128 omega   83.00  139.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -27.5363 56

#__ type_ start__ end____ width___ exp.time_
129 omega   70.00  123.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   23.9275 53

#__ type_ start__ end____ width___ exp.time_
130 omega   78.00  103.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  103.1698 25

#__ type_ start__ end____ width___ exp.time_
131 omega   48.00  134.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  -90.7929 86

#__ type_ start__ end____ width___ exp.time_
132 omega   46.00  107.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  152.2262 61

#__ type_ start__ end____ width___ exp.time_
133 omega   70.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000   73.3462 34

#__ type_ start__ end____ width___ exp.time_
134 omega  132.00  176.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000 -157.2657 44

#__ type_ start__ end____ width___ exp.time_
135 omega   86.00  112.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000 -157.2657 26

#__ type_ start__ end____ width___ exp.time_
136 omega   85.00  162.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000 -120.0000 77

#__ type_ start__ end____ width___ exp.time_
137 omega   87.00  156.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  120.0000 69

#__ type_ start__ end____ width___ exp.time_
138 omega   85.00  111.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  150.0000 26

#__ type_ start__ end____ width___ exp.time_
139 omega   85.00  111.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
140 omega   86.00  115.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   60.0000 29

#__ type_ start__ end____ width___ exp.time_
141 omega   85.00  111.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
142 omega   85.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -120.0000 89

#__ type_ start__ end____ width___ exp.time_
143 omega   83.00  127.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000 -130.4789 44

#__ type_ start__ end____ width___ exp.time_
144 omega   78.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 99

#__ type_ start__ end____ width___ exp.time_
145 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 26

#__ type_ start__ end____ width___ exp.time_
146 omega   44.00   70.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000 -130.4789 26

#__ type_ start__ end____ width___ exp.time_
147 omega   79.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
148 omega  123.00  173.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 50

#__ type_ start__ end____ width___ exp.time_
149 omega   56.00  108.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000 -161.7266 52

#__ type_ start__ end____ width___ exp.time_
150 omega  -69.00   21.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000    0.0000 90

#__ type_ start__ end____ width___ exp.time_
151 omega  -72.00   26.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000   30.0000 98

#__ type_ start__ end____ width___ exp.time_
152 omega  -73.00   44.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -19.0000   30.0000 117

#__ type_ start__ end____ width___ exp.time_
153 omega  -19.00   80.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0000   76.0000  148.4008 99

#__ type_ start__ end____ width___ exp.time_
154 omega  -11.00   88.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0000   76.0000  -36.3579 99

#__ type_ start__ end____ width___ exp.time_
155 omega   -7.00   92.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0000   76.0000   76.1932 99

#__ type_ start__ end____ width___ exp.time_
156 omega   -8.00   92.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0000   77.0000    7.1442 100

#__ type_ start__ end____ width___ exp.time_
157 omega   -4.00   96.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   77.0000 -175.4551 100

#__ type_ start__ end____ width___ exp.time_
158 omega    2.00   97.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   44.0000  -70.1503 95

#__ type_ start__ end____ width___ exp.time_
159 omega  -18.00   80.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -38.0000   90.0000 98

#__ type_ start__ end____ width___ exp.time_
160 omega  -15.00   75.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  -30.0000 90

#__ type_ start__ end____ width___ exp.time_
161 omega    0.00  101.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -78.0000  -61.1795 101

#__ type_ start__ end____ width___ exp.time_
162 omega   55.00  138.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   66.0000  132.6372 83

#__ type_ start__ end____ width___ exp.time_
163 omega   57.00  148.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   53.0000  -85.0892 91

#__ type_ start__ end____ width___ exp.time_
164 omega   49.00  148.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   75.0000   30.7817 99

;
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Agilent EOS'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_ambient_environment      'perfluoro polyether oil / N~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_ga_ff20
_database_code_depnum_ccdc_archive 'CCDC 1817691'
_audit_update_record             
;
2018-01-17 deposited with the CCDC.
2018-02-05 downloaded from the CCDC.
;
_audit_creation_date             2017-10-25

_audit_block_code                ga_ff20
_audit_block_refno               2966
_audit_block_usercomment         'FF459, irregular, colourless'


_audit_creation_method           
;
Olex2 1.2
(compiled Aug 10 2017 17:44:14 for OlexSys, GUI svn.r5381)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C45 H27 F6 N'
_chemical_formula_sum            'C45 H27 F6 N'
_chemical_formula_weight         695.67
_chemical_melting_point          ?
_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_diffrn_ambient_temperature      120(1)
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'
_chemical_absolute_configuration .
loop_
_symmetry_equiv_pos_as_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                   16.1155(4)
_cell_length_b                   10.2929(3)
_cell_length_c                   20.6155(5)
_cell_angle_alpha                90
_cell_angle_beta                 90.803(2)
_cell_angle_gamma                90
_cell_volume                     3419.27(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10025
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      29.6050
_cell_measurement_theta_min      2.5380
_shelx_estimated_absorpt_T_max   0.990
_shelx_estimated_absorpt_T_min   0.990
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.804
_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 (Busing & Levy, 1957).
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1432
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 13 12 0.0460
-20 1 -14 0.0428
11 0 26 0.0540
-11 0 -26 0.0540
-18 -2 18 0.0270
-3 -13 -11 0.0659
17 2 -20 0.0390
8 -12 14 0.0706
-1 -3 29 0.0502
-8 12 -14 0.0706
_exptl_crystal_size_max          0.144
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.070
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
2.9911 12.9942 11.9975 0.1781 -0.9390 0.2786
-19.9884 0.9975 -13.9916 0.5299 0.1235 -0.8519
10.9893 -0.0004 25.9853 0.0190 -0.1626 1.0093
-10.9893 0.0004 -25.9853 -0.0190 0.1626 -1.0093
-17.9953 -2.0037 17.9894 0.9693 0.2112 0.1795
-2.9914 -12.9943 -10.9980 -0.1614 0.9359 -0.2487
16.9962 2.0037 -19.9883 -0.9649 -0.1975 -0.2603
7.9978 -11.9950 13.9882 -0.1522 0.7088 0.7196
-1.0049 -3.0014 28.9828 0.5028 0.1192 0.8784
-7.9978 11.9950 -13.9882 0.1522 -0.7088 -0.7196

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0795
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            73029
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.545
_diffrn_reflns_theta_min         2.212
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_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    -43.00  57.00   0.50   20.00    --   26.87 -77.00 -30.00  200
  2  ω    -20.00  69.00   0.50   20.00    --   26.87 -99.00 150.00  178
  3  ω    -42.00  48.00   0.50   20.00    --   26.87 -57.00-150.00  180
  4  ω      6.00  96.00   0.50   20.00    --   26.87  57.00-180.00  180
  5  ω    -42.00  48.00   0.50   20.00    --   26.87 -57.00  30.00  180
  6  ω     -3.00  97.00   0.50   20.00    --   26.87  77.00 -90.00  200
  7  ω     -3.00  97.00   0.50   20.00    --   26.87  77.00  60.00  200
  8  ω      6.00  96.00   0.50   20.00    --   26.87  57.00   0.00  180
  9  ω      6.00  67.00   0.50   20.00    --   26.87  57.00-120.00  122
 10  ω    -20.00  69.00   0.50   20.00    --   26.87 -99.00 -60.00  178
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0378916000
_diffrn_orient_matrix_UB_12      0.0069613000
_diffrn_orient_matrix_UB_13      0.0167540000
_diffrn_orient_matrix_UB_21      -0.0073493000
_diffrn_orient_matrix_UB_22      -0.0676652000
_diffrn_orient_matrix_UB_23      -0.0031496000
_diffrn_orient_matrix_UB_31      0.0211436000
_diffrn_orient_matrix_UB_32      -0.0110293000
_diffrn_orient_matrix_UB_33      0.0298975000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6833
_reflns_number_total             10459
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-17); encifer 1.5.2 (CCDC, 2016)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_shelxl_version_number           2017/1
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         10459
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0574
_refine_ls_restrained_S_all      1.026
_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)+(0.0352P)²+1.9980P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1288
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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
F1 F -0.22175(7) 0.52225(13) 0.64341(6) 0.0439(3) Uani 1 1 d . . . . .
F2 F -0.03870(7) 1.05967(13) 0.90571(6) 0.0446(3) Uani 1 1 d . . . . .
F3 F 0.47506(7) 0.90383(13) 0.68656(6) 0.0460(3) Uani 1 1 d . . . . .
F4 F 0.59843(6) 0.82148(13) 0.45296(6) 0.0422(3) Uani 1 1 d . . . . .
F5 F -0.14317(7) 0.78578(12) 0.40352(7) 0.0508(4) Uani 1 1 d . . . . .
F6 F 0.31750(8) 1.29413(13) 0.27830(7) 0.0520(4) Uani 1 1 d . . . . .
N1 N 0.17433(8) 0.76056(14) 0.56210(7) 0.0216(3) Uani 1 1 d . . . . .
C1 C 0.15139(10) 0.67596(16) 0.60810(8) 0.0210(3) Uani 1 1 d . . . . .
C2 C 0.17248(10) 0.54498(17) 0.60689(9) 0.0237(3) Uani 1 1 d . . . . .
H2 H 0.1543(11) 0.4885(19) 0.6410(9) 0.028 Uiso 1 1 d R . . . .
C3 C 0.22160(10) 0.49986(17) 0.55746(9) 0.0246(4) Uani 1 1 d . . . . .
H3 H 0.2376(12) 0.408(2) 0.5554(9) 0.030 Uiso 1 1 d R . . . .
C4 C 0.24852(10) 0.58664(17) 0.51096(9) 0.0244(3) Uani 1 1 d . . . . .
H4 H 0.2826(12) 0.560(2) 0.4764(10) 0.029 Uiso 1 1 d R . . . .
C5 C 0.22241(10) 0.71565(16) 0.51420(8) 0.0212(3) Uani 1 1 d . . . . .
C6 C 0.09917(10) 0.72928(16) 0.66134(8) 0.0214(3) Uani 1 1 d . . . . .
C7 C 0.13267(10) 0.81178(16) 0.70520(8) 0.0221(3) Uani 1 1 d . . . . .
C8 C 0.01222(10) 0.68041(16) 0.65891(8) 0.0220(3) Uani 1 1 d . . . . .
C9 C -0.02434(11) 0.62166(18) 0.71196(9) 0.0274(4) Uani 1 1 d . . . . .
H9 H 0.0082(12) 0.615(2) 0.7529(10) 0.033 Uiso 1 1 d R . . . .
C10 C -0.10343(11) 0.5689(2) 0.70747(10) 0.0318(4) Uani 1 1 d . . . . .
H10 H -0.1280(12) 0.528(2) 0.7446(10) 0.038 Uiso 1 1 d R . . . .
C11 C -0.14483(11) 0.57610(19) 0.64887(10) 0.0305(4) Uani 1 1 d . . . . .
C12 C -0.11113(11) 0.63327(19) 0.59496(9) 0.0302(4) Uani 1 1 d . . . . .
H12 H -0.1441(13) 0.635(2) 0.5544(10) 0.036 Uiso 1 1 d R . . . .
C13 C -0.03183(11) 0.68399(18) 0.60004(8) 0.0252(4) Uani 1 1 d . . . . .
H13 H -0.0065(12) 0.7190(19) 0.5616(10) 0.030 Uiso 1 1 d R . . . .
C14 C 0.08657(10) 0.87924(17) 0.75732(8) 0.0234(3) Uani 1 1 d . . . . .
C15 C 0.12471(11) 0.90037(19) 0.81789(9) 0.0281(4) Uani 1 1 d . . . . .
H15 H 0.1802(13) 0.867(2) 0.8258(9) 0.034 Uiso 1 1 d R . . . .
C16 C 0.08300(12) 0.9609(2) 0.86778(9) 0.0320(4) Uani 1 1 d . . . . .
H16 H 0.1085(13) 0.975(2) 0.9088(10) 0.038 Uiso 1 1 d R . . . .
C17 C 0.00324(12) 1.00187(19) 0.85665(9) 0.0310(4) Uani 1 1 d . . . . .
C18 C -0.03637(12) 0.98684(19) 0.79781(9) 0.0302(4) Uani 1 1 d . . . . .
H18 H -0.0917(13) 1.020(2) 0.7924(10) 0.036 Uiso 1 1 d R . . . .
C19 C 0.00575(11) 0.92582(18) 0.74822(9) 0.0273(4) Uani 1 1 d . . . . .
H19 H -0.0213(12) 0.917(2) 0.7059(10) 0.033 Uiso 1 1 d R . . . .
C20 C 0.22417(10) 0.83889(17) 0.70271(8) 0.0232(3) Uani 1 1 d . . . . .
C21 C 0.25352(11) 0.95837(18) 0.68118(9) 0.0277(4) Uani 1 1 d . . . . .
H21 H 0.2141(12) 1.027(2) 0.6676(9) 0.033 Uiso 1 1 d R . . . .
C22 C 0.33813(12) 0.9809(2) 0.67624(10) 0.0326(4) Uani 1 1 d . . . . .
H22 H 0.3589(13) 1.059(2) 0.6601(10) 0.039 Uiso 1 1 d R . . . .
C23 C 0.39216(11) 0.8836(2) 0.69366(9) 0.0316(4) Uani 1 1 d . . . . .
C24 C 0.36638(12) 0.7658(2) 0.71600(10) 0.0352(4) Uani 1 1 d . . . . .
H24 H 0.4060(13) 0.702(2) 0.7292(10) 0.042 Uiso 1 1 d R . . . .
C25 C 0.28138(11) 0.7435(2) 0.71993(10) 0.0317(4) Uani 1 1 d . . . . .
H25 H 0.2615(12) 0.660(2) 0.7331(10) 0.038 Uiso 1 1 d R . . . .
C26 C 0.25123(10) 0.81297(16) 0.46598(8) 0.0211(3) Uani 1 1 d . . . . .
C27 C 0.19811(10) 0.88710(16) 0.43050(8) 0.0208(3) Uani 1 1 d . . . . .
C28 C 0.34308(10) 0.82036(16) 0.46130(8) 0.0224(3) Uani 1 1 d . . . . .
C29 C 0.38308(11) 0.81219(18) 0.40197(8) 0.0262(4) Uani 1 1 d . . . . .
H29 H 0.3497(12) 0.8063(19) 0.3621(10) 0.031 Uiso 1 1 d R . . . .
C30 C 0.46894(11) 0.81273(19) 0.39896(9) 0.0296(4) Uani 1 1 d . . . . .
H30 H 0.4977(12) 0.808(2) 0.3573(10) 0.035 Uiso 1 1 d R . . . .
C31 C 0.51392(11) 0.82191(19) 0.45597(9) 0.0296(4) Uani 1 1 d . . . . .
C32 C 0.47742(11) 0.8305(2) 0.51563(9) 0.0302(4) Uani 1 1 d . . . . .
H32 H 0.5100(12) 0.837(2) 0.5540(10) 0.036 Uiso 1 1 d R . . . .
C33 C 0.39171(11) 0.82796(19) 0.51789(8) 0.0264(4) Uani 1 1 d . . . . .
H33 H 0.3645(12) 0.831(2) 0.5593(10) 0.032 Uiso 1 1 d R . . . .
C34 C 0.10728(10) 0.85974(17) 0.42567(8) 0.0224(3) Uani 1 1 d . . . . .
C35 C 0.07804(12) 0.73332(19) 0.41642(10) 0.0322(4) Uani 1 1 d . . . . .
H35 H 0.1171(13) 0.661(2) 0.4131(10) 0.039 Uiso 1 1 d R . . . .
C36 C -0.00592(13) 0.7080(2) 0.40935(11) 0.0399(5) Uani 1 1 d . . . . .
H36 H -0.0259(14) 0.622(2) 0.4031(11) 0.048 Uiso 1 1 d R . . . .
C37 C -0.06034(11) 0.8105(2) 0.41091(10) 0.0339(4) Uani 1 1 d . . . . .
C38 C -0.03523(11) 0.93690(19) 0.41960(9) 0.0285(4) Uani 1 1 d . . . . .
H38 H -0.0750(12) 1.007(2) 0.4208(10) 0.034 Uiso 1 1 d R . . . .
C39 C 0.04947(11) 0.96045(18) 0.42647(8) 0.0251(4) Uani 1 1 d . . . . .
H39 H 0.0699(12) 1.049(2) 0.4315(9) 0.030 Uiso 1 1 d R . . . .
C40 C 0.22786(10) 0.99877(16) 0.39149(8) 0.0223(3) Uani 1 1 d . . . . .
C41 C 0.20134(10) 1.01306(17) 0.32717(8) 0.0235(3) Uani 1 1 d . . . . .
H41 H 0.1619(12) 0.9492(19) 0.3084(9) 0.028 Uiso 1 1 d R . . . .
C42 C 0.23118(11) 1.11279(19) 0.28916(9) 0.0293(4) Uani 1 1 d . . . . .
H42 H 0.2150(12) 1.122(2) 0.2446(10) 0.035 Uiso 1 1 d R . . . .
C43 C 0.28668(12) 1.19788(19) 0.31624(10) 0.0335(4) Uani 1 1 d . . . . .
C44 C 0.31243(12) 1.1914(2) 0.38022(10) 0.0346(4) Uani 1 1 d . . . . .
H44 H 0.3502(13) 1.256(2) 0.3969(10) 0.041 Uiso 1 1 d R . . . .
C45 C 0.28225(11) 1.09058(18) 0.41772(9) 0.0293(4) Uani 1 1 d . . . . .
H45 H 0.2996(12) 1.085(2) 0.4634(10) 0.035 Uiso 1 1 d 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
F1 C11 1.361(2) . ?
F2 C17 1.361(2) . ?
F3 C23 1.362(2) . ?
F4 C31 1.364(2) . ?
F5 C37 1.365(2) . ?
F6 C43 1.360(2) . ?
N1 C1 1.343(2) . ?
N1 C5 1.346(2) . ?
C1 C2 1.391(2) . ?
C1 C6 1.497(2) . ?
C2 H2 0.962(19) . ?
C2 C3 1.380(3) . ?
C3 H3 0.98(2) . ?
C3 C4 1.384(2) . ?
C4 H4 0.95(2) . ?
C4 C5 1.395(2) . ?
C5 C26 1.490(2) . ?
C6 C7 1.348(2) . ?
C6 C8 1.489(2) . ?
C7 C14 1.487(2) . ?
C7 C20 1.502(2) . ?
C8 C9 1.388(2) . ?
C8 C13 1.398(2) . ?
C9 H9 0.99(2) . ?
C9 C10 1.387(3) . ?
C10 H10 0.96(2) . ?
C10 C11 1.374(3) . ?
C11 C12 1.376(3) . ?
C12 H12 0.98(2) . ?
C12 C13 1.383(2) . ?
C13 H13 0.97(2) . ?
C14 C15 1.401(2) . ?
C14 C19 1.398(2) . ?
C15 H15 0.97(2) . ?
C15 C16 1.385(3) . ?
C16 H16 0.95(2) . ?
C16 C17 1.369(3) . ?
C17 C18 1.372(3) . ?
C18 H18 0.96(2) . ?
C18 C19 1.386(3) . ?
C19 H19 0.98(2) . ?
C20 C21 1.393(2) . ?
C20 C25 1.389(3) . ?
C21 H21 0.99(2) . ?
C21 C22 1.388(3) . ?
C22 H22 0.94(2) . ?
C22 C23 1.372(3) . ?
C23 C24 1.364(3) . ?
C24 H24 0.95(2) . ?
C24 C25 1.392(3) . ?
C25 H25 0.96(2) . ?
C26 C27 1.354(2) . ?
C26 C28 1.487(2) . ?
C27 C34 1.493(2) . ?
C27 C40 1.486(2) . ?
C28 C29 1.393(2) . ?
C28 C33 1.398(2) . ?
C29 H29 0.98(2) . ?
C29 C30 1.386(2) . ?
C30 H30 0.98(2) . ?
C30 C31 1.375(3) . ?
C31 C32 1.374(3) . ?
C32 H32 0.95(2) . ?
C32 C33 1.383(2) . ?
C33 H33 0.97(2) . ?
C34 C35 1.396(2) . ?
C34 C39 1.394(2) . ?
C35 H35 0.98(2) . ?
C35 C36 1.384(3) . ?
C36 H36 0.95(2) . ?
C36 C37 1.372(3) . ?
C37 C38 1.374(3) . ?
C38 H38 0.97(2) . ?
C38 C39 1.392(2) . ?
C39 H39 0.97(2) . ?
C40 C41 1.395(2) . ?
C40 C45 1.393(2) . ?
C41 H41 0.99(2) . ?
C41 C42 1.382(2) . ?
C42 H42 0.96(2) . ?
C42 C43 1.366(3) . ?
C43 C44 1.379(3) . ?
C44 H44 0.96(2) . ?
C44 C45 1.386(3) . ?
C45 H45 0.98(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C5 117.55(15) . . ?
N1 C1 C2 123.09(16) . . ?
N1 C1 C6 116.31(15) . . ?
C2 C1 C6 120.58(15) . . ?
C1 C2 H2 119.8(12) . . ?
C3 C2 C1 118.85(16) . . ?
C3 C2 H2 121.4(12) . . ?
C2 C3 H3 120.7(11) . . ?
C2 C3 C4 118.87(17) . . ?
C4 C3 H3 120.4(11) . . ?
C3 C4 H4 121.7(12) . . ?
C3 C4 C5 118.91(16) . . ?
C5 C4 H4 119.3(12) . . ?
N1 C5 C4 122.63(15) . . ?
N1 C5 C26 116.53(15) . . ?
C4 C5 C26 120.74(15) . . ?
C7 C6 C1 119.94(15) . . ?
C7 C6 C8 127.10(15) . . ?
C8 C6 C1 112.96(14) . . ?
C6 C7 C14 125.43(15) . . ?
C6 C7 C20 118.56(15) . . ?
C14 C7 C20 116.01(14) . . ?
C9 C8 C6 122.02(15) . . ?
C9 C8 C13 118.65(16) . . ?
C13 C8 C6 119.12(15) . . ?
C8 C9 H9 118.3(12) . . ?
C10 C9 C8 121.18(17) . . ?
C10 C9 H9 120.5(12) . . ?
C9 C10 H10 120.3(12) . . ?
C11 C10 C9 118.15(18) . . ?
C11 C10 H10 121.5(12) . . ?
F1 C11 C10 118.75(17) . . ?
F1 C11 C12 118.47(17) . . ?
C10 C11 C12 122.76(17) . . ?
C11 C12 H12 118.6(12) . . ?
C11 C12 C13 118.36(17) . . ?
C13 C12 H12 123.0(12) . . ?
C8 C13 H13 120.5(12) . . ?
C12 C13 C8 120.88(17) . . ?
C12 C13 H13 118.6(12) . . ?
C15 C14 C7 119.94(15) . . ?
C19 C14 C7 122.49(15) . . ?
C19 C14 C15 117.56(16) . . ?
C14 C15 H15 119.3(12) . . ?
C16 C15 C14 121.36(17) . . ?
C16 C15 H15 119.3(12) . . ?
C15 C16 H16 121.6(13) . . ?
C17 C16 C15 118.59(17) . . ?
C17 C16 H16 119.8(13) . . ?
F2 C17 C16 119.01(16) . . ?
F2 C17 C18 118.46(16) . . ?
C16 C17 C18 122.53(18) . . ?
C17 C18 H18 118.9(12) . . ?
C17 C18 C19 118.48(17) . . ?
C19 C18 H18 122.6(12) . . ?
C14 C19 H19 119.4(12) . . ?
C18 C19 C14 121.44(16) . . ?
C18 C19 H19 119.1(12) . . ?
C21 C20 C7 120.86(15) . . ?
C25 C20 C7 120.55(16) . . ?
C25 C20 C21 118.56(16) . . ?
C20 C21 H21 119.9(12) . . ?
C22 C21 C20 120.61(18) . . ?
C22 C21 H21 119.4(12) . . ?
C21 C22 H22 121.8(13) . . ?
C23 C22 C21 118.65(18) . . ?
C23 C22 H22 119.6(13) . . ?
F3 C23 C22 118.70(18) . . ?
F3 C23 C24 118.43(18) . . ?
C24 C23 C22 122.83(17) . . ?
C23 C24 H24 120.1(13) . . ?
C23 C24 C25 118.06(19) . . ?
C25 C24 H24 121.8(13) . . ?
C20 C25 C24 121.27(19) . . ?
C20 C25 H25 118.9(13) . . ?
C24 C25 H25 119.8(12) . . ?
C27 C26 C5 122.59(15) . . ?
C27 C26 C28 123.98(15) . . ?
C28 C26 C5 113.43(14) . . ?
C26 C27 C34 122.81(15) . . ?
C26 C27 C40 121.46(15) . . ?
C40 C27 C34 115.68(14) . . ?
C29 C28 C26 121.82(15) . . ?
C29 C28 C33 118.37(15) . . ?
C33 C28 C26 119.70(15) . . ?
C28 C29 H29 119.1(11) . . ?
C30 C29 C28 120.90(16) . . ?
C30 C29 H29 120.0(11) . . ?
C29 C30 H30 121.5(12) . . ?
C31 C30 C29 118.46(17) . . ?
C31 C30 H30 120.0(12) . . ?
F4 C31 C30 118.39(16) . . ?
F4 C31 C32 118.76(16) . . ?
C32 C31 C30 122.85(16) . . ?
C31 C32 H32 120.9(12) . . ?
C31 C32 C33 117.99(16) . . ?
C33 C32 H32 121.1(12) . . ?
C28 C33 H33 118.9(12) . . ?
C32 C33 C28 121.41(16) . . ?
C32 C33 H33 119.7(11) . . ?
C35 C34 C27 120.92(16) . . ?
C39 C34 C27 120.92(15) . . ?
C39 C34 C35 118.06(16) . . ?
C34 C35 H35 120.2(13) . . ?
C36 C35 C34 121.16(18) . . ?
C36 C35 H35 118.6(13) . . ?
C35 C36 H36 121.2(14) . . ?
C37 C36 C35 118.52(18) . . ?
C37 C36 H36 120.3(14) . . ?
F5 C37 C36 118.59(18) . . ?
F5 C37 C38 118.47(17) . . ?
C36 C37 C38 122.94(17) . . ?
C37 C38 H38 121.2(12) . . ?
C37 C38 C39 117.71(18) . . ?
C39 C38 H38 121.1(12) . . ?
C34 C39 H39 118.1(11) . . ?
C38 C39 C34 121.60(17) . . ?
C38 C39 H39 120.3(11) . . ?
C41 C40 C27 119.93(15) . . ?
C45 C40 C27 121.38(15) . . ?
C45 C40 C41 118.69(16) . . ?
C40 C41 H41 119.3(11) . . ?
C42 C41 C40 120.85(17) . . ?
C42 C41 H41 119.9(11) . . ?
C41 C42 H42 121.9(13) . . ?
C43 C42 C41 118.41(17) . . ?
C43 C42 H42 119.6(13) . . ?
F6 C43 C42 118.32(18) . . ?
F6 C43 C44 118.56(18) . . ?
C42 C43 C44 123.12(17) . . ?
C43 C44 H44 119.2(13) . . ?
C43 C44 C45 117.83(18) . . ?
C45 C44 H44 123.0(13) . . ?
C40 C45 H45 119.9(12) . . ?
C44 C45 C40 121.00(17) . . ?
C44 C45 H45 119.1(12) . . ?

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
F1 C11 C12 C13 -177.83(17) . . . . ?
F2 C17 C18 C19 -178.81(17) . . . . ?
F3 C23 C24 C25 -176.74(17) . . . . ?
F4 C31 C32 C33 -178.60(17) . . . . ?
F5 C37 C38 C39 -179.44(17) . . . . ?
F6 C43 C44 C45 -178.22(18) . . . . ?
N1 C1 C2 C3 2.3(2) . . . . ?
N1 C1 C6 C7 -69.9(2) . . . . ?
N1 C1 C6 C8 110.61(16) . . . . ?
N1 C5 C26 C27 -57.6(2) . . . . ?
N1 C5 C26 C28 122.13(16) . . . . ?
C1 N1 C5 C4 0.0(2) . . . . ?
C1 N1 C5 C26 -176.43(14) . . . . ?
C1 C2 C3 C4 0.3(2) . . . . ?
C1 C6 C7 C14 175.19(15) . . . . ?
C1 C6 C7 C20 -5.3(2) . . . . ?
C1 C6 C8 C9 126.14(17) . . . . ?
C1 C6 C8 C13 -48.5(2) . . . . ?
C2 C1 C6 C7 111.50(19) . . . . ?
C2 C1 C6 C8 -68.04(19) . . . . ?
C2 C3 C4 C5 -2.5(2) . . . . ?
C3 C4 C5 N1 2.4(2) . . . . ?
C3 C4 C5 C26 178.74(15) . . . . ?
C4 C5 C26 C27 125.88(18) . . . . ?
C4 C5 C26 C28 -54.4(2) . . . . ?
C5 N1 C1 C2 -2.4(2) . . . . ?
C5 N1 C1 C6 178.97(14) . . . . ?
C5 C26 C27 C34 -13.4(3) . . . . ?
C5 C26 C27 C40 169.13(15) . . . . ?
C5 C26 C28 C29 128.74(17) . . . . ?
C5 C26 C28 C33 -47.4(2) . . . . ?
C6 C1 C2 C3 -179.17(15) . . . . ?
C6 C7 C14 C15 144.25(18) . . . . ?
C6 C7 C14 C19 -37.0(3) . . . . ?
C6 C7 C20 C21 107.9(2) . . . . ?
C6 C7 C20 C25 -70.0(2) . . . . ?
C6 C8 C9 C10 -175.58(17) . . . . ?
C6 C8 C13 C12 176.56(16) . . . . ?
C7 C6 C8 C9 -53.4(3) . . . . ?
C7 C6 C8 C13 131.99(19) . . . . ?
C7 C14 C15 C16 -178.90(17) . . . . ?
C7 C14 C19 C18 179.11(17) . . . . ?
C7 C20 C21 C22 -177.11(16) . . . . ?
C7 C20 C25 C24 178.02(18) . . . . ?
C8 C6 C7 C14 -5.3(3) . . . . ?
C8 C6 C7 C20 174.17(15) . . . . ?
C8 C9 C10 C11 0.1(3) . . . . ?
C9 C8 C13 C12 1.7(3) . . . . ?
C9 C10 C11 F1 178.62(17) . . . . ?
C9 C10 C11 C12 0.0(3) . . . . ?
C10 C11 C12 C13 0.8(3) . . . . ?
C11 C12 C13 C8 -1.7(3) . . . . ?
C13 C8 C9 C10 -0.9(3) . . . . ?
C14 C7 C20 C21 -72.5(2) . . . . ?
C14 C7 C20 C25 109.54(19) . . . . ?
C14 C15 C16 C17 -0.8(3) . . . . ?
C15 C14 C19 C18 -2.1(3) . . . . ?
C15 C16 C17 F2 178.98(18) . . . . ?
C15 C16 C17 C18 -1.0(3) . . . . ?
C16 C17 C18 C19 1.1(3) . . . . ?
C17 C18 C19 C14 0.5(3) . . . . ?
C19 C14 C15 C16 2.3(3) . . . . ?
C20 C7 C14 C15 -35.3(2) . . . . ?
C20 C7 C14 C19 143.47(17) . . . . ?
C20 C21 C22 C23 -0.7(3) . . . . ?
C21 C20 C25 C24 0.0(3) . . . . ?
C21 C22 C23 F3 177.61(16) . . . . ?
C21 C22 C23 C24 -0.4(3) . . . . ?
C22 C23 C24 C25 1.3(3) . . . . ?
C23 C24 C25 C20 -1.1(3) . . . . ?
C25 C20 C21 C22 0.9(3) . . . . ?
C26 C27 C34 C35 -43.8(2) . . . . ?
C26 C27 C34 C39 139.96(18) . . . . ?
C26 C27 C40 C41 132.09(17) . . . . ?
C26 C27 C40 C45 -47.8(2) . . . . ?
C26 C28 C29 C30 -176.73(17) . . . . ?
C26 C28 C33 C32 177.79(17) . . . . ?
C27 C26 C28 C29 -51.6(2) . . . . ?
C27 C26 C28 C33 132.33(18) . . . . ?
C27 C34 C35 C36 -177.42(18) . . . . ?
C27 C34 C39 C38 177.58(16) . . . . ?
C27 C40 C41 C42 -177.01(16) . . . . ?
C27 C40 C45 C44 177.25(17) . . . . ?
C28 C26 C27 C34 166.93(15) . . . . ?
C28 C26 C27 C40 -10.6(3) . . . . ?
C28 C29 C30 C31 -0.2(3) . . . . ?
C29 C28 C33 C32 1.5(3) . . . . ?
C29 C30 C31 F4 179.53(17) . . . . ?
C29 C30 C31 C32 0.0(3) . . . . ?
C30 C31 C32 C33 0.9(3) . . . . ?
C31 C32 C33 C28 -1.7(3) . . . . ?
C33 C28 C29 C30 -0.6(3) . . . . ?
C34 C27 C40 C41 -45.6(2) . . . . ?
C34 C27 C40 C45 134.52(17) . . . . ?
C34 C35 C36 C37 0.7(3) . . . . ?
C35 C34 C39 C38 1.3(3) . . . . ?
C35 C36 C37 F5 179.59(19) . . . . ?
C35 C36 C37 C38 -0.4(3) . . . . ?
C36 C37 C38 C39 0.6(3) . . . . ?
C37 C38 C39 C34 -1.0(3) . . . . ?
C39 C34 C35 C36 -1.1(3) . . . . ?
C40 C27 C34 C35 133.80(18) . . . . ?
C40 C27 C34 C39 -42.4(2) . . . . ?
C40 C41 C42 C43 -0.6(3) . . . . ?
C41 C40 C45 C44 -2.7(3) . . . . ?
C41 C42 C43 F6 178.45(16) . . . . ?
C41 C42 C43 C44 -2.0(3) . . . . ?
C42 C43 C44 C45 2.2(3) . . . . ?
C43 C44 C45 C40 0.2(3) . . . . ?
C45 C40 C41 C42 2.9(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.092
_oxdiff_exptl_absorpt_empirical_full_min 0.911
_cell_oxdiff_length_a            16.1184(6)
_cell_oxdiff_length_b            10.2930(2)
_cell_oxdiff_length_c            20.6114(8)
_cell_oxdiff_angle_alpha         90.000(3)
_cell_oxdiff_angle_beta          90.774(3)
_cell_oxdiff_angle_gamma         90.006(3)
_cell_oxdiff_volume              3419.3(2)
_cell_oxdiff_measurement_reflns_used 10025
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_ambient_environment      'perfluoro polyether oil / N~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_ga_tro129
_database_code_depnum_ccdc_archive 'CCDC 1817690'
_audit_update_record             
;
2018-01-17 deposited with the CCDC.
2018-02-05 downloaded from the CCDC.
;
_audit_creation_date             2018-01-15

_audit_block_code                ga_tro129
_audit_block_refno               2398
_audit_block_usercomment         tr1493_3


_audit_creation_method           
;
Olex2 1.2
(compiled Aug 10 2017 17:44:14 for OlexSys, GUI svn.r5381)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C25 H19 N'
_chemical_formula_sum            'C25 H19 N'
_chemical_formula_weight         333.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_chemical_absolute_configuration unk
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
_chemical_melting_point          ?
_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_diffrn_ambient_temperature      100(1)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

_cell_length_a                   9.652(5)
_cell_length_b                   9.262(4)
_cell_length_c                   10.579(5)
_cell_angle_alpha                90
_cell_angle_beta                 107.030(14)
_cell_angle_gamma                90
_cell_volume                     904.2(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6018
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.19
_cell_measurement_theta_min      2.51
_shelx_estimated_absorpt_T_max   0.989
_shelx_estimated_absorpt_T_min   0.983
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  0.8623
_exptl_absorpt_correction_T_min  0.8055

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements (Blessing 1995)
SADABS (see _computing_data_reduction)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.150
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21932
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.504
_diffrn_reflns_theta_min         2.013
_diffrn_detector_area_resol_mean 8.19
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker AXS Smart 1000'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-Ray tube (Mo)'
_diffrn_source_type              'fine focus tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.887
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                4474
_reflns_number_total             5499
_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       
;
SAINT (see _computing_data_reduction). Includes estimated systematic errors
 of the unit cell constants from Monte Carlo simulations.
;
_computing_data_collection       'SMART-5.631 (Bruker AXS, 2003)'
_computing_data_reduction        
'SAINT V8.34A (Bruker AXS, 1997-2013),SADABS-2014_5 (Sheldrick and Bruker AXS, 1997-2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-17); encifer 1.5.2 (CCDC, 2016)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_shelxl_version_number           2018/1
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details 
;
 Flack x determined using 1701 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         5499
_refine_ls_number_restraints     86
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0449
_refine_ls_restrained_S_all      1.049
_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)+(0.0421P)²+0.1187P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.1009
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C1-C3A \\sim C1-C3B
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim
C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim
C23 \\sim C24 \\sim C25 \\sim C26 \\sim C3A \\sim C5A \\sim C6A \\sim C7A \\sim
C8A \\sim C3B \\sim C4B \\sim C5B \\sim C6B \\sim C7B \\sim N4B \\sim N8B:
within 0.5A with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C3A) = Uanis(C3B)
4. Rigid body (RIGU) restrains
 C3A, N4B, C5A, C6A, C7A, C8A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3B, C4B, C5B, C6B, C7B, N8B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C3B)=Sof(C4B)=Sof(H4B)=Sof(C5B)=Sof(H5B)=Sof(C6B)=Sof(H6B)=Sof(C7B)=
 Sof(H7B)=Sof(N8B)=1-FVAR(1)
 Sof(C3A)=Sof(N4B)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7A)=
 Sof(C8A)=Sof(H8A)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C5A(H5A), C6A(H6A), C7A(H7A), C8A(H8A), C4B(H4B), C5B(H5B), C6B(H6B), C7B(H7B)
6.b Fitted hexagon refined as free rotating group:
 C3A(N4B,C5A,C6A,C7A,C8A), C3B(C4B,C5B,C6B,C7B,N8B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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 -0.1126(2) -0.6840(2) -0.20294(19) 0.0231(4) Uani 1 1 d D U . . .
C2 C -0.2531(2) -0.7195(2) -0.26092(18) 0.0213(4) Uani 1 1 d . U . . .
C9 C -0.0100(2) -0.6537(2) -0.28083(18) 0.0209(4) Uani 1 1 d . U . . .
C10 C 0.0105(2) -0.7538(2) -0.37171(19) 0.0226(4) Uani 1 1 d . U . . .
H10 H -0.040(2) -0.844(3) -0.385(2) 0.023(6) Uiso 1 1 d . . . . .
C11 C 0.1059(2) -0.7245(3) -0.4436(2) 0.0283(4) Uani 1 1 d . U . . .
H11 H 0.119(3) -0.794(3) -0.509(3) 0.040(7) Uiso 1 1 d . . . . .
C12 C 0.1814(2) -0.5950(3) -0.4264(2) 0.0306(5) Uani 1 1 d . U . . .
H12 H 0.250(3) -0.568(3) -0.478(3) 0.047(8) Uiso 1 1 d . . . . .
C13 C 0.1618(2) -0.4958(3) -0.3354(2) 0.0277(5) Uani 1 1 d . U . . .
H13 H 0.215(3) -0.409(3) -0.325(2) 0.026(6) Uiso 1 1 d . . . . .
C14 C 0.0686(2) -0.5254(2) -0.2616(2) 0.0239(4) Uani 1 1 d . U . . .
H14 H 0.056(3) -0.458(3) -0.198(2) 0.034(7) Uiso 1 1 d . . . . .
C15 C -0.3488(2) -0.7765(2) -0.18461(19) 0.0219(4) Uani 1 1 d . U . . .
C16 C -0.4884(2) -0.7241(2) -0.2089(2) 0.0234(4) Uani 1 1 d . U . . .
H16 H -0.517(3) -0.657(4) -0.266(3) 0.052(9) Uiso 1 1 d . . . . .
C17 C -0.5781(2) -0.7780(2) -0.1404(2) 0.0294(5) Uani 1 1 d . U . . .
H17 H -0.674(3) -0.741(3) -0.162(3) 0.040(7) Uiso 1 1 d . . . . .
C18 C -0.5308(3) -0.8854(3) -0.0474(2) 0.0313(5) Uani 1 1 d . U . . .
H18 H -0.597(3) -0.920(4) 0.001(3) 0.048(8) Uiso 1 1 d . . . . .
C19 C -0.3924(3) -0.9399(3) -0.0233(2) 0.0310(5) Uani 1 1 d . U . . .
H19 H -0.357(3) -1.015(3) 0.044(2) 0.034(7) Uiso 1 1 d . . . . .
C20 C -0.3020(2) -0.8861(2) -0.0921(2) 0.0249(4) Uani 1 1 d . U . . .
H20 H -0.207(3) -0.921(3) -0.076(2) 0.024(6) Uiso 1 1 d . . . . .
C21 C -0.32098(19) -0.7086(2) -0.40691(19) 0.0222(4) Uani 1 1 d . U . . .
C22 C -0.2974(2) -0.5889(3) -0.4772(2) 0.0278(5) Uani 1 1 d . U . . .
H22 H -0.241(3) -0.513(3) -0.433(2) 0.030(6) Uiso 1 1 d . . . . .
C23 C -0.3586(3) -0.5815(3) -0.6128(2) 0.0337(5) Uani 1 1 d . U . . .
H23 H -0.340(3) -0.498(3) -0.662(3) 0.039(7) Uiso 1 1 d . . . . .
C24 C -0.4453(2) -0.6916(3) -0.6803(2) 0.0347(5) Uani 1 1 d . U . . .
H24 H -0.487(3) -0.689(3) -0.774(3) 0.040(7) Uiso 1 1 d . . . . .
C25 C -0.4724(2) -0.8102(3) -0.6112(2) 0.0322(5) Uani 1 1 d . U . . .
H25 H -0.534(3) -0.889(3) -0.656(2) 0.037(7) Uiso 1 1 d . . . . .
C26 C -0.4109(2) -0.8181(2) -0.4750(2) 0.0251(4) Uani 1 1 d . U . . .
H26 H -0.430(3) -0.900(3) -0.430(2) 0.028(6) Uiso 1 1 d . . . . .
C3A C -0.0403(6) -0.6854(8) -0.0546(3) 0.0279(8) Uani 0.559(12) 1 d D U P A 1
N4B N 0.0955(6) -0.7501(7) -0.0123(3) 0.0351(12) Uani 0.559(12) 1 d G U P A 1
C5A C 0.1728(5) -0.7493(6) 0.1211(4) 0.0340(13) Uani 0.559(12) 1 d G U P A 1
H5A H 0.265633 -0.793522 0.149996 0.041 Uiso 0.559(12) 1 calc R . P A 1
C6A C 0.1144(7) -0.6840(7) 0.2122(2) 0.0390(17) Uani 0.559(12) 1 d G U P A 1
H6A H 0.167296 -0.683461 0.303397 0.047 Uiso 0.559(12) 1 calc R . P A 1
C7A C -0.0213(7) -0.6193(6) 0.1699(4) 0.0354(19) Uani 0.559(12) 1 d G U P A 1
H7A H -0.061246 -0.574643 0.232202 0.042 Uiso 0.559(12) 1 calc R . P A 1
C8A C -0.0987(6) -0.6201(7) 0.0365(5) 0.0377(14) Uani 0.559(12) 1 d G U P A 1
H8A H -0.191452 -0.575885 0.007605 0.045 Uiso 0.559(12) 1 calc R . P A 1
C3B C -0.0583(8) -0.6615(10) -0.0627(3) 0.0279(8) Uani 0.441(12) 1 d D U P A 2
C4B C 0.0741(8) -0.7194(9) 0.0097(6) 0.0409(18) Uani 0.441(12) 1 d G U P A 2
H4B H 0.132154 -0.770055 -0.034200 0.049 Uiso 0.441(12) 1 calc R . P A 2
C5B C 0.1214(8) -0.7032(8) 0.1463(5) 0.036(2) Uani 0.441(12) 1 d G U P A 2
H5B H 0.211805 -0.742794 0.195725 0.043 Uiso 0.441(12) 1 calc R . P A 2
C6B C 0.0364(11) -0.6291(8) 0.2105(3) 0.047(3) Uani 0.441(12) 1 d G U P A 2
H6B H 0.068699 -0.618051 0.303825 0.056 Uiso 0.441(12) 1 calc R . P A 2
C7B C -0.0960(10) -0.5712(7) 0.1381(5) 0.043(2) Uani 0.441(12) 1 d G U P A 2
H7B H -0.154059 -0.520567 0.182001 0.051 Uiso 0.441(12) 1 calc R . P A 2
N8B N -0.1433(8) -0.5874(8) 0.0015(5) 0.0454(19) Uani 0.441(12) 1 d G U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.354(3) . ?
C1 C9 1.489(3) . ?
C1 C3A 1.519(3) . ?
C1 C3B 1.437(4) . ?
C2 C15 1.491(3) . ?
C2 C21 1.494(3) . ?
C9 C10 1.391(3) . ?
C9 C14 1.393(3) . ?
C10 H10 0.96(3) . ?
C10 C11 1.382(3) . ?
C11 H11 0.98(3) . ?
C11 C12 1.388(3) . ?
C12 H12 1.01(3) . ?
C12 C13 1.384(3) . ?
C13 H13 0.94(3) . ?
C13 C14 1.380(3) . ?
C14 H14 0.95(3) . ?
C15 C16 1.384(3) . ?
C15 C20 1.390(3) . ?
C16 H16 0.85(3) . ?
C16 C17 1.376(3) . ?
C17 H17 0.95(3) . ?
C17 C18 1.380(4) . ?
C18 H18 0.98(3) . ?
C18 C19 1.380(4) . ?
C19 H19 0.99(3) . ?
C19 C20 1.382(3) . ?
C20 H20 0.94(2) . ?
C21 C22 1.390(3) . ?
C21 C26 1.391(3) . ?
C22 H22 0.93(3) . ?
C22 C23 1.384(3) . ?
C23 H23 0.98(3) . ?
C23 C24 1.379(4) . ?
C24 H24 0.96(3) . ?
C24 C25 1.386(4) . ?
C25 H25 0.98(3) . ?
C25 C26 1.390(3) . ?
C26 H26 0.95(3) . ?
C3A N4B 1.3900 . ?
C3A C8A 1.3900 . ?
N4B C5A 1.3900 . ?
C5A H5A 0.9500 . ?
C5A C6A 1.3900 . ?
C6A H6A 0.9500 . ?
C6A C7A 1.3900 . ?
C7A H7A 0.9500 . ?
C7A C8A 1.3900 . ?
C8A H8A 0.9500 . ?
C3B C4B 1.3900 . ?
C3B N8B 1.3900 . ?
C4B H4B 0.9500 . ?
C4B C5B 1.3900 . ?
C5B H5B 0.9500 . ?
C5B C6B 1.3900 . ?
C6B H6B 0.9500 . ?
C6B C7B 1.3900 . ?
C7B H7B 0.9500 . ?
C7B N8B 1.3900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C9 122.32(17) . . ?
C2 C1 C3A 124.2(3) . . ?
C2 C1 C3B 121.1(4) . . ?
C9 C1 C3A 113.2(3) . . ?
C3B C1 C9 116.3(4) . . ?
C1 C2 C15 122.53(18) . . ?
C1 C2 C21 121.98(17) . . ?
C15 C2 C21 115.46(17) . . ?
C10 C9 C1 120.67(18) . . ?
C10 C9 C14 119.16(19) . . ?
C14 C9 C1 120.16(18) . . ?
C9 C10 H10 120.6(13) . . ?
C11 C10 C9 120.18(19) . . ?
C11 C10 H10 119.2(13) . . ?
C10 C11 H11 119.9(16) . . ?
C10 C11 C12 120.4(2) . . ?
C12 C11 H11 119.6(16) . . ?
C11 C12 H12 123.2(18) . . ?
C13 C12 C11 119.4(2) . . ?
C13 C12 H12 117.4(18) . . ?
C12 C13 H13 117.9(14) . . ?
C14 C13 C12 120.4(2) . . ?
C14 C13 H13 121.7(14) . . ?
C9 C14 H14 119.3(16) . . ?
C13 C14 C9 120.3(2) . . ?
C13 C14 H14 120.4(16) . . ?
C16 C15 C2 119.96(18) . . ?
C16 C15 C20 119.01(19) . . ?
C20 C15 C2 120.99(19) . . ?
C15 C16 H16 119(2) . . ?
C17 C16 C15 120.2(2) . . ?
C17 C16 H16 121(2) . . ?
C16 C17 H17 117.1(17) . . ?
C16 C17 C18 120.7(2) . . ?
C18 C17 H17 122.2(17) . . ?
C17 C18 H18 118.5(18) . . ?
C17 C18 C19 119.7(2) . . ?
C19 C18 H18 121.8(18) . . ?
C18 C19 H19 120.4(15) . . ?
C18 C19 C20 119.8(2) . . ?
C20 C19 H19 119.7(15) . . ?
C15 C20 H20 118.3(15) . . ?
C19 C20 C15 120.6(2) . . ?
C19 C20 H20 121.1(15) . . ?
C22 C21 C2 121.03(19) . . ?
C22 C21 C26 118.68(19) . . ?
C26 C21 C2 120.28(18) . . ?
C21 C22 H22 119.9(15) . . ?
C23 C22 C21 120.5(2) . . ?
C23 C22 H22 119.7(15) . . ?
C22 C23 H23 120.0(16) . . ?
C24 C23 C22 120.7(2) . . ?
C24 C23 H23 119.3(15) . . ?
C23 C24 H24 121.7(18) . . ?
C23 C24 C25 119.5(2) . . ?
C25 C24 H24 118.8(18) . . ?
C24 C25 H25 121.3(15) . . ?
C24 C25 C26 120.0(2) . . ?
C26 C25 H25 118.7(15) . . ?
C21 C26 H26 120.7(14) . . ?
C25 C26 C21 120.7(2) . . ?
C25 C26 H26 118.6(15) . . ?
N4B C3A C1 116.2(3) . . ?
N4B C3A C8A 120.0 . . ?
C8A C3A C1 123.7(3) . . ?
C3A N4B C5A 120.0 . . ?
N4B C5A H5A 120.0 . . ?
C6A C5A N4B 120.0 . . ?
C6A C5A H5A 120.0 . . ?
C5A C6A H6A 120.0 . . ?
C7A C6A C5A 120.0 . . ?
C7A C6A H6A 120.0 . . ?
C6A C7A H7A 120.0 . . ?
C6A C7A C8A 120.0 . . ?
C8A C7A H7A 120.0 . . ?
C3A C8A H8A 120.0 . . ?
C7A C8A C3A 120.0 . . ?
C7A C8A H8A 120.0 . . ?
C4B C3B C1 120.8(4) . . ?
C4B C3B N8B 120.0 . . ?
N8B C3B C1 119.1(4) . . ?
C3B C4B H4B 120.0 . . ?
C3B C4B C5B 120.0 . . ?
C5B C4B H4B 120.0 . . ?
C4B C5B H5B 120.0 . . ?
C6B C5B C4B 120.0 . . ?
C6B C5B H5B 120.0 . . ?
C5B C6B H6B 120.0 . . ?
C5B C6B C7B 120.0 . . ?
C7B C6B H6B 120.0 . . ?
C6B C7B H7B 120.0 . . ?
N8B C7B C6B 120.0 . . ?
N8B C7B H7B 120.0 . . ?
C7B N8B C3B 120.0 . . ?

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 C15 C16 135.5(2) . . . . ?
C1 C2 C15 C20 -46.9(3) . . . . ?
C1 C2 C21 C22 -44.0(3) . . . . ?
C1 C2 C21 C26 136.8(2) . . . . ?
C1 C9 C10 C11 179.91(19) . . . . ?
C1 C9 C14 C13 -178.79(19) . . . . ?
C1 C3A N4B C5A 176.6(6) . . . . ?
C1 C3A C8A C7A -176.3(6) . . . . ?
C1 C3B C4B C5B -176.5(8) . . . . ?
C1 C3B N8B C7B 176.6(8) . . . . ?
C2 C1 C9 C10 -54.6(3) . . . . ?
C2 C1 C9 C14 126.5(2) . . . . ?
C2 C1 C3A N4B 134.2(3) . . . . ?
C2 C1 C3A C8A -49.4(5) . . . . ?
C2 C1 C3B C4B 135.8(3) . . . . ?
C2 C1 C3B N8B -40.8(7) . . . . ?
C2 C15 C16 C17 178.90(19) . . . . ?
C2 C15 C20 C19 -179.0(2) . . . . ?
C2 C21 C22 C23 178.69(19) . . . . ?
C2 C21 C26 C25 -178.81(19) . . . . ?
C9 C1 C2 C15 168.19(19) . . . . ?
C9 C1 C2 C21 -9.7(3) . . . . ?
C9 C1 C3A N4B -40.0(4) . . . . ?
C9 C1 C3A C8A 136.4(3) . . . . ?
C9 C1 C3B C4B -49.3(6) . . . . ?
C9 C1 C3B N8B 134.1(4) . . . . ?
C9 C10 C11 C12 -0.3(3) . . . . ?
C10 C9 C14 C13 2.3(3) . . . . ?
C10 C11 C12 C13 0.8(3) . . . . ?
C11 C12 C13 C14 0.4(3) . . . . ?
C12 C13 C14 C9 -1.9(3) . . . . ?
C14 C9 C10 C11 -1.2(3) . . . . ?
C15 C2 C21 C22 138.00(19) . . . . ?
C15 C2 C21 C26 -41.2(3) . . . . ?
C15 C16 C17 C18 -0.4(3) . . . . ?
C16 C15 C20 C19 -1.3(3) . . . . ?
C16 C17 C18 C19 -0.4(3) . . . . ?
C17 C18 C19 C20 0.3(3) . . . . ?
C18 C19 C20 C15 0.6(3) . . . . ?
C20 C15 C16 C17 1.2(3) . . . . ?
C21 C2 C15 C16 -46.5(2) . . . . ?
C21 C2 C15 C20 131.2(2) . . . . ?
C21 C22 C23 C24 0.8(3) . . . . ?
C22 C21 C26 C25 2.0(3) . . . . ?
C22 C23 C24 C25 0.6(3) . . . . ?
C23 C24 C25 C26 -0.8(3) . . . . ?
C24 C25 C26 C21 -0.5(3) . . . . ?
C26 C21 C22 C23 -2.1(3) . . . . ?
C3A C1 C2 C15 -5.4(4) . . . . ?
C3A C1 C2 C21 176.7(3) . . . . ?
C3A C1 C9 C10 119.7(3) . . . . ?
C3A C1 C9 C14 -59.2(4) . . . . ?
C3A N4B C5A C6A 0.0 . . . . ?
N4B C3A C8A C7A 0.0 . . . . ?
N4B C5A C6A C7A 0.0 . . . . ?
C5A C6A C7A C8A 0.0 . . . . ?
C6A C7A C8A C3A 0.0 . . . . ?
C8A C3A N4B C5A 0.0 . . . . ?
C3B C1 C2 C15 -17.2(5) . . . . ?
C3B C1 C2 C21 164.9(5) . . . . ?
C3B C1 C9 C10 130.6(4) . . . . ?
C3B C1 C9 C14 -48.3(5) . . . . ?
C3B C4B C5B C6B 0.0 . . . . ?
C4B C3B N8B C7B 0.0 . . . . ?
C4B C5B C6B C7B 0.0 . . . . ?
C5B C6B C7B N8B 0.0 . . . . ?
C6B C7B N8B C3B 0.0 . . . . ?
N8B C3B C4B C5B 0.0 . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'

_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            CCD-PXL-KAF2
