# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_gzhang91
_database_code_depnum_ccdc_archive 'CCDC 2171899'
loop_
_audit_author_name
_audit_author_address
'Guoqi Zhang'
;John Jay College, City University of New York
United States of America
;
_audit_update_record             
;
2022-05-10 deposited with the CCDC.	2022-06-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            GZ-479
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H21 F12 N5 P2'
_chemical_formula_weight         633.37

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.2706(3)
_cell_length_b                   9.6225(3)
_cell_length_c                   14.6054(5)
_cell_angle_alpha                88.2720(10)
_cell_angle_beta                 72.8160(10)
_cell_angle_gamma                83.8840(10)
_cell_volume                     1237.65(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9938
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      25.35

_exptl_crystal_description       Plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_F_000             640
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.289
_shelx_estimated_absorpt_T_min   0.944
_shelx_estimated_absorpt_T_max   0.972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.950
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21658
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.129
_diffrn_reflns_theta_max         25.383
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4545
_reflns_number_gt                3965
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0502P)²+1.0659P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4545
_refine_ls_number_parameters     363
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0376
_refine_ls_wR_factor_ref         0.1022
_refine_ls_wR_factor_gt          0.0973
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.002

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
P1 P 2.04710(6) -0.40309(6) 0.16469(4) 0.02764(15) Uani 1 1 d . . . . .
P2 P 1.36207(6) 0.07714(5) 0.29968(4) 0.02242(14) Uani 1 1 d . . . . .
F1 F 1.87400(15) -0.43427(15) 0.18794(10) 0.0401(3) Uani 1 1 d . . . . .
F2 F 2.21958(17) -0.37448(17) 0.13911(15) 0.0625(5) Uani 1 1 d . . . . .
F3 F 1.99528(17) -0.24781(14) 0.20357(11) 0.0460(4) Uani 1 1 d . . . . .
F4 F 2.09810(16) -0.55964(14) 0.12437(10) 0.0442(4) Uani 1 1 d . . . . .
F5 F 2.04473(19) -0.45805(16) 0.26886(11) 0.0493(4) Uani 1 1 d . . . . .
F6 F 2.0438(2) -0.35156(16) 0.06008(10) 0.0593(5) Uani 1 1 d . . . . .
F7 F 1.48962(14) -0.01563(14) 0.33528(9) 0.0354(3) Uani 1 1 d . . . . .
F8 F 1.49200(16) 0.15690(14) 0.22615(10) 0.0441(4) Uani 1 1 d . . . . .
F9 F 1.37874(16) -0.03788(15) 0.22022(10) 0.0439(4) Uani 1 1 d . . . . .
F10 F 1.23250(14) -0.00042(14) 0.37340(11) 0.0406(3) Uani 1 1 d . . . . .
F11 F 1.34805(15) 0.19148(15) 0.37921(10) 0.0396(3) Uani 1 1 d . . . . .
F12 F 1.23576(15) 0.16933(14) 0.26336(9) 0.0388(3) Uani 1 1 d . . . . .
N1 N 0.85300(18) 0.12752(17) 0.30866(11) 0.0207(3) Uani 1 1 d . . . . .
N2 N 0.17312(18) -0.08533(17) 0.82978(11) 0.0214(3) Uani 1 1 d . . . . .
N3 N 0.27241(18) 0.10456(17) 0.87068(11) 0.0215(4) Uani 1 1 d . . . . .
N4 N 0.37458(19) 0.30331(17) 0.89335(11) 0.0221(4) Uani 1 1 d . . . . .
N5 N 0.46003(18) 0.45342(17) 0.78360(12) 0.0217(4) Uani 1 1 d . . . . .
C1 C 0.3503(2) 0.3524(2) 0.58346(15) 0.0278(5) Uani 1 1 d . . . . .
H1A H 0.3132 0.4500 0.5760 0.042 Uiso 1 1 calc R U . . .
H1B H 0.3041 0.3219 0.6493 0.042 Uiso 1 1 calc R U . . .
H1C H 0.3231 0.2936 0.5388 0.042 Uiso 1 1 calc R U . . .
C2 C 0.5209(2) 0.3394(2) 0.56237(14) 0.0212(4) Uani 1 1 d . . . . .
C3 C 0.6117(2) 0.2435(2) 0.49449(13) 0.0211(4) Uani 1 1 d . . . . .
H3 H 0.5647 0.1889 0.4606 0.025 Uiso 1 1 calc R U . . .
C4 C 0.7690(2) 0.22488(19) 0.47448(13) 0.0197(4) Uani 1 1 d . . . . .
C5 C 0.8576(2) 0.1073(2) 0.40842(14) 0.0234(4) Uani 1 1 d . . . . .
H5A H 0.9646 0.0993 0.4091 0.028 Uiso 1 1 calc R U . . .
H5B H 0.8159 0.0184 0.4330 0.028 Uiso 1 1 calc R U . . .
C6 C 0.8131(2) 0.0344(2) 0.25830(14) 0.0215(4) Uani 1 1 d . . . . .
H6 H 0.7801 -0.0538 0.2809 0.026 Uiso 1 1 calc R U . . .
C7 C 0.2131(2) -0.0126(2) 0.90162(14) 0.0229(4) Uani 1 1 d . . . . .
C8 C 0.3116(2) 0.1777(2) 0.93338(14) 0.0231(4) Uani 1 1 d . . . . .
C9 C 0.4321(2) 0.3224(2) 0.79889(14) 0.0225(4) Uani 1 1 d . . . . .
H9 H 0.4497 0.2528 0.7510 0.027 Uiso 1 1 calc R U . . .
C10 C 0.5081(3) 0.5215(2) 0.68860(14) 0.0276(5) Uani 1 1 d . . . . .
H10A H 0.5734 0.5953 0.6913 0.033 Uiso 1 1 calc R U . . .
H10B H 0.4174 0.5665 0.6727 0.033 Uiso 1 1 calc R U . . .
C11 C 0.5939(2) 0.4178(2) 0.61121(13) 0.0214(4) Uani 1 1 d . . . . .
C12 C 1.0110(2) 0.2919(2) 0.50342(17) 0.0325(5) Uani 1 1 d . . . . .
H12A H 1.0608 0.3048 0.4350 0.049 Uiso 1 1 calc R U . . .
H12B H 1.0445 0.1989 0.5232 0.049 Uiso 1 1 calc R U . . .
H12C H 1.0378 0.3632 0.5403 0.049 Uiso 1 1 calc R U . . .
C13 C 0.8413(2) 0.3057(2) 0.52157(14) 0.0219(4) Uani 1 1 d . . . . .
C14 C 0.7509(2) 0.4009(2) 0.58957(14) 0.0229(4) Uani 1 1 d . . . . .
H14 H 0.7982 0.4566 0.6225 0.027 Uiso 1 1 calc R U . . .
C15 C 0.8948(2) 0.2421(2) 0.25148(15) 0.0249(4) Uani 1 1 d . . . . .
H15 H 0.9288 0.3238 0.2697 0.030 Uiso 1 1 calc R U . . .
C16 C 0.1217(2) -0.2166(2) 0.83507(15) 0.0251(4) Uani 1 1 d . . . . .
H16 H 0.1019 -0.2768 0.8891 0.030 Uiso 1 1 calc R U . . .
C17 C 0.1876(2) -0.0628(2) 0.99404(15) 0.0294(5) Uani 1 1 d . . . . .
H17 H 0.1436 -0.1478 1.0130 0.035 Uiso 1 1 calc R U . . .
C18 C 0.2293(3) 0.0169(2) 1.05772(15) 0.0326(5) Uani 1 1 d . . . . .
H18 H 0.2136 -0.0131 1.1222 0.039 Uiso 1 1 calc R U . . .
C19 C 0.2937(2) 0.1404(2) 1.02774(15) 0.0294(5) Uani 1 1 d . . . . .
H19 H 0.3239 0.1963 1.0700 0.035 Uiso 1 1 calc R U . . .
C20 C 0.4206(2) 0.5223(2) 0.87078(15) 0.0263(4) Uani 1 1 d . . . . .
H20 H 0.4299 0.6178 0.8802 0.032 Uiso 1 1 calc R U . . .
C21 C 0.3670(2) 0.4291(2) 0.93956(15) 0.0272(4) Uani 1 1 d . . . . .
H21 H 0.3309 0.4460 1.0066 0.033 Uiso 1 1 calc R U . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 F2 1.5833(15) . ?
P1 F3 1.5884(14) . ?
P1 F5 1.5903(15) . ?
P1 F1 1.5984(14) . ?
P1 F6 1.5999(15) . ?
P1 F4 1.6052(14) . ?
P2 F9 1.5908(13) . ?
P2 F11 1.5919(13) . ?
P2 F10 1.5929(14) . ?
P2 F12 1.5990(13) . ?
P2 F7 1.6049(13) . ?
P2 F8 1.6051(14) . ?
N1 C6 1.324(3) . ?
N1 C15 1.381(3) . ?
N1 C5 1.477(2) . ?
N2 C6 1.338(3) 2_656 ?
N2 C16 1.389(3) . ?
N2 C7 1.434(3) . ?
N3 C7 1.316(3) . ?
N3 C8 1.325(3) . ?
N4 C9 1.339(3) . ?
N4 C21 1.389(3) . ?
N4 C8 1.432(3) . ?
N5 C9 1.314(3) . ?
N5 C20 1.385(3) . ?
N5 C10 1.482(3) . ?
C1 C2 1.511(3) . ?
C2 C3 1.392(3) . ?
C2 C11 1.401(3) . ?
C3 C4 1.393(3) . ?
C4 C13 1.394(3) . ?
C4 C5 1.512(3) . ?
C6 N2 1.338(3) 2_656 ?
C7 C17 1.381(3) . ?
C8 C19 1.379(3) . ?
C10 C11 1.508(3) . ?
C11 C14 1.387(3) . ?
C12 C13 1.507(3) . ?
C13 C14 1.388(3) . ?
C15 C16 1.350(3) 2_656 ?
C16 C15 1.350(3) 2_656 ?
C17 C18 1.386(3) . ?
C18 C19 1.388(3) . ?
C20 C21 1.344(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F2 P1 F3 90.44(8) . . ?
F2 P1 F5 92.28(10) . . ?
F3 P1 F5 91.18(8) . . ?
F2 P1 F1 178.49(9) . . ?
F3 P1 F1 90.72(8) . . ?
F5 P1 F1 88.67(8) . . ?
F2 P1 F6 89.87(11) . . ?
F3 P1 F6 89.79(9) . . ?
F5 P1 F6 177.63(9) . . ?
F1 P1 F6 89.16(9) . . ?
F2 P1 F4 90.00(8) . . ?
F3 P1 F4 179.21(9) . . ?
F5 P1 F4 89.47(8) . . ?
F1 P1 F4 88.84(8) . . ?
F6 P1 F4 89.54(8) . . ?
F9 P2 F11 179.10(8) . . ?
F9 P2 F10 90.65(8) . . ?
F11 P2 F10 89.75(8) . . ?
F9 P2 F12 90.69(7) . . ?
F11 P2 F12 90.12(8) . . ?
F10 P2 F12 89.78(8) . . ?
F9 P2 F7 88.98(7) . . ?
F11 P2 F7 90.21(8) . . ?
F10 P2 F7 90.52(7) . . ?
F12 P2 F7 179.55(8) . . ?
F9 P2 F8 89.98(8) . . ?
F11 P2 F8 89.62(8) . . ?
F10 P2 F8 179.33(8) . . ?
F12 P2 F8 90.00(8) . . ?
F7 P2 F8 89.70(8) . . ?
C6 N1 C15 108.90(16) . . ?
C6 N1 C5 124.71(17) . . ?
C15 N1 C5 126.34(16) . . ?
C6 N2 C16 108.40(16) 2_656 . ?
C6 N2 C7 122.95(17) 2_656 . ?
C16 N2 C7 128.60(17) . . ?
C7 N3 C8 116.78(17) . . ?
C9 N4 C21 108.53(17) . . ?
C9 N4 C8 122.72(16) . . ?
C21 N4 C8 128.05(17) . . ?
C9 N5 C20 108.96(17) . . ?
C9 N5 C10 125.75(16) . . ?
C20 N5 C10 124.91(17) . . ?
C3 C2 C11 117.34(18) . . ?
C3 C2 C1 120.17(18) . . ?
C11 C2 C1 122.45(18) . . ?
C4 C3 C2 122.32(18) . . ?
C3 C4 C13 120.08(18) . . ?
C3 C4 C5 118.96(17) . . ?
C13 C4 C5 120.71(18) . . ?
N1 C5 C4 113.08(16) . . ?
N1 C6 N2 108.63(17) . 2_656 ?
N3 C7 C17 124.84(19) . . ?
N3 C7 N2 113.45(17) . . ?
C17 C7 N2 121.70(18) . . ?
N3 C8 C19 124.91(19) . . ?
N3 C8 N4 112.76(17) . . ?
C19 C8 N4 122.33(18) . . ?
N5 C9 N4 108.57(17) . . ?
N5 C10 C11 111.55(16) . . ?
C14 C11 C2 120.09(18) . . ?
C14 C11 C10 117.42(18) . . ?
C2 C11 C10 122.49(18) . . ?
C14 C13 C4 117.63(18) . . ?
C14 C13 C12 119.25(18) . . ?
C4 C13 C12 123.11(18) . . ?
C13 C14 C11 122.50(18) . . ?
C16 C15 N1 107.32(18) 2_656 . ?
C15 C16 N2 106.76(18) 2_656 . ?
C7 C17 C18 116.7(2) . . ?
C19 C18 C17 120.3(2) . . ?
C8 C19 C18 116.46(19) . . ?
C21 C20 N5 107.40(18) . . ?
C20 C21 N4 106.54(18) . . ?

_refine_diff_density_max         0.559
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.066

_shelxl_version_number           2013-3

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

data_JF2587PT83FMI
_database_code_depnum_ccdc_archive 'CCDC 2171900'
loop_
_audit_author_name
_audit_author_address
'Guoqi Zhang'
;John Jay College, City University of New York
United States of America
;
_audit_update_record             
;
2022-06-18 deposited with the CCDC.	2022-06-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C78 H66 N10), 4(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C84 H75 F24 N13 P4'
_chemical_formula_weight         1846.45

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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.9230(3)
_cell_length_b                   12.4296(3)
_cell_length_c                   18.4932(6)
_cell_angle_alpha                82.9900(18)
_cell_angle_beta                 87.0124(19)
_cell_angle_gamma                85.1082(17)
_cell_volume                     2026.52(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6982
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      67.08

_exptl_crystal_description       Rod
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_F_000             946
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.047
_exptl_absorpt_coefficient_mu    1.842
_shelx_estimated_absorpt_T_min   0.747
_shelx_estimated_absorpt_T_max   0.918
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7892
_exptl_absorpt_correction_T_max  0.8850
_exptl_absorpt_process_details   'SADABS 2016/2 (Sheldrick, 2016)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Photon100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8389
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.409
_diffrn_reflns_theta_max         68.070
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.691
_diffrn_measured_fraction_theta_full 0.698
_diffrn_reflns_Laue_measured_fraction_max 0.691
_diffrn_reflns_Laue_measured_fraction_full 0.698
_diffrn_reflns_point_group_measured_fraction_max 0.691
_diffrn_reflns_point_group_measured_fraction_full 0.698
_reflns_number_total             5112
_reflns_number_gt                3336
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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. 
;

_computing_data_collection       'Apex3 (2016.9) (Bruker, 2016)'
_computing_cell_refinement       'SAINT (8.38a) (Bruker, 2017)'
_computing_data_reduction        'SAINT (8.38a) (Bruker, 2017)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
?
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0718P)²+1.3728P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5112
_refine_ls_number_parameters     667
_refine_ls_number_restraints     111
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0555
_refine_ls_wR_factor_ref         0.1461
_refine_ls_wR_factor_gt          0.1275
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.3100(4) 0.4374(3) 0.4561(2) 0.0336(11) Uani 1 1 d . . . . .
N1 N 0.2223(4) 0.4782(3) 0.50936(17) 0.0343(9) Uani 1 1 d . . . . .
C2 C 0.3161(5) 0.3289(3) 0.4464(2) 0.0444(12) Uani 1 1 d . . . . .
H2 H 0.379429 0.302001 0.408587 0.053 Uiso 1 1 calc R U . . .
C3 C 0.2290(6) 0.2585(4) 0.4920(3) 0.0603(15) Uani 1 1 d . . . . .
C4 C 0.1363(5) 0.3031(4) 0.5447(3) 0.0525(14) Uani 1 1 d . . . . .
H4 H 0.072318 0.258487 0.575604 0.063 Uiso 1 1 calc R U . . .
C5 C 0.1363(5) 0.4117(3) 0.5527(2) 0.0363(11) Uani 1 1 d . . . . .
C6 C 0.263(2) 1.1406(12) 0.5012(6) 0.071(5) Uani 0.5 1 d . U P A -1
C7 C 0.156(3) 1.0698(14) 0.5347(6) 0.058(3) Uani 0.5 1 d . U P A -1
H7 H 0.062632 1.099308 0.553940 0.069 Uiso 0.5 1 calc R U P A -1
C8 C 0.187(3) 0.9568(13) 0.5396(7) 0.067(3) Uani 0.5 1 d . U P A -1
H8 H 0.116210 0.910049 0.563503 0.080 Uiso 0.5 1 calc R U P A -1
C9 C 0.3251(12) 0.9120(8) 0.5088(5) 0.056(3) Uani 0.5 1 d . . P A -1
H9 H 0.344127 0.835348 0.510420 0.067 Uiso 0.5 1 calc R U P A -1
C10 C 0.4289(12) 0.9783(8) 0.4772(5) 0.060(3) Uani 0.5 1 d . . P A -1
H10 H 0.520804 0.947459 0.457475 0.072 Uiso 0.5 1 calc R U P A -1
C11 C 0.4034(11) 1.0906(7) 0.4732(5) 0.058(3) Uani 0.5 1 d . . P A -1
H11 H 0.479067 1.135330 0.451874 0.069 Uiso 0.5 1 calc R U P A -1
C6B C 0.2181(19) 1.1400(8) 0.4694(5) 0.076(5) Uani 0.5 1 d G U P B -2
C7B C 0.190(3) 1.0601(11) 0.5268(4) 0.058(3) Uani 0.5 1 d G U P B -2
H7B H 0.171980 1.079219 0.574866 0.069 Uiso 0.5 1 calc R U P B -2
C8B C 0.188(2) 0.9524(9) 0.5139(6) 0.068(3) Uani 0.5 1 d G U P B -2
H8B H 0.169170 0.897860 0.553130 0.082 Uiso 0.5 1 calc R U P B -2
C9B C 0.2147(12) 0.9245(6) 0.4435(7) 0.106(5) Uani 0.5 1 d G . P B -2
H9B H 0.213599 0.850861 0.434724 0.128 Uiso 0.5 1 calc R U P B -2
C10B C 0.2428(10) 1.0043(6) 0.3861(5) 0.095(4) Uani 0.5 1 d G . P B -2
H10B H 0.260839 0.985219 0.338052 0.114 Uiso 0.5 1 calc R U P B -2
C11B C 0.2445(10) 1.1120(6) 0.3990(4) 0.066(3) Uani 0.5 1 d G . P B -2
H11B H 0.263650 1.166579 0.359786 0.079 Uiso 0.5 1 calc R U P B -2
C12 C 0.4033(4) 0.5149(3) 0.4110(2) 0.0304(10) Uani 1 1 d . . . . .
C13 C 0.3878(5) 0.6243(3) 0.4199(2) 0.0463(12) Uani 1 1 d . . . . .
H13 H 0.315838 0.648837 0.455219 0.056 Uiso 1 1 calc R U . . .
C14 C 0.4735(5) 0.6986(3) 0.3792(2) 0.0465(12) Uani 1 1 d . . . . .
H14 H 0.460021 0.773281 0.386223 0.056 Uiso 1 1 calc R U . . .
C15 C 0.5786(4) 0.6641(3) 0.3284(2) 0.0318(10) Uani 1 1 d . . . . .
N15 N 0.6718(4) 0.7403(2) 0.28709(17) 0.0325(9) Uani 1 1 d . . . . .
C16 C 0.5962(5) 0.5563(3) 0.3179(2) 0.0427(12) Uani 1 1 d . . . . .
H16 H 0.668485 0.532266 0.282586 0.051 Uiso 1 1 calc R U . . .
C17 C 0.5092(5) 0.4833(3) 0.3586(2) 0.0432(12) Uani 1 1 d . . . . .
H17 H 0.521951 0.408965 0.350579 0.052 Uiso 1 1 calc R U . . .
C18 C 0.7644(4) 0.7212(3) 0.2308(2) 0.0344(11) Uani 1 1 d . . . . .
H18 H 0.778998 0.654147 0.210614 0.041 Uiso 1 1 calc R U . . .
N18 N 0.8335(4) 0.8096(3) 0.20709(18) 0.0362(9) Uani 1 1 d . . . . .
C19 C 0.6829(5) 0.8467(3) 0.2993(2) 0.0465(12) Uani 1 1 d . . . . .
H19 H 0.628993 0.883261 0.335996 0.056 Uiso 1 1 calc R U . . .
C20 C 0.7841(5) 0.8893(3) 0.2495(2) 0.0527(14) Uani 1 1 d . . . . .
H20 H 0.815220 0.961143 0.244831 0.063 Uiso 1 1 calc R U . . .
C21 C 0.9445(5) 0.8181(3) 0.1443(2) 0.0455(12) Uani 1 1 d . . . . .
H21A H 0.899418 0.795458 0.101275 0.055 Uiso 1 1 calc R U . . .
H21B H 1.034110 0.767602 0.156052 0.055 Uiso 1 1 calc R U . . .
C22 C 0.9925(5) 0.9308(3) 0.1256(2) 0.0338(11) Uani 1 1 d . . . . .
C23 C 0.8991(5) 1.0118(4) 0.0889(2) 0.0385(12) Uani 1 1 d . . . . .
C24 C 0.9530(6) 1.1130(4) 0.0697(2) 0.0451(12) Uani 1 1 d . . . . .
H24 H 0.889481 1.169350 0.044931 0.054 Uiso 1 1 calc R U . . .
C25 C 1.0957(6) 1.1345(4) 0.0854(2) 0.0420(12) Uani 1 1 d . . . . .
C26 C 1.1913(5) 1.0551(4) 0.1232(3) 0.0514(13) Uani 1 1 d . . . . .
C27 C 1.1351(5) 0.9527(4) 0.1425(3) 0.0476(13) Uani 1 1 d . . . . .
H27 H 1.197446 0.896444 0.168087 0.057 Uiso 1 1 calc R U . . .
C28 C 0.7399(5) 0.9935(4) 0.0697(3) 0.0540(13) Uani 1 1 d . . . . .
H28A H 0.672715 0.995423 0.113289 0.081 Uiso 1 1 calc R U . . .
H28B H 0.739841 0.922510 0.051802 0.081 Uiso 1 1 calc R U . . .
H28C H 0.704756 1.050818 0.031823 0.081 Uiso 1 1 calc R U . . .
C29 C 1.3481(5) 1.0741(4) 0.1387(4) 0.0854(19) Uani 1 1 d . . . . .
H29A H 1.405562 1.090634 0.092581 0.128 Uiso 1 1 calc R U . . .
H29B H 1.395484 1.008762 0.166182 0.128 Uiso 1 1 calc R U . . .
H29C H 1.346771 1.135486 0.167360 0.128 Uiso 1 1 calc R U . . .
C30 C 1.1511(6) 1.2437(4) 0.0570(2) 0.0552(14) Uani 1 1 d . . . . .
H30A H 1.241917 1.232420 0.024825 0.066 Uiso 1 1 calc R U . . .
H30B H 1.072723 1.286297 0.027172 0.066 Uiso 1 1 calc R U . . .
N30 N 1.1886(4) 1.3075(3) 0.11600(19) 0.0476(10) Uani 1 1 d . . . . .
C31 C 1.1013(5) 1.3250(3) 0.1742(2) 0.0445(12) Uani 1 1 d . . . . .
H31 H 1.009676 1.292838 0.188123 0.053 Uiso 1 1 calc R U . . .
N31 N 1.1642(4) 1.3955(3) 0.21005(18) 0.0356(9) Uani 1 1 d . . . . .
C32 C 1.3101(5) 1.3691(3) 0.1144(3) 0.0477(13) Uani 1 1 d . . . . .
H32 H 1.390713 1.371629 0.078793 0.057 Uiso 1 1 calc R U . . .
C33 C 1.2940(5) 1.4245(3) 0.1719(3) 0.0488(13) Uani 1 1 d . . . . .
H33 H 1.359964 1.474767 0.184357 0.059 Uiso 1 1 calc R U . . .
C34 C 1.0961(4) 1.4425(3) 0.2726(2) 0.0332(11) Uani 1 1 d . . . . .
C35 C 1.0065(5) 1.3818(4) 0.3220(2) 0.0410(11) Uani 1 1 d . . . . .
H35 H 0.994484 1.307850 0.316990 0.049 Uiso 1 1 calc R U . . .
C36 C 0.9349(5) 1.4304(3) 0.3788(2) 0.0435(12) Uani 1 1 d . . . . .
H36 H 0.872668 1.389251 0.412973 0.052 Uiso 1 1 calc R U . . .
C37 C 0.9513(4) 1.5380(3) 0.3872(2) 0.0314(10) Uani 1 1 d . . . . .
C38 C 1.0461(4) 1.5961(3) 0.3379(2) 0.0367(11) Uani 1 1 d . . . . .
H38 H 1.062298 1.668872 0.344160 0.044 Uiso 1 1 calc R U . . .
C39 C 1.1171(5) 1.5491(3) 0.2799(2) 0.0376(11) Uani 1 1 d . . . . .
H39 H 1.179570 1.589780 0.245588 0.045 Uiso 1 1 calc R U . . .
P41 P 0.46139(13) 0.70904(10) 0.09507(7) 0.0444(4) Uani 1 1 d . . . . .
F41 F 0.6380(3) 0.7187(2) 0.08527(13) 0.0659(8) Uani 1 1 d D . . . .
F42 F 0.2954(7) 0.6866(5) 0.1163(3) 0.054(2) Uani 0.63 1 d D U P C 1
F43 F 0.5125(6) 0.6066(4) 0.1596(3) 0.0596(18) Uani 0.63 1 d D . P C 1
F44 F 0.4590(5) 0.7838(5) 0.1621(3) 0.0659(17) Uani 0.63 1 d D . P C 1
F45 F 0.4210(6) 0.8051(5) 0.0424(4) 0.0860(18) Uani 0.63 1 d D . P C 1
F46 F 0.4721(9) 0.6269(7) 0.0384(4) 0.081(4) Uani 0.63 1 d D . P C 1
F42B F 0.2729(15) 0.7182(10) 0.0827(5) 0.052(3) Uani 0.37 1 d D U P C 2
F43B F 0.4464(14) 0.6664(9) 0.1691(5) 0.083(4) Uani 0.37 1 d D . P C 2
F44B F 0.4487(10) 0.8293(7) 0.1072(8) 0.077(3) Uani 0.37 1 d D . P C 2
F45B F 0.4627(9) 0.7532(8) 0.0013(4) 0.057(2) Uani 0.37 1 d D . P C 2
F46B F 0.4684(18) 0.5916(12) 0.0659(7) 0.053(4) Uani 0.37 1 d D . P C 2
P51 P 0.66951(15) 0.21128(10) 0.26430(7) 0.0550(4) Uani 1 1 d . . . . .
F51 F 0.6253(3) 0.0943(2) 0.29859(17) 0.0780(9) Uani 1 1 d . . . . .
F52 F 0.7158(3) 0.3288(2) 0.23076(14) 0.0706(8) Uani 1 1 d . . . . .
F53 F 0.8427(3) 0.1651(2) 0.25591(16) 0.0727(9) Uani 1 1 d . . . . .
F54 F 0.4975(3) 0.2567(2) 0.27273(15) 0.0676(8) Uani 1 1 d . . . . .
F55 F 0.6982(3) 0.24125(19) 0.34329(13) 0.0598(8) Uani 1 1 d . . . . .
F56 F 0.6428(3) 0.1824(2) 0.18510(15) 0.0857(10) Uani 1 1 d . . . . .
N61 N 0.0558(5) 0.4477(3) 0.8960(2) 0.0670(13) Uani 1 1 d . . . . .
C61 C 0.1376(6) 0.5018(4) 0.9172(3) 0.0492(13) Uani 1 1 d . . . . .
C62 C 0.2381(5) 0.5710(4) 0.9437(3) 0.0566(14) Uani 1 1 d . . . . .
H62A H 0.198666 0.592123 0.990791 0.085 Uiso 1 1 calc R U . . .
H62B H 0.246579 0.636322 0.908644 0.085 Uiso 1 1 calc R U . . .
H62C H 0.337611 0.531914 0.949560 0.085 Uiso 1 1 calc R U . . .
N71 N 0.1251(9) 0.8639(6) 0.3320(4) 0.053(2) Uani 0.5 1 d . . P D 1
C71 C 0.1554(10) 0.9502(8) 0.3254(5) 0.045(2) Uani 0.5 1 d . . P D 1
C72 C 0.1918(12) 1.0635(8) 0.3169(6) 0.063(3) Uani 0.5 1 d . . P D 1
H72A H 0.149189 1.101429 0.272065 0.095 Uiso 0.5 1 calc R U P D 1
H72B H 0.301362 1.066417 0.313997 0.095 Uiso 0.5 1 calc R U P D 1
H72C H 0.149223 1.098635 0.358810 0.095 Uiso 0.5 1 calc R U P D 1


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.347(5) . ?
C1 C2 1.379(5) . ?
C1 C12 1.479(5) . ?
N1 C5 1.340(5) . ?
C2 C3 1.395(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.383(6) . ?
C4 C5 1.376(5) . ?
C4 H4 0.9500 . ?
C5 C37 1.494(5) 2_676 ?
C6 C7 1.420(16) . ?
C6 C11 1.451(19) . ?
C7 C8 1.401(14) . ?
C7 H7 0.9500 . ?
C8 C9 1.43(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.355(12) . ?
C9 H9 0.9500 . ?
C10 C11 1.388(12) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C6B C7B 1.3900 . ?
C6B C11B 1.3900 . ?
C7B C8B 1.3900 . ?
C7B H7B 0.9500 . ?
C8B C9B 1.3900 . ?
C8B H8B 0.9500 . ?
C9B C10B 1.3900 . ?
C9B H9B 0.9500 . ?
C10B C11B 1.3900 . ?
C10B H10B 0.9500 . ?
C11B H11B 0.9500 . ?
C12 C13 1.383(5) . ?
C12 C17 1.386(5) . ?
C13 C14 1.377(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.373(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.372(5) . ?
C15 N15 1.436(5) . ?
N15 C18 1.327(5) . ?
N15 C19 1.382(5) . ?
C16 C17 1.373(5) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 N18 1.322(5) . ?
C18 H18 0.9500 . ?
N18 C20 1.368(5) . ?
N18 C21 1.486(5) . ?
C19 C20 1.349(5) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C22 1.495(5) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C27 1.383(6) . ?
C22 C23 1.385(6) . ?
C23 C24 1.384(6) . ?
C23 C28 1.524(6) . ?
C24 C25 1.376(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.393(6) . ?
C25 C30 1.509(6) . ?
C26 C27 1.406(6) . ?
C26 C29 1.487(6) . ?
C27 H27 0.9500 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 N30 1.493(5) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
N30 C31 1.324(5) . ?
N30 C32 1.376(5) . ?
C31 N31 1.337(5) . ?
C31 H31 0.9500 . ?
N31 C33 1.376(5) . ?
N31 C34 1.442(5) . ?
C32 C33 1.331(6) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
C34 C39 1.377(5) . ?
C34 C35 1.380(5) . ?
C35 C36 1.377(5) . ?
C35 H35 0.9500 . ?
C36 C37 1.387(5) . ?
C36 H36 0.9500 . ?
C37 C38 1.389(5) . ?
C38 C39 1.383(5) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
P41 F43B 1.410(9) . ?
P41 F45 1.477(4) . ?
P41 F44B 1.533(8) . ?
P41 F46 1.544(7) . ?
P41 F42 1.552(7) . ?
P41 F41 1.590(3) . ?
P41 F46B 1.611(14) . ?
P41 F44 1.636(5) . ?
P41 F43 1.685(5) . ?
P41 F42B 1.701(13) . ?
P41 F45B 1.754(8) . ?
P51 F56 1.584(3) . ?
P51 F51 1.587(3) . ?
P51 F55 1.589(3) . ?
P51 F52 1.595(3) . ?
P51 F54 1.596(3) . ?
P51 F53 1.608(3) . ?
N61 C61 1.147(6) . ?
C61 C62 1.437(7) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
N71 C71 1.120(10) . ?
C71 C72 1.460(13) . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 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
N1 C1 C2 121.6(4) . . ?
N1 C1 C12 116.0(4) . . ?
C2 C1 C12 122.3(4) . . ?
C5 N1 C1 118.9(3) . . ?
C1 C2 C3 120.0(4) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 H2 120.0 . . ?
C4 C3 C2 117.2(4) . . ?
C5 C4 C3 120.3(4) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
N1 C5 C4 121.9(4) . . ?
N1 C5 C37 115.4(4) . 2_676 ?
C4 C5 C37 122.5(4) . 2_676 ?
C7 C6 C11 117.1(11) . . ?
C8 C7 C6 120.5(12) . . ?
C8 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C7 C8 C9 120.0(11) . . ?
C7 C8 H8 120.0 . . ?
C9 C8 H8 120.0 . . ?
C10 C9 C8 120.2(10) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C9 C10 C11 121.2(9) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
C10 C11 C6 120.9(9) . . ?
C10 C11 H11 119.6 . . ?
C6 C11 H11 119.6 . . ?
C7B C6B C11B 120.0 . . ?
C6B C7B C8B 120.0 . . ?
C6B C7B H7B 120.0 . . ?
C8B C7B H7B 120.0 . . ?
C7B C8B C9B 120.0 . . ?
C7B C8B H8B 120.0 . . ?
C9B C8B H8B 120.0 . . ?
C10B C9B C8B 120.0 . . ?
C10B C9B H9B 120.0 . . ?
C8B C9B H9B 120.0 . . ?
C11B C10B C9B 120.0 . . ?
C11B C10B H10B 120.0 . . ?
C9B C10B H10B 120.0 . . ?
C10B C11B C6B 120.0 . . ?
C10B C11B H11B 120.0 . . ?
C6B C11B H11B 120.0 . . ?
C13 C12 C17 116.8(4) . . ?
C13 C12 C1 120.4(4) . . ?
C17 C12 C1 122.8(4) . . ?
C14 C13 C12 121.9(4) . . ?
C14 C13 H13 119.0 . . ?
C12 C13 H13 119.0 . . ?
C15 C14 C13 119.7(4) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C16 C15 C14 119.8(4) . . ?
C16 C15 N15 120.0(4) . . ?
C14 C15 N15 120.2(3) . . ?
C18 N15 C19 107.3(3) . . ?
C18 N15 C15 126.4(3) . . ?
C19 N15 C15 126.3(3) . . ?
C15 C16 C17 119.8(4) . . ?
C15 C16 H16 120.1 . . ?
C17 C16 H16 120.1 . . ?
C16 C17 C12 121.9(4) . . ?
C16 C17 H17 119.1 . . ?
C12 C17 H17 119.1 . . ?
N18 C18 N15 109.7(3) . . ?
N18 C18 H18 125.2 . . ?
N15 C18 H18 125.2 . . ?
C18 N18 C20 108.4(3) . . ?
C18 N18 C21 124.5(3) . . ?
C20 N18 C21 127.1(3) . . ?
C20 C19 N15 107.5(4) . . ?
C20 C19 H19 126.2 . . ?
N15 C19 H19 126.2 . . ?
C19 C20 N18 107.1(4) . . ?
C19 C20 H20 126.5 . . ?
N18 C20 H20 126.5 . . ?
N18 C21 C22 112.5(3) . . ?
N18 C21 H21A 109.1 . . ?
C22 C21 H21A 109.1 . . ?
N18 C21 H21B 109.1 . . ?
C22 C21 H21B 109.1 . . ?
H21A C21 H21B 107.8 . . ?
C27 C22 C23 119.8(4) . . ?
C27 C22 C21 119.1(4) . . ?
C23 C22 C21 121.0(4) . . ?
C24 C23 C22 118.3(4) . . ?
C24 C23 C28 119.3(4) . . ?
C22 C23 C28 122.4(4) . . ?
C25 C24 C23 122.0(4) . . ?
C25 C24 H24 119.0 . . ?
C23 C24 H24 119.0 . . ?
C24 C25 C26 121.0(4) . . ?
C24 C25 C30 118.8(5) . . ?
C26 C25 C30 120.1(4) . . ?
C25 C26 C27 116.5(4) . . ?
C25 C26 C29 122.4(5) . . ?
C27 C26 C29 121.1(5) . . ?
C22 C27 C26 122.5(4) . . ?
C22 C27 H27 118.8 . . ?
C26 C27 H27 118.8 . . ?
C23 C28 H28A 109.5 . . ?
C23 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C23 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N30 C30 C25 113.3(4) . . ?
N30 C30 H30A 108.9 . . ?
C25 C30 H30A 108.9 . . ?
N30 C30 H30B 108.9 . . ?
C25 C30 H30B 108.9 . . ?
H30A C30 H30B 107.7 . . ?
C31 N30 C32 108.5(4) . . ?
C31 N30 C30 125.5(4) . . ?
C32 N30 C30 125.5(3) . . ?
N30 C31 N31 108.3(4) . . ?
N30 C31 H31 125.9 . . ?
N31 C31 H31 125.9 . . ?
C31 N31 C33 108.2(3) . . ?
C31 N31 C34 125.0(3) . . ?
C33 N31 C34 126.4(4) . . ?
C33 C32 N30 107.5(4) . . ?
C33 C32 H32 126.2 . . ?
N30 C32 H32 126.2 . . ?
C32 C33 N31 107.4(4) . . ?
C32 C33 H33 126.3 . . ?
N31 C33 H33 126.3 . . ?
C39 C34 C35 121.4(4) . . ?
C39 C34 N31 119.0(4) . . ?
C35 C34 N31 119.6(4) . . ?
C36 C35 C34 118.6(4) . . ?
C36 C35 H35 120.7 . . ?
C34 C35 H35 120.7 . . ?
C35 C36 C37 121.6(4) . . ?
C35 C36 H36 119.2 . . ?
C37 C36 H36 119.2 . . ?
C36 C37 C38 118.4(4) . . ?
C36 C37 C5 119.1(4) . 2_676 ?
C38 C37 C5 122.4(4) . 2_676 ?
C39 C38 C37 120.8(4) . . ?
C39 C38 H38 119.6 . . ?
C37 C38 H38 119.6 . . ?
C34 C39 C38 119.1(4) . . ?
C34 C39 H39 120.4 . . ?
C38 C39 H39 120.4 . . ?
F43B P41 F44B 96.8(6) . . ?
F45 P41 F46 95.2(5) . . ?
F45 P41 F42 94.1(3) . . ?
F46 P41 F42 91.7(3) . . ?
F43B P41 F41 101.6(5) . . ?
F45 P41 F41 95.1(2) . . ?
F44B P41 F41 86.5(3) . . ?
F46 P41 F41 89.9(3) . . ?
F42 P41 F41 170.4(2) . . ?
F43B P41 F46B 94.1(6) . . ?
F44B P41 F46B 168.7(8) . . ?
F41 P41 F46B 94.4(6) . . ?
F45 P41 F44 91.7(4) . . ?
F46 P41 F44 172.9(4) . . ?
F42 P41 F44 88.9(3) . . ?
F41 P41 F44 88.3(2) . . ?
F45 P41 F43 175.3(4) . . ?
F46 P41 F43 89.2(4) . . ?
F42 P41 F43 87.5(2) . . ?
F41 P41 F43 83.1(2) . . ?
F44 P41 F43 83.8(3) . . ?
F43B P41 F42B 93.7(6) . . ?
F44B P41 F42B 89.2(6) . . ?
F41 P41 F42B 164.5(4) . . ?
F46B P41 F42B 87.0(6) . . ?
F43B P41 F45B 173.4(5) . . ?
F44B P41 F45B 87.1(6) . . ?
F41 P41 F45B 84.0(3) . . ?
F46B P41 F45B 81.8(5) . . ?
F42B P41 F45B 80.9(4) . . ?
F56 P51 F51 90.40(17) . . ?
F56 P51 F55 179.17(17) . . ?
F51 P51 F55 90.29(16) . . ?
F56 P51 F52 90.31(16) . . ?
F51 P51 F52 179.13(19) . . ?
F55 P51 F52 89.00(14) . . ?
F56 P51 F54 90.50(16) . . ?
F51 P51 F54 89.63(15) . . ?
F55 P51 F54 89.96(14) . . ?
F52 P51 F54 90.88(16) . . ?
F56 P51 F53 89.49(15) . . ?
F51 P51 F53 90.18(15) . . ?
F55 P51 F53 90.05(16) . . ?
F52 P51 F53 89.32(15) . . ?
F54 P51 F53 179.80(19) . . ?
N61 C61 C62 179.1(5) . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
N71 C71 C72 178.9(10) . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 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
C2 C1 N1 C5 -1.5(6) . . . . ?
C12 C1 N1 C5 -179.3(3) . . . . ?
N1 C1 C2 C3 0.4(7) . . . . ?
C12 C1 C2 C3 178.0(4) . . . . ?
C1 C2 C3 C4 1.6(7) . . . . ?
C2 C3 C4 C5 -2.5(7) . . . . ?
C1 N1 C5 C4 0.6(6) . . . . ?
C1 N1 C5 C37 176.9(3) . . . 2_676 ?
C3 C4 C5 N1 1.5(7) . . . . ?
C3 C4 C5 C37 -174.6(4) . . . 2_676 ?
C11 C6 C7 C8 -0.3(9) . . . . ?
C6 C7 C8 C9 -2.0(10) . . . . ?
C7 C8 C9 C10 2.6(16) . . . . ?
C8 C9 C10 C11 -0.8(17) . . . . ?
C9 C10 C11 C6 -1.6(15) . . . . ?
C7 C6 C11 C10 2.1(14) . . . . ?
C11B C6B C7B C8B 0.0 . . . . ?
C6B C7B C8B C9B 0.0 . . . . ?
C7B C8B C9B C10B 0.0 . . . . ?
C8B C9B C10B C11B 0.0 . . . . ?
C9B C10B C11B C6B 0.0 . . . . ?
C7B C6B C11B C10B 0.0 . . . . ?
N1 C1 C12 C13 -5.9(6) . . . . ?
C2 C1 C12 C13 176.4(4) . . . . ?
N1 C1 C12 C17 174.0(4) . . . . ?
C2 C1 C12 C17 -3.7(6) . . . . ?
C17 C12 C13 C14 -0.3(7) . . . . ?
C1 C12 C13 C14 179.5(4) . . . . ?
C12 C13 C14 C15 -0.4(7) . . . . ?
C13 C14 C15 C16 0.8(7) . . . . ?
C13 C14 C15 N15 -178.1(4) . . . . ?
C16 C15 N15 C18 9.6(6) . . . . ?
C14 C15 N15 C18 -171.5(4) . . . . ?
C16 C15 N15 C19 -169.5(4) . . . . ?
C14 C15 N15 C19 9.4(6) . . . . ?
C14 C15 C16 C17 -0.3(7) . . . . ?
N15 C15 C16 C17 178.6(4) . . . . ?
C15 C16 C17 C12 -0.5(7) . . . . ?
C13 C12 C17 C16 0.8(6) . . . . ?
C1 C12 C17 C16 -179.1(4) . . . . ?
C19 N15 C18 N18 0.2(5) . . . . ?
C15 N15 C18 N18 -179.1(3) . . . . ?
N15 C18 N18 C20 0.0(5) . . . . ?
N15 C18 N18 C21 -179.5(4) . . . . ?
C18 N15 C19 C20 -0.4(5) . . . . ?
C15 N15 C19 C20 178.9(4) . . . . ?
N15 C19 C20 N18 0.4(5) . . . . ?
C18 N18 C20 C19 -0.3(5) . . . . ?
C21 N18 C20 C19 179.2(4) . . . . ?
C18 N18 C21 C22 174.4(4) . . . . ?
C20 N18 C21 C22 -5.0(6) . . . . ?
N18 C21 C22 C27 106.9(4) . . . . ?
N18 C21 C22 C23 -76.0(5) . . . . ?
C27 C22 C23 C24 0.5(6) . . . . ?
C21 C22 C23 C24 -176.6(3) . . . . ?
C27 C22 C23 C28 -179.0(4) . . . . ?
C21 C22 C23 C28 3.9(6) . . . . ?
C22 C23 C24 C25 0.6(6) . . . . ?
C28 C23 C24 C25 -179.9(4) . . . . ?
C23 C24 C25 C26 -1.6(6) . . . . ?
C23 C24 C25 C30 174.7(3) . . . . ?
C24 C25 C26 C27 1.5(6) . . . . ?
C30 C25 C26 C27 -174.8(4) . . . . ?
C24 C25 C26 C29 177.6(4) . . . . ?
C30 C25 C26 C29 1.3(7) . . . . ?
C23 C22 C27 C26 -0.6(6) . . . . ?
C21 C22 C27 C26 176.6(4) . . . . ?
C25 C26 C27 C22 -0.4(6) . . . . ?
C29 C26 C27 C22 -176.6(4) . . . . ?
C24 C25 C30 N30 118.9(4) . . . . ?
C26 C25 C30 N30 -64.8(5) . . . . ?
C25 C30 N30 C31 -48.8(6) . . . . ?
C25 C30 N30 C32 139.8(4) . . . . ?
C32 N30 C31 N31 -0.3(5) . . . . ?
C30 N30 C31 N31 -172.9(4) . . . . ?
N30 C31 N31 C33 1.1(5) . . . . ?
N30 C31 N31 C34 173.9(3) . . . . ?
C31 N30 C32 C33 -0.6(5) . . . . ?
C30 N30 C32 C33 172.0(4) . . . . ?
N30 C32 C33 N31 1.3(5) . . . . ?
C31 N31 C33 C32 -1.5(5) . . . . ?
C34 N31 C33 C32 -174.2(4) . . . . ?
C31 N31 C34 C39 -143.1(4) . . . . ?
C33 N31 C34 C39 28.5(6) . . . . ?
C31 N31 C34 C35 34.3(6) . . . . ?
C33 N31 C34 C35 -154.2(4) . . . . ?
C39 C34 C35 C36 1.4(6) . . . . ?
N31 C34 C35 C36 -175.9(4) . . . . ?
C34 C35 C36 C37 -0.2(7) . . . . ?
C35 C36 C37 C38 -1.8(6) . . . . ?
C35 C36 C37 C5 176.4(4) . . . 2_676 ?
C36 C37 C38 C39 2.8(6) . . . . ?
C5 C37 C38 C39 -175.3(4) 2_676 . . . ?
C35 C34 C39 C38 -0.4(6) . . . . ?
N31 C34 C39 C38 176.9(4) . . . . ?
C37 C38 C39 C34 -1.8(6) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C20 H20 F51 0.95 2.52 3.022(5) 113. 1_565 yes
C21 H21B F42B 0.99 2.54 3.287(13) 132. 1_655 yes
C30 H30A F41 0.99 2.29 3.164(5) 147. 2_775 yes
C31 H31 F53 0.95 2.46 3.353(5) 157. 1_565 yes
C32 H32 F46 0.95 2.43 3.343(9) 161. 2_775 yes
C32 H32 F45B 0.95 2.51 3.289(9) 139. 2_775 yes
C33 H33 F43 0.95 2.21 3.092(7) 154. 1_665 yes
C33 H33 F43B 0.95 2.54 3.398(11) 150. 1_665 yes
C62 H62C F46 0.98 2.49 3.414(10) 158. 2_666 yes
C62 H62C F46B 0.98 2.24 3.180(17) 159. 2_666 yes

_refine_diff_density_max         0.379
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.054


# start Validation Reply Form
_vrf_PLAT029_JF2587PT83FMI       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.698 Why?
RESPONSE: 

029_ALERT_3_A _diffrn_measured_fraction_theta_full value Low .      0.698 Why?
088_ALERT_3_B Poor Data / Parameter Ratio ....................       7.66 Note
911_ALERT_3_B Missing FCF Refl Between Thmin & STh/L=    0.600       2158 Report

Data were collected at varying 2theta angles but due to the data being quite
weak the data collection was abandoned with some unique data not being
collected. It was believed that the sample would be recrystallized and new
crystals submitted for analysis but this never occurred.
;

# end Validation Reply Form
