# 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_2
_database_code_depnum_ccdc_archive 'CCDC 2127865'
loop_
_audit_author_name
_audit_author_address
'Daniel Unruh'
;Texas Tech University
United States of America
;
_audit_update_record             
;
2021-12-10 deposited with the CCDC.	2022-07-22 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT410_2                   
;
PROBLEM: Short Intra H...H Contact  H15B     ..H19B     .       1.99 Ang.  
RESPONSE: This is a typical distance for the 9-borabicyclo[3.3.1]nonane moiety
          in the chair conformation. 
;
_vrf_PLAT978_2                   
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info  
RESPONSE: The remaining electron density was primarily located between C-B,
          C-N, and C-O bonds. The remaining density was located outside of the 
          molecule.
;
# end Validation Reply Form

_audit_creation_date             2020-03-04T10:50:00-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C20 H30 B N3 O2'
_chemical_formula_weight         355.28
_chemical_absolute_configuration ad

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_Int_Tables_number      4
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   7.87410(10)
_cell_length_b                   11.4742(2)
_cell_length_c                   10.7498(2)
_cell_angle_alpha                90
_cell_angle_beta                 100.649(2)
_cell_angle_gamma                90
_cell_volume                     954.51(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    11064
_cell_measurement_theta_min      4.135
_cell_measurement_theta_max      76.202

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_size_max          0.238
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.103
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_F_000             384
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -7 2 0.0688
-5 0 0 0.0676
4 5 -2 0.045
3 6 -2 0.0558
5 3 -1 0.0631
0 0 -7 0.0488
4 5 0 0.0517
1 2 6 0.0473
-2 -2 7 0.0613
-3 -4 -4 0.0595
-3 -3 6 0.0648
1 -5 -5 0.0581
-1 -6 -4 0.0571
2 6 2 0.0571
-3 3 6 0.0853
3 -6 1 0.1011
0 -4 5 0.0577
-4 0 -4 0.069
-5 1 2 0.0742
-3 -1 -5 0.057


#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.626
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.40.70a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
                        a multifaceted crystal model
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.596
_exptl_absorpt_correction_T_max  1
_shelx_estimated_absorpt_T_min   0.865
_shelx_estimated_absorpt_T_max   0.938

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_ambient_temperature      100(2)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_detector_area_resol_mean 10
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_ub_11      -0.040186
_diffrn_orient_matrix_ub_12      -0.0117982
_diffrn_orient_matrix_ub_13      -0.1452287
_diffrn_orient_matrix_ub_21      -0.1232426
_diffrn_orient_matrix_ub_22      0.1051122
_diffrn_orient_matrix_ub_23      -0.0083953
_diffrn_orient_matrix_ub_31      0.1510971
_diffrn_orient_matrix_ub_32      0.0826852
_diffrn_orient_matrix_ub_33      -0.010029
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_unetI/netI     0.067
_diffrn_reflns_number            16818
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.185
_diffrn_reflns_theta_max         77.445
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.962
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.937
_reflns_Friedel_coverage         0.858
_reflns_number_total             3897
_reflns_number_gt                3752
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrysAlisPro 1.171.40.70a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.70a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.70a (Rigaku OD, 2020)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_shelx_SHELXL_version_number     2018/3

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0456P)²+0.3021P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_coef       0.0048(10)
_refine_ls_number_reflns         3897
_refine_ls_number_parameters     241
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0392
_refine_ls_wR_factor_ref         0.1049
_refine_ls_wR_factor_gt          0.1025
_refine_ls_goodness_of_fit_ref   1.11
_refine_ls_restrained_S_all      1.11
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.1(3)
_refine_diff_density_max         0.176
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.043

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#

_refine_special_details          
;The structure was refined as a 2-component inversion twin with a final BASF
 value of 0.109.,Twin
;

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.009 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.7322(2) 0.65504(16) 0.67102(17) 0.0262(4) Uani 1 1 d . . . . .
O2 O 0.8977(2) 0.58670(17) 0.54086(18) 0.0298(4) Uani 1 1 d . . . . .
N1 N 0.6883(3) 0.46836(19) 0.5945(2) 0.0235(5) Uani 1 1 d . . . . .
N2 N 0.7540(3) 0.3887(2) 0.4083(2) 0.0258(5) Uani 1 1 d . . . . .
N3 N 0.7685(3) 0.27280(19) 0.5871(2) 0.0249(5) Uani 1 1 d . . . . .
C1 C 0.7816(3) 0.5756(2) 0.6009(2) 0.0240(5) Uani 1 1 d . . . . .
C2 C 0.5319(3) 0.4562(2) 0.6466(2) 0.0230(5) Uani 1 1 d . . . . .
C3 C 0.5094(3) 0.5291(2) 0.7463(2) 0.0237(5) Uani 1 1 d . . . . .
C4 C 0.3524(3) 0.5136(2) 0.7888(3) 0.0275(6) Uani 1 1 d . . . . .
H4 H 0.329796 0.560596 0.856661 0.033 Uiso 1 1 calc R U . . .
C5 C 0.2290(3) 0.4327(3) 0.7360(3) 0.0295(6) Uani 1 1 d . . . . .
H5 H 0.125347 0.424728 0.768501 0.035 Uiso 1 1 calc R U . . .
C6 C 0.2564(4) 0.3634(3) 0.6361(3) 0.0289(6) Uani 1 1 d . . . . .
H6 H 0.172077 0.307963 0.599885 0.035 Uiso 1 1 calc R U . . .
C7 C 0.4086(3) 0.3759(2) 0.5895(3) 0.0260(5) Uani 1 1 d . . . . .
H7 H 0.428504 0.330435 0.519699 0.031 Uiso 1 1 calc R U . . .
C8 C 0.7410(3) 0.3754(2) 0.5285(2) 0.0236(5) Uani 1 1 d . . . . .
C9 C 0.8749(4) 0.3214(3) 0.3476(3) 0.0310(6) Uani 1 1 d . . . . .
H9A H 0.80991 0.274656 0.278533 0.046 Uiso 1 1 calc R U . . .
H9B H 0.943511 0.269742 0.41013 0.046 Uiso 1 1 calc R U . . .
H9C H 0.952072 0.374852 0.31363 0.046 Uiso 1 1 calc R U . . .
C10 C 0.6718(4) 0.4856(3) 0.3318(3) 0.0299(6) Uani 1 1 d . . . . .
H10A H 0.75598 0.548305 0.330983 0.045 Uiso 1 1 calc R U . . .
H10B H 0.574422 0.514637 0.367962 0.045 Uiso 1 1 calc R U . . .
H10C H 0.629685 0.458673 0.245014 0.045 Uiso 1 1 calc R U . . .
C11 C 0.7297(4) 0.1622(3) 0.5196(3) 0.0307(6) Uani 1 1 d . . . . .
H11A H 0.663563 0.17744 0.434601 0.046 Uiso 1 1 calc R U . . .
H11B H 0.661777 0.112579 0.566146 0.046 Uiso 1 1 calc R U . . .
H11C H 0.837976 0.122672 0.512809 0.046 Uiso 1 1 calc R U . . .
C12 C 0.8021(4) 0.2634(3) 0.7250(3) 0.0296(6) Uani 1 1 d . . . . .
H12A H 0.696937 0.237437 0.753417 0.044 Uiso 1 1 calc R U . . .
H12B H 0.837064 0.339576 0.762311 0.044 Uiso 1 1 calc R U . . .
H12C H 0.894796 0.206744 0.751879 0.044 Uiso 1 1 calc R U . . .
C13 C 0.8123(3) 0.5815(2) 0.9044(2) 0.0260(5) Uani 1 1 d . . . . .
H13 H 0.854022 0.504836 0.877519 0.031 Uiso 1 1 calc R U . . .
C14 C 0.7371(4) 0.5617(2) 1.0250(3) 0.0281(6) Uani 1 1 d . . . . .
H14A H 0.650335 0.498415 1.008543 0.034 Uiso 1 1 calc R U . . .
H14B H 0.831155 0.534837 1.093179 0.034 Uiso 1 1 calc R U . . .
C15 C 0.6517(4) 0.6692(3) 1.0723(3) 0.0318(6) Uani 1 1 d . . . . .
H15A H 0.580675 0.643038 1.134048 0.038 Uiso 1 1 calc R U . . .
H15B H 0.743827 0.720277 1.118085 0.038 Uiso 1 1 calc R U . . .
C16 C 0.5371(4) 0.7419(3) 0.9703(3) 0.0314(6) Uani 1 1 d . . . . .
H16A H 0.528018 0.821572 1.003859 0.038 Uiso 1 1 calc R U . . .
H16B H 0.419566 0.707778 0.954676 0.038 Uiso 1 1 calc R U . . .
C17 C 0.5986(4) 0.7515(2) 0.8423(3) 0.0286(6) Uani 1 1 d . . . . .
H17 H 0.500273 0.781403 0.777713 0.034 Uiso 1 1 calc R U . . .
C18 C 0.7508(4) 0.8375(2) 0.8503(3) 0.0316(6) Uani 1 1 d . . . . .
H18A H 0.776095 0.849212 0.764324 0.038 Uiso 1 1 calc R U . . .
H18B H 0.715802 0.913756 0.880622 0.038 Uiso 1 1 calc R U . . .
C19 C 0.9166(4) 0.7965(3) 0.9387(3) 0.0326(6) Uani 1 1 d . . . . .
H19A H 1.013854 0.846261 0.92425 0.039 Uiso 1 1 calc R U . . .
H19B H 0.902396 0.808037 1.027411 0.039 Uiso 1 1 calc R U . . .
C20 C 0.9644(4) 0.6683(3) 0.9212(3) 0.0295(6) Uani 1 1 d . . . . .
H20A H 1.050669 0.644132 0.995795 0.035 Uiso 1 1 calc R U . . .
H20B H 1.020258 0.66279 0.846155 0.035 Uiso 1 1 calc R U . . .
B1 B 0.6571(4) 0.6262(3) 0.7946(3) 0.0256(6) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.288(3) . ?
O1 B1 1.586(3) . ?
O2 C1 1.219(3) . ?
N1 C8 1.387(3) . ?
N1 C1 1.429(3) . ?
N1 C2 1.451(3) . ?
N2 C8 1.324(3) . ?
N2 C10 1.461(4) . ?
N2 C9 1.469(3) . ?
N3 C8 1.333(3) . ?
N3 C12 1.461(3) . ?
N3 C11 1.466(3) . ?
C2 C7 1.396(4) . ?
C2 C3 1.396(4) . ?
C3 C4 1.406(4) . ?
C3 B1 1.625(4) . ?
C4 C5 1.387(4) . ?
C4 H4 0.95 . ?
C5 C6 1.384(4) . ?
C5 H5 0.95 . ?
C6 C7 1.389(4) . ?
C6 H6 0.95 . ?
C7 H7 0.95 . ?
C9 H9A 0.98 . ?
C9 H9B 0.98 . ?
C9 H9C 0.98 . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 H11A 0.98 . ?
C11 H11B 0.98 . ?
C11 H11C 0.98 . ?
C12 H12A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C13 C14 1.538(4) . ?
C13 C20 1.543(4) . ?
C13 B1 1.617(4) . ?
C13 H13 1 . ?
C14 C15 1.536(4) . ?
C14 H14A 0.99 . ?
C14 H14B 0.99 . ?
C15 C16 1.532(4) . ?
C15 H15A 0.99 . ?
C15 H15B 0.99 . ?
C16 C17 1.545(4) . ?
C16 H16A 0.99 . ?
C16 H16B 0.99 . ?
C17 C18 1.543(4) . ?
C17 B1 1.622(4) . ?
C17 H17 1 . ?
C18 C19 1.540(4) . ?
C18 H18A 0.99 . ?
C18 H18B 0.99 . ?
C19 C20 1.538(4) . ?
C19 H19A 0.99 . ?
C19 H19B 0.99 . ?
C20 H20A 0.99 . ?
C20 H20B 0.99 . ?

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 O1 B1 122.8(2) . . ?
C8 N1 C1 119.2(2) . . ?
C8 N1 C2 118.6(2) . . ?
C1 N1 C2 122.0(2) . . ?
C8 N2 C10 122.1(2) . . ?
C8 N2 C9 123.1(2) . . ?
C10 N2 C9 114.0(2) . . ?
C8 N3 C12 121.9(2) . . ?
C8 N3 C11 122.0(2) . . ?
C12 N3 C11 114.9(2) . . ?
O2 C1 O1 125.0(2) . . ?
O2 C1 N1 119.6(2) . . ?
O1 C1 N1 115.4(2) . . ?
C7 C2 C3 123.9(2) . . ?
C7 C2 N1 117.7(2) . . ?
C3 C2 N1 118.4(2) . . ?
C2 C3 C4 114.7(2) . . ?
C2 C3 B1 118.1(2) . . ?
C4 C3 B1 127.1(2) . . ?
C5 C4 C3 122.9(3) . . ?
C5 C4 H4 118.6 . . ?
C3 C4 H4 118.6 . . ?
C6 C5 C4 120.3(2) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C7 119.3(3) . . ?
C5 C6 H6 120.3 . . ?
C7 C6 H6 120.3 . . ?
C6 C7 C2 119.0(3) . . ?
C6 C7 H7 120.5 . . ?
C2 C7 H7 120.5 . . ?
N2 C8 N3 121.9(2) . . ?
N2 C8 N1 119.7(2) . . ?
N3 C8 N1 118.3(2) . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 H12A 109.5 . . ?
N3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C20 114.1(2) . . ?
C14 C13 B1 107.8(2) . . ?
C20 C13 B1 110.3(2) . . ?
C14 C13 H13 108.2 . . ?
C20 C13 H13 108.2 . . ?
B1 C13 H13 108.2 . . ?
C15 C14 C13 114.9(2) . . ?
C15 C14 H14A 108.5 . . ?
C13 C14 H14A 108.5 . . ?
C15 C14 H14B 108.5 . . ?
C13 C14 H14B 108.5 . . ?
H14A C14 H14B 107.5 . . ?
C16 C15 C14 115.9(2) . . ?
C16 C15 H15A 108.3 . . ?
C14 C15 H15A 108.3 . . ?
C16 C15 H15B 108.3 . . ?
C14 C15 H15B 108.3 . . ?
H15A C15 H15B 107.4 . . ?
C15 C16 C17 115.9(2) . . ?
C15 C16 H16A 108.3 . . ?
C17 C16 H16A 108.3 . . ?
C15 C16 H16B 108.3 . . ?
C17 C16 H16B 108.3 . . ?
H16A C16 H16B 107.4 . . ?
C18 C17 C16 111.4(2) . . ?
C18 C17 B1 108.8(2) . . ?
C16 C17 B1 111.9(2) . . ?
C18 C17 H17 108.2 . . ?
C16 C17 H17 108.2 . . ?
B1 C17 H17 108.2 . . ?
C19 C18 C17 113.6(2) . . ?
C19 C18 H18A 108.8 . . ?
C17 C18 H18A 108.8 . . ?
C19 C18 H18B 108.8 . . ?
C17 C18 H18B 108.8 . . ?
H18A C18 H18B 107.7 . . ?
C20 C19 C18 114.6(2) . . ?
C20 C19 H19A 108.6 . . ?
C18 C19 H19A 108.6 . . ?
C20 C19 H19B 108.6 . . ?
C18 C19 H19B 108.6 . . ?
H19A C19 H19B 107.6 . . ?
C19 C20 C13 115.5(2) . . ?
C19 C20 H20A 108.4 . . ?
C13 C20 H20A 108.4 . . ?
C19 C20 H20B 108.4 . . ?
C13 C20 H20B 108.4 . . ?
H20A C20 H20B 107.5 . . ?
O1 B1 C13 109.2(2) . . ?
O1 B1 C17 104.5(2) . . ?
C13 B1 C17 105.7(2) . . ?
O1 B1 C3 103.4(2) . . ?
C13 B1 C3 114.6(2) . . ?
C17 B1 C3 118.7(2) . . ?


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

data_4
_database_code_depnum_ccdc_archive 'CCDC 2127867'
loop_
_audit_author_name
_audit_author_address
'Daniel Unruh'
;Texas Tech University
United States of America
;
_audit_update_record             
;
2021-12-10 deposited with the CCDC.	2022-07-22 downloaded from the CCDC.
;

_audit_creation_date             2020-02-17T14:44:14-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C38 H30 Al B F15 N3 O2'
_chemical_formula_weight         883.44
_chemical_absolute_configuration ad

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_Int_Tables_number      33
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   18.7204(2)
_cell_length_b                   10.81340(10)
_cell_length_c                   18.6892(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3783.28(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    50961
_cell_measurement_theta_min      2.328
_cell_measurement_theta_max      77.324

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.208
_exptl_crystal_size_min          0.162
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_F_000             1792
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-6 -4 -8 0.1025
9 -5 -1 0.1113
5 5 8 0.0874
11 0 5 0.0979
-3 6 6 0.1225
-10 -1 -6 0.1086
-5 -3 10 0.103
6 0 -11 0.1058
-1 7 -1 0.0913
0 -1 -12 0.1001
-4 6 -2 0.1007
-2 3 11 0.1231
-1 2 -12 0.1095
-7 -1 -10 0.1075
-6 -6 -3 0.0742
-9 -4 -1 0.0769
-6 -6 1 0.0659
1 -2 12 0.0984
-1 1 12 0.1037
7 0 10 0.1002
-1 5 8 0.1077
12 -1 1 0.0904
10 3 5 0.0796
12 -1 -3 0.0872
11 3 0 0.0808
7 6 2 0.0856
5 5 -6 0.1041


#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.511
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.40.70a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
                        a multifaceted crystal model
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.413
_exptl_absorpt_correction_T_max  1
_shelx_estimated_absorpt_T_min   0.673
_shelx_estimated_absorpt_T_max   0.792

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_ambient_temperature      100(2)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_detector_area_resol_mean 10
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_ub_11      0.0456148
_diffrn_orient_matrix_ub_12      0.0767246
_diffrn_orient_matrix_ub_13      -0.0523059
_diffrn_orient_matrix_ub_21      0.0625335
_diffrn_orient_matrix_ub_22      -0.0023862
_diffrn_orient_matrix_ub_23      0.0535343
_diffrn_orient_matrix_ub_31      0.0280003
_diffrn_orient_matrix_ub_32      -0.1200714
_diffrn_orient_matrix_ub_33      -0.0344364
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_number            66315
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         4.722
_diffrn_reflns_theta_max         77.495
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.975
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.954
_reflns_Friedel_coverage         0.9
_reflns_number_total             7871
_reflns_number_gt                7763
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrysAlisPro 1.171.40.70a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.70a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.70a (Rigaku OD, 2020)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_shelx_SHELXL_version_number     2018/3
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0347P)²+0.7084P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         7871
_refine_ls_number_parameters     545
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0241
_refine_ls_wR_factor_ref         0.0624
_refine_ls_wR_factor_gt          0.0622
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 
;
 Flack x determined using 3606 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(12)
_refine_diff_density_max         0.159
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.033

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.213 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.009 0.0039 '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 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
Al1 Al 0.56030(3) 0.63568(5) 0.46460(3) 0.01647(11) Uani 1 1 d . . . . .
F1 F 0.41084(6) 0.65201(12) 0.55693(7) 0.0298(3) Uani 1 1 d . . . . .
F2 F 0.38739(7) 0.73202(13) 0.68927(8) 0.0345(3) Uani 1 1 d . . . . .
F3 F 0.49572(8) 0.82174(13) 0.76977(7) 0.0359(3) Uani 1 1 d . . . . .
F4 F 0.63187(7) 0.82579(13) 0.71568(7) 0.0354(3) Uani 1 1 d . . . . .
F5 F 0.65686(6) 0.73969(12) 0.58294(7) 0.0283(3) Uani 1 1 d . . . . .
F6 F 0.55268(7) 0.93472(11) 0.47647(7) 0.0317(3) Uani 1 1 d . . . . .
F7 F 0.59856(8) 1.11015(12) 0.38634(9) 0.0410(3) Uani 1 1 d . . . . .
F8 F 0.66301(8) 1.04617(13) 0.26083(9) 0.0416(4) Uani 1 1 d . . . . .
F9 F 0.68749(7) 0.80406(14) 0.23034(8) 0.0376(3) Uani 1 1 d . . . . .
F10 F 0.64236(7) 0.62717(11) 0.32107(7) 0.0276(3) Uani 1 1 d . . . . .
F11 F 0.52426(6) 0.34739(11) 0.40980(7) 0.0269(3) Uani 1 1 d . . . . .
F12 F 0.39952(7) 0.25651(11) 0.36108(8) 0.0333(3) Uani 1 1 d . . . . .
F13 F 0.28858(7) 0.40912(13) 0.33453(9) 0.0391(3) Uani 1 1 d . . . . .
F14 F 0.29904(6) 0.65466(13) 0.36469(9) 0.0359(3) Uani 1 1 d . . . . .
F15 F 0.42187(6) 0.74612(10) 0.41776(7) 0.0257(3) Uani 1 1 d . . . . .
O1 O 0.59277(7) 0.38947(12) 0.54479(8) 0.0198(3) Uani 1 1 d . . . . .
O2 O 0.63594(7) 0.53164(11) 0.47082(7) 0.0184(3) Uani 1 1 d . . . . .
N1 N 0.70524(8) 0.37039(14) 0.49975(9) 0.0183(3) Uani 1 1 d . . . . .
N2 N 0.76086(8) 0.43420(15) 0.39345(9) 0.0217(3) Uani 1 1 d . . . . .
N3 N 0.81300(8) 0.47741(15) 0.50527(10) 0.0229(3) Uani 1 1 d . . . . .
C1 C 0.64148(9) 0.43025(16) 0.50591(10) 0.0167(3) Uani 1 1 d . . . . .
C2 C 0.71843(10) 0.24859(16) 0.52910(11) 0.0186(3) Uani 1 1 d . . . . .
C3 C 0.66661(10) 0.19483(17) 0.57306(11) 0.0206(4) Uani 1 1 d . . . . .
C4 C 0.68321(11) 0.07385(19) 0.59532(13) 0.0280(4) Uani 1 1 d . . . . .
H4 H 0.649523 0.031314 0.624294 0.034 Uiso 1 1 calc R U . . .
C5 C 0.74600(11) 0.01325(19) 0.57733(13) 0.0287(4) Uani 1 1 d . . . . .
H5 H 0.754665 -0.068176 0.594326 0.034 Uiso 1 1 calc R U . . .
C6 C 0.79588(11) 0.07166(18) 0.53464(12) 0.0252(4) Uani 1 1 d . . . . .
H6 H 0.839478 0.031619 0.522788 0.03 Uiso 1 1 calc R U . . .
C7 C 0.78141(10) 0.18972(18) 0.50929(12) 0.0230(4) Uani 1 1 d . . . . .
H7 H 0.814415 0.230099 0.478548 0.028 Uiso 1 1 calc R U . . .
C8 C 0.76196(9) 0.43146(16) 0.46373(11) 0.0194(3) Uani 1 1 d . . . . .
C9 C 0.71238(11) 0.35566(19) 0.35137(12) 0.0258(4) Uani 1 1 d . . . . .
H9A H 0.670332 0.403776 0.337215 0.039 Uiso 1 1 calc R U . . .
H9B H 0.697321 0.284791 0.380366 0.039 Uiso 1 1 calc R U . . .
H9C H 0.737193 0.326067 0.308485 0.039 Uiso 1 1 calc R U . . .
C10 C 0.80135(11) 0.5260(2) 0.35146(12) 0.0282(4) Uani 1 1 d . . . . .
H10A H 0.844104 0.486928 0.331359 0.042 Uiso 1 1 calc R U . . .
H10B H 0.815519 0.594691 0.382592 0.042 Uiso 1 1 calc R U . . .
H10C H 0.771322 0.557416 0.31254 0.042 Uiso 1 1 calc R U . . .
C11 C 0.80010(12) 0.5003(2) 0.58150(13) 0.0312(4) Uani 1 1 d . . . . .
H11A H 0.832449 0.565297 0.598442 0.047 Uiso 1 1 calc R U . . .
H11B H 0.8087 0.42422 0.608616 0.047 Uiso 1 1 calc R U . . .
H11C H 0.75051 0.526849 0.588395 0.047 Uiso 1 1 calc R U . . .
C12 C 0.88846(10) 0.4847(2) 0.48339(13) 0.0303(5) Uani 1 1 d . . . . .
H12A H 0.894545 0.444006 0.43694 0.045 Uiso 1 1 calc R U . . .
H12B H 0.918336 0.443383 0.519185 0.045 Uiso 1 1 calc R U . . .
H12C H 0.902704 0.571676 0.479471 0.045 Uiso 1 1 calc R U . . .
C13 C 0.51911(10) 0.20685(18) 0.59120(11) 0.0218(4) Uani 1 1 d . . . . .
H13 H 0.514565 0.171951 0.54186 0.026 Uiso 1 1 calc R U . . .
C14 C 0.51141(11) 0.10009(19) 0.64558(12) 0.0267(4) Uani 1 1 d . . . . .
H14A H 0.460606 0.074798 0.647018 0.032 Uiso 1 1 calc R U . . .
H14B H 0.539254 0.028565 0.627808 0.032 Uiso 1 1 calc R U . . .
C15 C 0.53565(11) 0.12850(19) 0.72225(12) 0.0278(4) Uani 1 1 d . . . . .
H15A H 0.546683 0.049217 0.74633 0.033 Uiso 1 1 calc R U . . .
H15B H 0.495098 0.166616 0.74813 0.033 Uiso 1 1 calc R U . . .
C16 C 0.60100(11) 0.21420(19) 0.72992(12) 0.0260(4) Uani 1 1 d . . . . .
H16A H 0.644742 0.164697 0.721837 0.031 Uiso 1 1 calc R U . . .
H16B H 0.602688 0.245322 0.779713 0.031 Uiso 1 1 calc R U . . .
C17 C 0.60215(11) 0.32594(18) 0.67866(11) 0.0221(4) Uani 1 1 d . . . . .
H17 H 0.64905 0.369245 0.683959 0.027 Uiso 1 1 calc R U . . .
C18 C 0.54163(11) 0.42032(18) 0.69249(12) 0.0264(4) Uani 1 1 d . . . . .
H18A H 0.542173 0.44279 0.743841 0.032 Uiso 1 1 calc R U . . .
H18B H 0.552019 0.496307 0.664835 0.032 Uiso 1 1 calc R U . . .
C19 C 0.46590(12) 0.3757(2) 0.67291(13) 0.0293(5) Uani 1 1 d . . . . .
H19A H 0.448388 0.320796 0.711491 0.035 Uiso 1 1 calc R U . . .
H19B H 0.43377 0.448362 0.670939 0.035 Uiso 1 1 calc R U . . .
C20 C 0.46086(10) 0.3061(2) 0.60141(12) 0.0257(4) Uani 1 1 d . . . . .
H20A H 0.464304 0.366647 0.561828 0.031 Uiso 1 1 calc R U . . .
H20B H 0.413436 0.265975 0.598236 0.031 Uiso 1 1 calc R U . . .
C21 C 0.53541(11) 0.69265(17) 0.56329(11) 0.0196(4) Uani 1 1 d . . . . .
C22 C 0.46813(10) 0.69376(17) 0.59406(11) 0.0224(4) Uani 1 1 d . . . . .
C23 C 0.45396(11) 0.73472(18) 0.66269(12) 0.0247(4) Uani 1 1 d . . . . .
C24 C 0.50918(12) 0.77929(18) 0.70394(11) 0.0260(4) Uani 1 1 d . . . . .
C25 C 0.57770(12) 0.78113(18) 0.67615(11) 0.0248(4) Uani 1 1 d . . . . .
C26 C 0.58882(10) 0.73783(17) 0.60754(11) 0.0212(4) Uani 1 1 d . . . . .
C27 C 0.59637(10) 0.77284(17) 0.40302(11) 0.0196(4) Uani 1 1 d . . . . .
C28 C 0.58660(10) 0.89777(19) 0.41628(12) 0.0238(4) Uani 1 1 d . . . . .
C29 C 0.60908(11) 0.99042(18) 0.37034(13) 0.0287(5) Uani 1 1 d . . . . .
C30 C 0.64248(11) 0.9586(2) 0.30715(13) 0.0296(5) Uani 1 1 d . . . . .
C31 C 0.65417(10) 0.8354(2) 0.29130(12) 0.0269(4) Uani 1 1 d . . . . .
C32 C 0.63088(10) 0.74697(18) 0.33918(11) 0.0213(4) Uani 1 1 d . . . . .
C33 C 0.47813(10) 0.55111(17) 0.41656(10) 0.0191(4) Uani 1 1 d . . . . .
C34 C 0.46996(10) 0.42750(18) 0.39990(11) 0.0212(4) Uani 1 1 d . . . . .
C35 C 0.40706(11) 0.37850(18) 0.37306(12) 0.0244(4) Uani 1 1 d . . . . .
C36 C 0.34963(10) 0.4556(2) 0.36014(12) 0.0271(4) Uani 1 1 d . . . . .
C37 C 0.35510(11) 0.57978(19) 0.37541(12) 0.0255(4) Uani 1 1 d . . . . .
C38 C 0.41858(10) 0.62328(17) 0.40279(11) 0.0206(4) Uani 1 1 d . . . . .
B1 B 0.59691(11) 0.27107(19) 0.59854(12) 0.0190(4) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Al1 O2 1.8123(13) . ?
Al1 C27 1.9951(19) . ?
Al1 C21 2.000(2) . ?
Al1 C33 2.0022(19) . ?
F1 C22 1.355(2) . ?
F2 C23 1.342(2) . ?
F3 C24 1.337(2) . ?
F4 C25 1.344(2) . ?
F5 C26 1.354(2) . ?
F6 C28 1.352(3) . ?
F7 C29 1.343(2) . ?
F8 C30 1.339(2) . ?
F9 C31 1.342(3) . ?
F10 C32 1.356(2) . ?
F11 C34 1.348(2) . ?
F12 C35 1.345(2) . ?
F13 C36 1.337(2) . ?
F14 C37 1.341(2) . ?
F15 C38 1.359(2) . ?
O1 C1 1.246(2) . ?
O1 B1 1.629(2) . ?
O2 C1 1.282(2) . ?
N1 C1 1.363(2) . ?
N1 C8 1.420(2) . ?
N1 C2 1.448(2) . ?
N2 C8 1.314(3) . ?
N2 C9 1.471(3) . ?
N2 C10 1.475(2) . ?
N3 C8 1.328(3) . ?
N3 C11 1.466(3) . ?
N3 C12 1.473(2) . ?
C2 C7 1.390(3) . ?
C2 C3 1.398(3) . ?
C3 C4 1.407(3) . ?
C3 B1 1.615(3) . ?
C4 C5 1.387(3) . ?
C4 H4 0.95 . ?
C5 C6 1.381(3) . ?
C5 H5 0.95 . ?
C6 C7 1.388(3) . ?
C6 H6 0.95 . ?
C7 H7 0.95 . ?
C9 H9A 0.98 . ?
C9 H9B 0.98 . ?
C9 H9C 0.98 . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 H11A 0.98 . ?
C11 H11B 0.98 . ?
C11 H11C 0.98 . ?
C12 H12A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C13 C20 1.542(3) . ?
C13 C14 1.545(3) . ?
C13 B1 1.619(3) . ?
C13 H13 1 . ?
C14 C15 1.534(3) . ?
C14 H14A 0.99 . ?
C14 H14B 0.99 . ?
C15 C16 1.541(3) . ?
C15 H15A 0.99 . ?
C15 H15B 0.99 . ?
C16 C17 1.542(3) . ?
C16 H16A 0.99 . ?
C16 H16B 0.99 . ?
C17 C18 1.547(3) . ?
C17 B1 1.614(3) . ?
C17 H17 1 . ?
C18 C19 1.542(3) . ?
C18 H18A 0.99 . ?
C18 H18B 0.99 . ?
C19 C20 1.537(3) . ?
C19 H19A 0.99 . ?
C19 H19B 0.99 . ?
C20 H20A 0.99 . ?
C20 H20B 0.99 . ?
C21 C22 1.385(3) . ?
C21 C26 1.386(3) . ?
C22 C23 1.382(3) . ?
C23 C24 1.377(3) . ?
C24 C25 1.384(3) . ?
C25 C26 1.381(3) . ?
C27 C32 1.385(3) . ?
C27 C28 1.386(3) . ?
C28 C29 1.385(3) . ?
C29 C30 1.380(4) . ?
C30 C31 1.383(3) . ?
C31 C32 1.380(3) . ?
C33 C34 1.381(3) . ?
C33 C38 1.385(3) . ?
C34 C35 1.385(3) . ?
C35 C36 1.381(3) . ?
C36 C37 1.377(3) . ?
C37 C38 1.377(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
O2 Al1 C27 103.53(7) . . ?
O2 Al1 C21 108.31(7) . . ?
C27 Al1 C21 112.45(8) . . ?
O2 Al1 C33 110.22(7) . . ?
C27 Al1 C33 109.93(8) . . ?
C21 Al1 C33 112.05(8) . . ?
C1 O1 B1 127.06(14) . . ?
C1 O2 Al1 128.83(12) . . ?
C1 N1 C8 118.31(15) . . ?
C1 N1 C2 123.32(15) . . ?
C8 N1 C2 118.36(15) . . ?
C8 N2 C9 122.08(17) . . ?
C8 N2 C10 122.61(18) . . ?
C9 N2 C10 114.91(17) . . ?
C8 N3 C11 120.85(17) . . ?
C8 N3 C12 123.24(19) . . ?
C11 N3 C12 114.76(17) . . ?
O1 C1 O2 122.80(16) . . ?
O1 C1 N1 121.47(17) . . ?
O2 C1 N1 115.71(16) . . ?
C7 C2 C3 123.69(17) . . ?
C7 C2 N1 117.41(17) . . ?
C3 C2 N1 118.86(16) . . ?
C2 C3 C4 114.02(17) . . ?
C2 C3 B1 121.44(16) . . ?
C4 C3 B1 124.44(17) . . ?
C5 C4 C3 123.68(19) . . ?
C5 C4 H4 118.2 . . ?
C3 C4 H4 118.2 . . ?
C6 C5 C4 119.80(18) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C7 119.06(18) . . ?
C5 C6 H6 120.5 . . ?
C7 C6 H6 120.5 . . ?
C6 C7 C2 119.72(18) . . ?
C6 C7 H7 120.1 . . ?
C2 C7 H7 120.1 . . ?
N2 C8 N3 125.96(18) . . ?
N2 C8 N1 118.20(17) . . ?
N3 C8 N1 115.79(18) . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 H12A 109.5 . . ?
N3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C20 C13 C14 111.88(17) . . ?
C20 C13 B1 109.09(16) . . ?
C14 C13 B1 110.41(16) . . ?
C20 C13 H13 108.5 . . ?
C14 C13 H13 108.5 . . ?
B1 C13 H13 108.5 . . ?
C15 C14 C13 115.93(17) . . ?
C15 C14 H14A 108.3 . . ?
C13 C14 H14A 108.3 . . ?
C15 C14 H14B 108.3 . . ?
C13 C14 H14B 108.3 . . ?
H14A C14 H14B 107.4 . . ?
C14 C15 C16 116.23(17) . . ?
C14 C15 H15A 108.2 . . ?
C16 C15 H15A 108.2 . . ?
C14 C15 H15B 108.2 . . ?
C16 C15 H15B 108.2 . . ?
H15A C15 H15B 107.4 . . ?
C15 C16 C17 115.11(17) . . ?
C15 C16 H16A 108.5 . . ?
C17 C16 H16A 108.5 . . ?
C15 C16 H16B 108.5 . . ?
C17 C16 H16B 108.5 . . ?
H16A C16 H16B 107.5 . . ?
C16 C17 C18 113.76(17) . . ?
C16 C17 B1 106.71(16) . . ?
C18 C17 B1 110.69(16) . . ?
C16 C17 H17 108.5 . . ?
C18 C17 H17 108.5 . . ?
B1 C17 H17 108.5 . . ?
C19 C18 C17 115.31(17) . . ?
C19 C18 H18A 108.4 . . ?
C17 C18 H18A 108.4 . . ?
C19 C18 H18B 108.4 . . ?
C17 C18 H18B 108.4 . . ?
H18A C18 H18B 107.5 . . ?
C20 C19 C18 114.59(17) . . ?
C20 C19 H19A 108.6 . . ?
C18 C19 H19A 108.6 . . ?
C20 C19 H19B 108.6 . . ?
C18 C19 H19B 108.6 . . ?
H19A C19 H19B 107.6 . . ?
C19 C20 C13 113.91(17) . . ?
C19 C20 H20A 108.8 . . ?
C13 C20 H20A 108.8 . . ?
C19 C20 H20B 108.8 . . ?
C13 C20 H20B 108.8 . . ?
H20A C20 H20B 107.7 . . ?
C22 C21 C26 113.90(18) . . ?
C22 C21 Al1 126.70(15) . . ?
C26 C21 Al1 119.39(15) . . ?
F1 C22 C23 115.47(18) . . ?
F1 C22 C21 120.29(18) . . ?
C23 C22 C21 124.23(19) . . ?
F2 C23 C24 119.84(19) . . ?
F2 C23 C22 120.97(19) . . ?
C24 C23 C22 119.19(19) . . ?
F3 C24 C23 119.6(2) . . ?
F3 C24 C25 120.99(19) . . ?
C23 C24 C25 119.39(19) . . ?
F4 C25 C26 121.2(2) . . ?
F4 C25 C24 119.87(19) . . ?
C26 C25 C24 118.90(19) . . ?
F5 C26 C25 116.86(18) . . ?
F5 C26 C21 118.75(18) . . ?
C25 C26 C21 124.38(19) . . ?
C32 C27 C28 114.36(17) . . ?
C32 C27 Al1 120.30(14) . . ?
C28 C27 Al1 125.24(16) . . ?
F6 C28 C29 116.40(18) . . ?
F6 C28 C27 119.93(18) . . ?
C29 C28 C27 123.7(2) . . ?
F7 C29 C30 119.8(2) . . ?
F7 C29 C28 121.0(2) . . ?
C30 C29 C28 119.2(2) . . ?
F8 C30 C29 120.5(2) . . ?
F8 C30 C31 119.8(2) . . ?
C29 C30 C31 119.69(19) . . ?
F9 C31 C32 121.5(2) . . ?
F9 C31 C30 119.91(19) . . ?
C32 C31 C30 118.6(2) . . ?
F10 C32 C31 116.73(19) . . ?
F10 C32 C27 118.81(17) . . ?
C31 C32 C27 124.46(19) . . ?
C34 C33 C38 114.48(17) . . ?
C34 C33 Al1 128.92(14) . . ?
C38 C33 Al1 116.39(14) . . ?
F11 C34 C33 120.50(17) . . ?
F11 C34 C35 116.41(17) . . ?
C33 C34 C35 123.09(18) . . ?
F12 C35 C36 118.73(18) . . ?
F12 C35 C34 121.63(18) . . ?
C36 C35 C34 119.61(18) . . ?
F13 C36 C37 120.28(19) . . ?
F13 C36 C35 120.09(19) . . ?
C37 C36 C35 119.61(18) . . ?
F14 C37 C38 121.66(18) . . ?
F14 C37 C36 119.99(18) . . ?
C38 C37 C36 118.33(18) . . ?
F15 C38 C37 116.72(17) . . ?
F15 C38 C33 118.43(16) . . ?
C37 C38 C33 124.85(18) . . ?
C17 B1 C3 114.34(16) . . ?
C17 B1 C13 106.92(16) . . ?
C3 B1 C13 118.86(16) . . ?
C17 B1 O1 106.62(15) . . ?
C3 B1 O1 104.93(14) . . ?
C13 B1 O1 104.01(14) . . ?


####################################################################### 
# 
# 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_12
_database_code_depnum_ccdc_archive 'CCDC 2127873'
loop_
_audit_author_name
_audit_author_address
'Daniel Unruh'
;Texas Tech University
United States of America
;
_audit_update_record             
;
2021-12-10 deposited with the CCDC.	2022-07-22 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT230_12                  
;
PROBLEM: Hirshfeld Test Diff for    S1       --C20      .        5.3 s.u.  
RESPONSE: The sulfur and carbon atoms are part of a triflate molecule.
;
_vrf_PLAT410_12                  
;
PROBLEM: Short Intra H...H Contact  H14B     ..H18A     .       1.96 Ang.  
RESPONSE: This is a typical H...H contact distance in the boat configuration of
          the 9-Borabicyclo[3.3.1]nonane molecule.
;
_vrf_PLAT911_12                  
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         10 Report
RESPONSE: These inconsistent reflections were omitted during the integration.
;
# end Validation Reply Form

_audit_creation_date             2020-06-23T12:49:21-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C20 H31 B F3 N3 O3 S'
_chemical_formula_weight         461.35

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.6186(4)
_cell_length_b                   11.4262(6)
_cell_length_c                   11.6710(6)
_cell_angle_alpha                64.789(5)
_cell_angle_beta                 72.278(4)
_cell_angle_gamma                76.763(4)
_cell_volume                     1098.07(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9690
_cell_measurement_theta_min      4.298
_cell_measurement_theta_max      76.404

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.111
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_F_000             488
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 0 7 0.0712
5 -3 0 0.0505
-1 0 -7 0.064
-5 3 1 0.0627
-4 2 -5 0.0635
6 2 1 0.0472
-1 7 2 0.0622
-6 -1 -1 0.0664
2 -7 -2 0.0503
-5 -6 -3 0.0545
-3 -6 1 0.0505
1 -6 1 0.0509
6 0 -1 0.0527
2 1 -6 0.0681
-3 3 -4 0.0611
-1 -1 6 0.0822
-4 -4 -7 0.0627
3 5 7 0.0638
4 7 4 0.058
0 7 4 0.0565
-1 -7 -1 0.0438
-5 -6 -5 0.0517


#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.777
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
        a multifaceted crystal model
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_T_max  1
_shelx_estimated_absorpt_T_min   0.776
_shelx_estimated_absorpt_T_max   0.827

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_ambient_temperature      100(2)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_detector_area_resol_mean 10
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_ub_11      -0.0399364
_diffrn_orient_matrix_ub_12      -0.086988
_diffrn_orient_matrix_ub_13      0.1460286
_diffrn_orient_matrix_ub_21      -0.0528338
_diffrn_orient_matrix_ub_22      -0.09723
_diffrn_orient_matrix_ub_23      -0.0325863
_diffrn_orient_matrix_ub_31      0.155778
_diffrn_orient_matrix_ub_32      -0.0740657
_diffrn_orient_matrix_ub_33      -0.0119244
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0678
_diffrn_reflns_number            21343
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         4.305
_diffrn_reflns_theta_max         77.569
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.967
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.967
_reflns_Friedel_coverage         0
_reflns_number_total             4518
_reflns_number_gt                4080
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_shelx_SHELXL_version_number     2018/3
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0515P)²+0.4061P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4518
_refine_ls_number_parameters     287
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.042
_refine_ls_R_factor_gt           0.0387
_refine_ls_wR_factor_ref         0.106
_refine_ls_wR_factor_gt          0.1036
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_restrained_S_all      1.102
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.052

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.009 0.0039 '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 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.31817(4) 0.23719(4) 0.17962(3) 0.02131(11) Uani 1 1 d . . . . .
F1 F 0.09214(11) 0.36526(10) 0.07774(11) 0.0386(3) Uani 1 1 d . . . . .
F2 F 0.20120(12) 0.20361(12) 0.02296(10) 0.0392(3) Uani 1 1 d . . . . .
F3 F 0.06057(11) 0.16911(11) 0.21401(10) 0.0389(3) Uani 1 1 d . . . . .
O1 O 0.24475(11) 0.29165(10) 0.28048(10) 0.0215(2) Uani 1 1 d . . . . .
O2 O 0.41024(12) 0.32358(12) 0.06885(11) 0.0288(3) Uani 1 1 d . . . . .
O3 O 0.37287(13) 0.10231(11) 0.22818(12) 0.0307(3) Uani 1 1 d . . . . .
N1 N 0.34734(14) 0.53769(12) 0.22108(12) 0.0213(3) Uani 1 1 d . . . . .
H1 H 0.291(2) 0.4904(18) 0.2159(18) 0.026 Uiso 1 1 d . U . . .
N2 N 0.36517(14) 0.74562(12) 0.20306(12) 0.0217(3) Uani 1 1 d . . . . .
N3 N 0.25323(14) 0.71920(12) 0.06642(12) 0.0219(3) Uani 1 1 d . . . . .
C1 C 0.47194(16) 0.46062(14) 0.27140(14) 0.0197(3) Uani 1 1 d . . . . .
C2 C 0.45557(16) 0.33092(14) 0.35870(14) 0.0201(3) Uani 1 1 d . . . . .
C3 C 0.58559(16) 0.25527(15) 0.39168(14) 0.0213(3) Uani 1 1 d . . . . .
H3 H 0.582065 0.165617 0.446124 0.026 Uiso 1 1 calc R U . . .
C4 C 0.71919(16) 0.30564(15) 0.34827(15) 0.0226(3) Uani 1 1 d . . . . .
H4 H 0.803964 0.251247 0.37449 0.027 Uiso 1 1 calc R U . . .
C5 C 0.72825(16) 0.43527(15) 0.26675(15) 0.0227(3) Uani 1 1 d . . . . .
H5 H 0.81846 0.470976 0.238925 0.027 Uiso 1 1 calc R U . . .
C6 C 0.60451(16) 0.51296(15) 0.22580(14) 0.0215(3) Uani 1 1 d . . . . .
H6 H 0.610554 0.601143 0.1671 0.026 Uiso 1 1 calc R U . . .
C7 C 0.32403(15) 0.66827(15) 0.16260(14) 0.0202(3) Uani 1 1 d . . . . .
C8 C 0.37805(18) 0.70518(17) 0.33650(15) 0.0262(3) Uani 1 1 d . . . . .
H8A H 0.482115 0.686531 0.338537 0.039 Uiso 1 1 calc R U . . .
H8B H 0.329052 0.626698 0.392563 0.039 Uiso 1 1 calc R U . . .
H8C H 0.331632 0.775178 0.367937 0.039 Uiso 1 1 calc R U . . .
C9 C 0.42026(19) 0.86972(16) 0.11177(16) 0.0287(3) Uani 1 1 d . . . . .
H9A H 0.428448 0.879646 0.0224 0.043 Uiso 1 1 calc R U . . .
H9B H 0.51714 0.871301 0.122029 0.043 Uiso 1 1 calc R U . . .
H9C H 0.352107 0.94135 0.129741 0.043 Uiso 1 1 calc R U . . .
C10 C 0.25488(18) 0.64859(16) -0.01343(16) 0.0273(3) Uani 1 1 d . . . . .
H10A H 0.267059 0.708709 -0.104854 0.041 Uiso 1 1 calc R U . . .
H10B H 0.162032 0.611243 0.016085 0.041 Uiso 1 1 calc R U . . .
H10C H 0.336669 0.578573 -0.004958 0.041 Uiso 1 1 calc R U . . .
C11 C 0.16161(19) 0.84420(16) 0.03885(16) 0.0289(3) Uani 1 1 d . . . . .
H11A H 0.210399 0.908449 -0.043111 0.043 Uiso 1 1 calc R U . . .
H11B H 0.14636 0.873554 0.109822 0.043 Uiso 1 1 calc R U . . .
H11C H 0.066463 0.834634 0.031286 0.043 Uiso 1 1 calc R U . . .
C12 C 0.16274(16) 0.34820(14) 0.48849(15) 0.0219(3) Uani 1 1 d . . . . .
H12 H 0.157639 0.442384 0.429467 0.026 Uiso 1 1 calc R U . . .
C13 C 0.19525(18) 0.33407(17) 0.61561(16) 0.0279(3) Uani 1 1 d . . . . .
H13A H 0.282848 0.378245 0.592973 0.034 Uiso 1 1 calc R U . . .
H13B H 0.111295 0.379548 0.660616 0.034 Uiso 1 1 calc R U . . .
C14 C 0.22248(19) 0.19269(18) 0.71054(16) 0.0303(4) Uani 1 1 d . . . . .
H14A H 0.264556 0.192723 0.778099 0.036 Uiso 1 1 calc R U . . .
H14B H 0.12685 0.157228 0.754792 0.036 Uiso 1 1 calc R U . . .
C15 C 0.32572(18) 0.10173(17) 0.64661(15) 0.0279(3) Uani 1 1 d . . . . .
H15A H 0.314366 0.010562 0.708174 0.033 Uiso 1 1 calc R U . . .
H15B H 0.428315 0.116315 0.632171 0.033 Uiso 1 1 calc R U . . .
C16 C 0.30031(16) 0.11873(15) 0.51507(14) 0.0221(3) Uani 1 1 d . . . . .
H16 H 0.383937 0.068166 0.473901 0.026 Uiso 1 1 calc R U . . .
C17 C 0.15596(17) 0.06887(15) 0.53331(15) 0.0246(3) Uani 1 1 d . . . . .
H17A H 0.153889 0.067359 0.449662 0.03 Uiso 1 1 calc R U . . .
H17B H 0.155952 -0.021916 0.598156 0.03 Uiso 1 1 calc R U . . .
C18 C 0.01510(17) 0.14923(16) 0.57795(16) 0.0256(3) Uani 1 1 d . . . . .
H18A H -0.00268 0.123918 0.673131 0.031 Uiso 1 1 calc R U . . .
H18B H -0.06855 0.126529 0.561777 0.031 Uiso 1 1 calc R U . . .
C19 C 0.01755(16) 0.29778(15) 0.51082(16) 0.0252(3) Uani 1 1 d . . . . .
H19A H -0.006406 0.327442 0.425312 0.03 Uiso 1 1 calc R U . . .
H19B H -0.061341 0.338828 0.564062 0.03 Uiso 1 1 calc R U . . .
C20 C 0.15872(17) 0.24418(16) 0.12108(16) 0.0261(3) Uani 1 1 d . . . . .
B1 B 0.29980(18) 0.27024(16) 0.42150(16) 0.0205(3) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O3 1.4281(12) . ?
S1 O2 1.4304(12) . ?
S1 O1 1.4792(11) . ?
S1 C20 1.8333(16) . ?
F1 C20 1.332(2) . ?
F2 C20 1.3318(18) . ?
F3 C20 1.3260(19) . ?
O1 B1 1.7825(19) . ?
N1 C7 1.3471(19) . ?
N1 C1 1.4358(19) . ?
N1 H1 0.88(2) . ?
N2 C7 1.3380(19) . ?
N2 C8 1.4603(19) . ?
N2 C9 1.463(2) . ?
N3 C7 1.3379(19) . ?
N3 C11 1.458(2) . ?
N3 C10 1.4647(19) . ?
C1 C6 1.390(2) . ?
C1 C2 1.408(2) . ?
C2 C3 1.405(2) . ?
C2 B1 1.624(2) . ?
C3 C4 1.390(2) . ?
C3 H3 0.95 . ?
C4 C5 1.384(2) . ?
C4 H4 0.95 . ?
C5 C6 1.391(2) . ?
C5 H5 0.95 . ?
C6 H6 0.95 . ?
C8 H8A 0.98 . ?
C8 H8B 0.98 . ?
C8 H8C 0.98 . ?
C9 H9A 0.98 . ?
C9 H9B 0.98 . ?
C9 H9C 0.98 . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 H11A 0.98 . ?
C11 H11B 0.98 . ?
C11 H11C 0.98 . ?
C12 C19 1.539(2) . ?
C12 C13 1.543(2) . ?
C12 B1 1.603(2) . ?
C12 H12 1 . ?
C13 C14 1.538(2) . ?
C13 H13A 0.99 . ?
C13 H13B 0.99 . ?
C14 C15 1.536(2) . ?
C14 H14A 0.99 . ?
C14 H14B 0.99 . ?
C15 C16 1.551(2) . ?
C15 H15A 0.99 . ?
C15 H15B 0.99 . ?
C16 C17 1.542(2) . ?
C16 B1 1.606(2) . ?
C16 H16 1 . ?
C17 C18 1.536(2) . ?
C17 H17A 0.99 . ?
C17 H17B 0.99 . ?
C18 C19 1.539(2) . ?
C18 H18A 0.99 . ?
C18 H18B 0.99 . ?
C19 H19A 0.99 . ?
C19 H19B 0.99 . ?

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
O3 S1 O2 117.68(7) . . ?
O3 S1 O1 115.07(7) . . ?
O2 S1 O1 112.77(7) . . ?
O3 S1 C20 104.88(7) . . ?
O2 S1 C20 104.09(7) . . ?
O1 S1 C20 99.48(7) . . ?
S1 O1 B1 129.46(9) . . ?
C7 N1 C1 127.91(12) . . ?
C7 N1 H1 118.5(12) . . ?
C1 N1 H1 112.4(12) . . ?
C7 N2 C8 122.78(13) . . ?
C7 N2 C9 121.67(13) . . ?
C8 N2 C9 115.01(12) . . ?
C7 N3 C11 122.84(13) . . ?
C7 N3 C10 121.92(13) . . ?
C11 N3 C10 115.12(12) . . ?
C6 C1 C2 123.05(13) . . ?
C6 C1 N1 119.38(13) . . ?
C2 C1 N1 117.40(13) . . ?
C3 C2 C1 114.95(13) . . ?
C3 C2 B1 120.98(13) . . ?
C1 C2 B1 124.06(13) . . ?
C4 C3 C2 122.99(14) . . ?
C4 C3 H3 118.5 . . ?
C2 C3 H3 118.5 . . ?
C5 C4 C3 119.77(14) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 119.60(14) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C1 C6 C5 119.50(14) . . ?
C1 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?
N3 C7 N2 120.51(13) . . ?
N3 C7 N1 118.50(13) . . ?
N2 C7 N1 120.93(13) . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C19 C12 C13 113.17(13) . . ?
C19 C12 B1 111.16(12) . . ?
C13 C12 B1 106.55(12) . . ?
C19 C12 H12 108.6 . . ?
C13 C12 H12 108.6 . . ?
B1 C12 H12 108.6 . . ?
C14 C13 C12 114.60(13) . . ?
C14 C13 H13A 108.6 . . ?
C12 C13 H13A 108.6 . . ?
C14 C13 H13B 108.6 . . ?
C12 C13 H13B 108.6 . . ?
H13A C13 H13B 107.6 . . ?
C15 C14 C13 114.54(13) . . ?
C15 C14 H14A 108.6 . . ?
C13 C14 H14A 108.6 . . ?
C15 C14 H14B 108.6 . . ?
C13 C14 H14B 108.6 . . ?
H14A C14 H14B 107.6 . . ?
C14 C15 C16 115.14(13) . . ?
C14 C15 H15A 108.5 . . ?
C16 C15 H15A 108.5 . . ?
C14 C15 H15B 108.5 . . ?
C16 C15 H15B 108.5 . . ?
H15A C15 H15B 107.5 . . ?
C17 C16 C15 111.98(12) . . ?
C17 C16 B1 110.78(12) . . ?
C15 C16 B1 108.20(12) . . ?
C17 C16 H16 108.6 . . ?
C15 C16 H16 108.6 . . ?
B1 C16 H16 108.6 . . ?
C18 C17 C16 115.06(13) . . ?
C18 C17 H17A 108.5 . . ?
C16 C17 H17A 108.5 . . ?
C18 C17 H17B 108.5 . . ?
C16 C17 H17B 108.5 . . ?
H17A C17 H17B 107.5 . . ?
C17 C18 C19 114.86(13) . . ?
C17 C18 H18A 108.6 . . ?
C19 C18 H18A 108.6 . . ?
C17 C18 H18B 108.6 . . ?
C19 C18 H18B 108.6 . . ?
H18A C18 H18B 107.5 . . ?
C12 C19 C18 116.18(12) . . ?
C12 C19 H19A 108.2 . . ?
C18 C19 H19A 108.2 . . ?
C12 C19 H19B 108.2 . . ?
C18 C19 H19B 108.2 . . ?
H19A C19 H19B 107.4 . . ?
F3 C20 F2 107.87(13) . . ?
F3 C20 F1 108.00(13) . . ?
F2 C20 F1 107.75(13) . . ?
F3 C20 S1 111.70(11) . . ?
F2 C20 S1 109.99(11) . . ?
F1 C20 S1 111.37(10) . . ?
C12 B1 C16 107.41(12) . . ?
C12 B1 C2 118.21(12) . . ?
C16 B1 C2 118.06(12) . . ?
C12 B1 O1 101.32(11) . . ?
C16 B1 O1 107.58(11) . . ?
C2 B1 O1 102.22(11) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1 O1 0.88(2) 2.173(19) 2.9242(16) 143.1(17) . yes



# END of CIF
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 2127866'
loop_
_audit_author_name
_audit_author_address
'Daniel Unruh'
;Texas Tech University
United States of America
;
_audit_update_record             
;
2021-12-10 deposited with the CCDC.	2022-07-22 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT911_3                   
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          3 Report
RESPONSE: These reflections were omitted during the absorption correction.
;
# end Validation Reply Form

_audit_creation_date             2020-01-24T09:11:51-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C41 H33 B2 F15 N3 O2'
_chemical_formula_weight         906.32

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_Int_Tables_number      61
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   18.11110(10)
_cell_length_b                   19.79510(10)
_cell_length_c                   21.89340(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7849.03(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    89682
_cell_measurement_theta_min      3.854
_cell_measurement_theta_max      77.386

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_size_max          0.186
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.052
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_F_000             3688
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0299
0 0 -1 0.0224
-7 -7 -9 0.0625
-7 -7 7 0.0763
7 7 -7 0.0722
8 8 6 0.0761
0 -13 0 0.0278
0 13 0 0.0317
11 -3 0 0.0918
11 3 0 0.0914
-12 -3 0 0.0882
-11 5 0 0.0865
0 -11 -8 0.0254
10 -1 -8 0.0763
-11 3 -5 0.0738
10 -5 6 0.084
-2 12 5 0.0379


#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.263
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
                        a multifaceted crystal model
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_T_max  1
_shelx_estimated_absorpt_T_min   0.799
_shelx_estimated_absorpt_T_max   0.937

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_ambient_temperature      100(2)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_detector_area_resol_mean 10
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_ub_11      -0.0209257
_diffrn_orient_matrix_ub_12      0.0197055
_diffrn_orient_matrix_ub_13      0.0658124
_diffrn_orient_matrix_ub_21      -0.0544277
_diffrn_orient_matrix_ub_22      0.0531172
_diffrn_orient_matrix_ub_23      -0.0248823
_diffrn_orient_matrix_ub_31      -0.0619205
_diffrn_orient_matrix_ub_32      -0.0533757
_diffrn_orient_matrix_ub_33      -0.0004561
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_number            137589
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.875
_diffrn_reflns_theta_max         77.463
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.992
_reflns_Friedel_coverage         0
_reflns_number_total             8269
_reflns_number_gt                7673
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_shelx_SHELXL_version_number     2018/3
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0419P)²+3.6007P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         8269
_refine_ls_number_parameters     601
_refine_ls_number_restraints     64
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0307
_refine_ls_wR_factor_ref         0.0816
_refine_ls_wR_factor_gt          0.0799
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.043

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 The carbon atoms (C39 < C41) of the interstitial benzene molecule were modeled
 as disordered over two positions (A and B). SIMU and free variable DFIX 
 restraints were applied to maintain reasonable ADP values and C-C bond lengths.  
;

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.009 0.0039 '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 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.70613(4) 0.65451(4) 0.71431(3) 0.02076(14) Uani 1 1 d . . . . .
F2 F 0.80744(4) 0.72525(4) 0.77486(3) 0.02646(16) Uani 1 1 d . . . . .
F3 F 0.78622(4) 0.75830(4) 0.89453(4) 0.03121(18) Uani 1 1 d . . . . .
F4 F 0.66291(4) 0.71380(4) 0.95309(3) 0.03237(18) Uani 1 1 d . . . . .
F5 F 0.56281(4) 0.64074(4) 0.89550(3) 0.02295(15) Uani 1 1 d . . . . .
F6 F 0.61005(4) 0.50630(3) 0.84996(3) 0.01886(14) Uani 1 1 d . . . . .
F7 F 0.68392(4) 0.39036(3) 0.83629(3) 0.02215(15) Uani 1 1 d . . . . .
F8 F 0.73309(4) 0.35235(3) 0.72366(3) 0.02588(16) Uani 1 1 d . . . . .
F9 F 0.70149(4) 0.43043(4) 0.62463(3) 0.02225(15) Uani 1 1 d . . . . .
F10 F 0.62312(4) 0.54294(3) 0.63622(3) 0.01865(14) Uani 1 1 d . . . . .
F11 F 0.47508(4) 0.70978(3) 0.80067(3) 0.01969(14) Uani 1 1 d . . . . .
F12 F 0.34485(4) 0.70204(3) 0.85718(3) 0.02302(15) Uani 1 1 d . . . . .
F13 F 0.28420(4) 0.57841(4) 0.88318(3) 0.02565(16) Uani 1 1 d . . . . .
F14 F 0.35567(4) 0.46455(3) 0.84833(3) 0.02394(15) Uani 1 1 d . . . . .
F15 F 0.48306(4) 0.47001(3) 0.79088(3) 0.01930(14) Uani 1 1 d . . . . .
O1 O 0.47370(4) 0.58642(4) 0.65140(3) 0.01560(15) Uani 1 1 d . . . . .
O2 O 0.55783(4) 0.64609(4) 0.70319(3) 0.01413(15) Uani 1 1 d . . . . .
N1 N 0.52338(5) 0.68388(4) 0.61196(4) 0.01460(18) Uani 1 1 d . . . . .
N2 N 0.63589(5) 0.74199(5) 0.60152(4) 0.01560(18) Uani 1 1 d . . . . .
N3 N 0.54398(5) 0.78430(5) 0.66582(4) 0.01713(19) Uani 1 1 d . . . . .
C1 C 0.48923(6) 0.67784(5) 0.55233(5) 0.0160(2) Uani 1 1 d . . . . .
C2 C 0.50187(7) 0.72963(6) 0.51060(5) 0.0216(2) Uani 1 1 d . . . . .
H2 H 0.531373 0.767385 0.521645 0.026 Uiso 1 1 calc R U . . .
C3 C 0.47101(7) 0.72561(7) 0.45278(6) 0.0256(3) Uani 1 1 d . . . . .
H3 H 0.479159 0.760518 0.423771 0.031 Uiso 1 1 calc R U . . .
C4 C 0.42819(7) 0.67013(7) 0.43781(6) 0.0247(3) Uani 1 1 d . . . . .
H4 H 0.407422 0.666416 0.398107 0.03 Uiso 1 1 calc R U . . .
C5 C 0.41557(6) 0.61993(6) 0.48080(5) 0.0207(2) Uani 1 1 d . . . . .
H5 H 0.385747 0.582512 0.469423 0.025 Uiso 1 1 calc R U . . .
C6 C 0.44466(6) 0.62159(5) 0.54037(5) 0.0158(2) Uani 1 1 d . . . . .
C7 C 0.57017(6) 0.73874(5) 0.62691(5) 0.0147(2) Uani 1 1 d . . . . .
C8 C 0.66930(6) 0.68414(6) 0.56968(5) 0.0191(2) Uani 1 1 d . . . . .
H8A H 0.661543 0.688886 0.525584 0.029 Uiso 1 1 calc R U . . .
H8B H 0.646241 0.642209 0.583908 0.029 Uiso 1 1 calc R U . . .
H8C H 0.722371 0.68278 0.578315 0.029 Uiso 1 1 calc R U . . .
C9 C 0.67904(7) 0.80477(6) 0.59849(6) 0.0227(2) Uani 1 1 d . . . . .
H9A H 0.700074 0.809753 0.557492 0.034 Uiso 1 1 calc R U . . .
H9B H 0.718984 0.803087 0.62864 0.034 Uiso 1 1 calc R U . . .
H9C H 0.646825 0.843337 0.607299 0.034 Uiso 1 1 calc R U . . .
C10 C 0.46425(7) 0.79463(6) 0.67304(6) 0.0249(3) Uani 1 1 d . . . . .
H10A H 0.438522 0.777869 0.636701 0.037 Uiso 1 1 calc R U . . .
H10B H 0.454084 0.842931 0.678135 0.037 Uiso 1 1 calc R U . . .
H10C H 0.446893 0.770005 0.709121 0.037 Uiso 1 1 calc R U . . .
C11 C 0.59027(7) 0.81573(6) 0.71299(5) 0.0214(2) Uani 1 1 d . . . . .
H11A H 0.639348 0.794886 0.712609 0.032 Uiso 1 1 calc R U . . .
H11B H 0.56747 0.809094 0.753137 0.032 Uiso 1 1 calc R U . . .
H11C H 0.594887 0.864202 0.704702 0.032 Uiso 1 1 calc R U . . .
C12 C 0.43884(6) 0.48763(6) 0.58160(5) 0.0188(2) Uani 1 1 d . . . . .
H12 H 0.490966 0.482476 0.567267 0.023 Uiso 1 1 calc R U . . .
C13 C 0.38695(7) 0.45958(6) 0.53177(6) 0.0261(3) Uani 1 1 d . . . . .
H13A H 0.402949 0.477901 0.491825 0.031 Uiso 1 1 calc R U . . .
H13B H 0.393059 0.409917 0.530148 0.031 Uiso 1 1 calc R U . . .
C14 C 0.30425(8) 0.47540(7) 0.54010(6) 0.0316(3) Uani 1 1 d . . . . .
H14A H 0.282896 0.441299 0.568061 0.038 Uiso 1 1 calc R U . . .
H14B H 0.279486 0.470186 0.500065 0.038 Uiso 1 1 calc R U . . .
C15 C 0.28597(7) 0.54618(7) 0.56531(6) 0.0275(3) Uani 1 1 d . . . . .
H15A H 0.235095 0.54537 0.581831 0.033 Uiso 1 1 calc R U . . .
H15B H 0.28668 0.578691 0.530954 0.033 Uiso 1 1 calc R U . . .
C16 C 0.33835(6) 0.57241(6) 0.61570(5) 0.0189(2) Uani 1 1 d . . . . .
H16 H 0.326959 0.621175 0.622999 0.023 Uiso 1 1 calc R U . . .
C17 C 0.32965(6) 0.53440(6) 0.67666(5) 0.0207(2) Uani 1 1 d . . . . .
H17A H 0.357806 0.558796 0.708527 0.025 Uiso 1 1 calc R U . . .
H17B H 0.27694 0.535237 0.688619 0.025 Uiso 1 1 calc R U . . .
C18 C 0.35590(7) 0.46050(6) 0.67517(6) 0.0230(2) Uani 1 1 d . . . . .
H18A H 0.317788 0.432903 0.654481 0.028 Uiso 1 1 calc R U . . .
H18B H 0.360147 0.443942 0.717695 0.028 Uiso 1 1 calc R U . . .
C19 C 0.43025(7) 0.44925(6) 0.64268(6) 0.0213(2) Uani 1 1 d . . . . .
H19A H 0.436318 0.400319 0.63481 0.026 Uiso 1 1 calc R U . . .
H19B H 0.470495 0.463387 0.670489 0.026 Uiso 1 1 calc R U . . .
C20 C 0.51576(6) 0.63557(5) 0.65669(5) 0.0134(2) Uani 1 1 d . . . . .
C21 C 0.62661(6) 0.64607(5) 0.80047(5) 0.0149(2) Uani 1 1 d . . . . .
C22 C 0.69160(6) 0.66933(5) 0.77348(5) 0.0162(2) Uani 1 1 d . . . . .
C23 C 0.74493(6) 0.70689(6) 0.80336(5) 0.0194(2) Uani 1 1 d . . . . .
C24 C 0.73474(7) 0.72330(6) 0.86407(6) 0.0220(2) Uani 1 1 d . . . . .
C25 C 0.67243(7) 0.70033(6) 0.89332(5) 0.0216(2) Uani 1 1 d . . . . .
C26 C 0.62066(6) 0.66226(6) 0.86198(5) 0.0177(2) Uani 1 1 d . . . . .
C27 C 0.61144(6) 0.53034(5) 0.74415(5) 0.0144(2) Uani 1 1 d . . . . .
C28 C 0.63083(6) 0.48871(6) 0.79298(5) 0.0155(2) Uani 1 1 d . . . . .
C29 C 0.66954(6) 0.42911(6) 0.78730(5) 0.0171(2) Uani 1 1 d . . . . .
C30 C 0.69382(6) 0.40947(6) 0.73021(6) 0.0184(2) Uani 1 1 d . . . . .
C31 C 0.67781(6) 0.44910(6) 0.68024(5) 0.0173(2) Uani 1 1 d . . . . .
C32 C 0.63698(6) 0.50789(5) 0.68791(5) 0.0153(2) Uani 1 1 d . . . . .
C33 C 0.48728(6) 0.59086(5) 0.79255(5) 0.0151(2) Uani 1 1 d . . . . .
C34 C 0.44675(6) 0.64732(5) 0.81051(5) 0.0162(2) Uani 1 1 d . . . . .
C35 C 0.37949(6) 0.64509(6) 0.84021(5) 0.0181(2) Uani 1 1 d . . . . .
C36 C 0.34884(6) 0.58293(6) 0.85373(5) 0.0192(2) Uani 1 1 d . . . . .
C37 C 0.38575(6) 0.52538(6) 0.83651(5) 0.0181(2) Uani 1 1 d . . . . .
C38 C 0.45290(6) 0.53004(5) 0.80642(5) 0.0160(2) Uani 1 1 d . . . . .
C39A C 0.5177(5) 0.5586(3) 1.0302(3) 0.0758(15) Uani 0.630(10) 1 d D U P A 1
H39A H 0.527649 0.599729 1.051014 0.091 Uiso 0.630(10) 1 calc R U P A 1
C40A C 0.5750(3) 0.5187(4) 1.0114(2) 0.0696(14) Uani 0.630(10) 1 d D U P A 1
H40A H 0.625096 0.5303 1.018764 0.084 Uiso 0.630(10) 1 calc R U P A 1
C41A C 0.5550(5) 0.4604(4) 0.9808(2) 0.0744(16) Uani 0.630(10) 1 d D U P A 1
H41A H 0.593198 0.431622 0.96642 0.089 Uiso 0.630(10) 1 calc R U P A 1
C39B C 0.5507(8) 0.5456(7) 1.0071(5) 0.075(2) Uani 0.370(10) 1 d D U P A 2
H39B H 0.587515 0.579258 1.012432 0.09 Uiso 0.370(10) 1 calc R U P A 2
C40B C 0.5771(6) 0.4793(7) 0.9939(5) 0.076(2) Uani 0.370(10) 1 d D U P A 2
H40B H 0.628038 0.468709 0.990302 0.091 Uiso 0.370(10) 1 calc R U P A 2
C41B C 0.5224(8) 0.4327(5) 0.9868(4) 0.078(2) Uani 0.370(10) 1 d D U P A 2
H41B H 0.533608 0.386792 0.978089 0.093 Uiso 0.370(10) 1 calc R U P A 2
B1 B 0.42259(7) 0.56685(6) 0.59211(6) 0.0151(2) Uani 1 1 d . . . . .
B2 B 0.56803(7) 0.60092(6) 0.75978(5) 0.0136(2) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 C22 1.3540(13) . ?
F2 C23 1.3429(14) . ?
F3 C24 1.3395(13) . ?
F4 C25 1.3466(14) . ?
F5 C26 1.3482(13) . ?
F6 C28 1.3489(12) . ?
F7 C29 1.3441(13) . ?
F8 C30 1.3435(13) . ?
F9 C31 1.3428(13) . ?
F10 C32 1.3508(13) . ?
F11 C34 1.3558(12) . ?
F12 C35 1.3424(12) . ?
F13 C36 1.3396(13) . ?
F14 C37 1.3466(13) . ?
F15 C38 1.3515(12) . ?
O1 C20 1.2411(13) . ?
O1 B1 1.6407(14) . ?
O2 C20 1.2886(13) . ?
O2 B2 1.5389(13) . ?
N1 C20 1.3756(14) . ?
N1 C7 1.4158(13) . ?
N1 C1 1.4494(13) . ?
N2 C7 1.3151(15) . ?
N2 C9 1.4695(14) . ?
N2 C8 1.4709(14) . ?
N3 C7 1.3282(14) . ?
N3 C10 1.4670(15) . ?
N3 C11 1.4685(14) . ?
C1 C2 1.3923(16) . ?
C1 C6 1.4001(15) . ?
C2 C3 1.3860(17) . ?
C2 H2 0.95 . ?
C3 C4 1.3838(18) . ?
C3 H3 0.95 . ?
C4 C5 1.3876(17) . ?
C4 H4 0.95 . ?
C5 C6 1.4070(15) . ?
C5 H5 0.95 . ?
C6 B1 1.6177(16) . ?
C8 H8A 0.98 . ?
C8 H8B 0.98 . ?
C8 H8C 0.98 . ?
C9 H9A 0.98 . ?
C9 H9B 0.98 . ?
C9 H9C 0.98 . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 H11A 0.98 . ?
C11 H11B 0.98 . ?
C11 H11C 0.98 . ?
C12 C13 1.5432(16) . ?
C12 C19 1.5458(16) . ?
C12 B1 1.6121(16) . ?
C12 H12 1 . ?
C13 C14 1.541(2) . ?
C13 H13A 0.99 . ?
C13 H13B 0.99 . ?
C14 C15 1.542(2) . ?
C14 H14A 0.99 . ?
C14 H14B 0.99 . ?
C15 C16 1.5449(16) . ?
C15 H15A 0.99 . ?
C15 H15B 0.99 . ?
C16 C17 1.5403(16) . ?
C16 B1 1.6144(16) . ?
C16 H16 1 . ?
C17 C18 1.5385(17) . ?
C17 H17A 0.99 . ?
C17 H17B 0.99 . ?
C18 C19 1.5390(17) . ?
C18 H18A 0.99 . ?
C18 H18B 0.99 . ?
C19 H19A 0.99 . ?
C19 H19B 0.99 . ?
C21 C26 1.3885(15) . ?
C21 C22 1.3952(15) . ?
C21 B2 1.6486(16) . ?
C22 C23 1.3833(16) . ?
C23 C24 1.3806(17) . ?
C24 C25 1.3749(18) . ?
C25 C26 1.3848(16) . ?
C27 C32 1.3884(15) . ?
C27 C28 1.3947(15) . ?
C27 B2 1.6392(15) . ?
C28 C29 1.3779(15) . ?
C29 C30 1.3809(17) . ?
C30 C31 1.3770(17) . ?
C31 C32 1.3891(15) . ?
C33 C38 1.3889(15) . ?
C33 C34 1.3938(15) . ?
C33 B2 1.6412(16) . ?
C34 C35 1.3816(16) . ?
C35 C36 1.3820(16) . ?
C36 C37 1.3735(16) . ?
C37 C38 1.3863(16) . ?
C39A C40A 1.368(8) . ?
C39A C41A 1.390(8) 5_667 ?
C39A H39A 0.95 . ?
C40A C41A 1.383(8) . ?
C40A H40A 0.95 . ?
C41A H41A 0.95 . ?
C39B C41B 1.399(16) 5_667 ?
C39B C40B 1.425(14) . ?
C39B H39B 0.95 . ?
C40B C41B 1.363(9) . ?
C40B H40B 0.95 . ?
C41B H41B 0.95 . ?

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
C20 O1 B1 127.24(9) . . ?
C20 O2 B2 127.82(8) . . ?
C20 N1 C7 115.39(9) . . ?
C20 N1 C1 122.75(9) . . ?
C7 N1 C1 121.79(9) . . ?
C7 N2 C9 122.80(9) . . ?
C7 N2 C8 122.31(9) . . ?
C9 N2 C8 114.72(9) . . ?
C7 N3 C10 121.02(10) . . ?
C7 N3 C11 122.34(10) . . ?
C10 N3 C11 115.28(10) . . ?
C2 C1 C6 123.89(10) . . ?
C2 C1 N1 117.40(10) . . ?
C6 C1 N1 118.69(9) . . ?
C3 C2 C1 119.40(11) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C4 C3 C2 119.20(11) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C3 C4 C5 120.00(11) . . ?
C3 C4 H4 120 . . ?
C5 C4 H4 120 . . ?
C4 C5 C6 123.39(11) . . ?
C4 C5 H5 118.3 . . ?
C6 C5 H5 118.3 . . ?
C1 C6 C5 114.07(10) . . ?
C1 C6 B1 122.97(10) . . ?
C5 C6 B1 122.75(10) . . ?
N2 C7 N3 124.13(10) . . ?
N2 C7 N1 118.79(10) . . ?
N3 C7 N1 117.09(10) . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 C19 111.93(10) . . ?
C13 C12 B1 109.85(10) . . ?
C19 C12 B1 109.64(9) . . ?
C13 C12 H12 108.4 . . ?
C19 C12 H12 108.4 . . ?
B1 C12 H12 108.4 . . ?
C14 C13 C12 115.79(10) . . ?
C14 C13 H13A 108.3 . . ?
C12 C13 H13A 108.3 . . ?
C14 C13 H13B 108.3 . . ?
C12 C13 H13B 108.3 . . ?
H13A C13 H13B 107.4 . . ?
C13 C14 C15 115.83(10) . . ?
C13 C14 H14A 108.3 . . ?
C15 C14 H14A 108.3 . . ?
C13 C14 H14B 108.3 . . ?
C15 C14 H14B 108.3 . . ?
H14A C14 H14B 107.4 . . ?
C14 C15 C16 115.41(11) . . ?
C14 C15 H15A 108.4 . . ?
C16 C15 H15A 108.4 . . ?
C14 C15 H15B 108.4 . . ?
C16 C15 H15B 108.4 . . ?
H15A C15 H15B 107.5 . . ?
C17 C16 C15 113.06(10) . . ?
C17 C16 B1 109.91(9) . . ?
C15 C16 B1 109.21(9) . . ?
C17 C16 H16 108.2 . . ?
C15 C16 H16 108.2 . . ?
B1 C16 H16 108.2 . . ?
C18 C17 C16 114.49(10) . . ?
C18 C17 H17A 108.6 . . ?
C16 C17 H17A 108.6 . . ?
C18 C17 H17B 108.6 . . ?
C16 C17 H17B 108.6 . . ?
H17A C17 H17B 107.6 . . ?
C17 C18 C19 114.69(9) . . ?
C17 C18 H18A 108.6 . . ?
C19 C18 H18A 108.6 . . ?
C17 C18 H18B 108.6 . . ?
C19 C18 H18B 108.6 . . ?
H18A C18 H18B 107.6 . . ?
C18 C19 C12 114.63(10) . . ?
C18 C19 H19A 108.6 . . ?
C12 C19 H19A 108.6 . . ?
C18 C19 H19B 108.6 . . ?
C12 C19 H19B 108.6 . . ?
H19A C19 H19B 107.6 . . ?
O1 C20 O2 124.28(10) . . ?
O1 C20 N1 122.69(10) . . ?
O2 C20 N1 113.00(9) . . ?
C26 C21 C22 113.58(10) . . ?
C26 C21 B2 126.82(10) . . ?
C22 C21 B2 119.53(9) . . ?
F1 C22 C23 115.68(10) . . ?
F1 C22 C21 119.84(10) . . ?
C23 C22 C21 124.48(11) . . ?
F2 C23 C24 119.77(10) . . ?
F2 C23 C22 120.95(11) . . ?
C24 C23 C22 119.23(11) . . ?
F3 C24 C25 120.70(11) . . ?
F3 C24 C23 120.53(11) . . ?
C25 C24 C23 118.71(10) . . ?
F4 C25 C24 119.49(11) . . ?
F4 C25 C26 120.17(11) . . ?
C24 C25 C26 120.32(11) . . ?
F5 C26 C25 115.37(10) . . ?
F5 C26 C21 121.01(10) . . ?
C25 C26 C21 123.62(11) . . ?
C32 C27 C28 113.99(10) . . ?
C32 C27 B2 128.15(10) . . ?
C28 C27 B2 117.68(9) . . ?
F6 C28 C29 116.51(10) . . ?
F6 C28 C27 119.08(10) . . ?
C29 C28 C27 124.40(10) . . ?
F7 C29 C28 121.01(10) . . ?
F7 C29 C30 120.00(10) . . ?
C28 C29 C30 118.99(10) . . ?
F8 C30 C31 120.41(10) . . ?
F8 C30 C29 120.15(10) . . ?
C31 C30 C29 119.45(10) . . ?
F9 C31 C30 119.76(10) . . ?
F9 C31 C32 120.67(10) . . ?
C30 C31 C32 119.57(10) . . ?
F10 C32 C27 121.11(10) . . ?
F10 C32 C31 115.34(10) . . ?
C27 C32 C31 123.55(10) . . ?
C38 C33 C34 113.41(10) . . ?
C38 C33 B2 126.89(10) . . ?
C34 C33 B2 119.69(9) . . ?
F11 C34 C35 115.95(9) . . ?
F11 C34 C33 119.15(10) . . ?
C35 C34 C33 124.86(10) . . ?
F12 C35 C34 121.03(10) . . ?
F12 C35 C36 120.05(10) . . ?
C34 C35 C36 118.90(10) . . ?
F13 C36 C37 120.13(10) . . ?
F13 C36 C35 120.90(10) . . ?
C37 C36 C35 118.97(10) . . ?
F14 C37 C36 119.47(10) . . ?
F14 C37 C38 120.38(10) . . ?
C36 C37 C38 120.14(10) . . ?
F15 C38 C37 114.56(9) . . ?
F15 C38 C33 121.73(10) . . ?
C37 C38 C33 123.71(10) . . ?
C40A C39A C41A 120.7(5) . 5_667 ?
C40A C39A H39A 119.7 . . ?
C41A C39A H39A 119.7 5_667 . ?
C39A C40A C41A 115.4(6) . . ?
C39A C40A H40A 122.3 . . ?
C41A C40A H40A 122.3 . . ?
C40A C41A C39A 123.9(6) . 5_667 ?
C40A C41A H41A 118 . . ?
C39A C41A H41A 118 5_667 . ?
C41B C39B C40B 128.3(8) 5_667 . ?
C41B C39B H39B 115.9 5_667 . ?
C40B C39B H39B 115.9 . . ?
C41B C40B C39B 113.8(11) . . ?
C41B C40B H40B 123.1 . . ?
C39B C40B H40B 123.1 . . ?
C40B C41B H41B 121 . . ?
C39B C41B H41B 121 5_667 . ?
C12 B1 C16 106.53(9) . . ?
C12 B1 C6 120.44(9) . . ?
C16 B1 C6 114.32(9) . . ?
C12 B1 O1 103.86(8) . . ?
C16 B1 O1 105.31(8) . . ?
C6 B1 O1 104.86(8) . . ?
O2 B2 C27 112.63(9) . . ?
O2 B2 C33 108.39(8) . . ?
C27 B2 C33 114.53(9) . . ?
O2 B2 C21 101.39(8) . . ?
C27 B2 C21 105.43(8) . . ?
C33 B2 C21 113.77(9) . . ?


####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 2127869'
loop_
_audit_author_name
_audit_author_address
'Daniel Unruh'
;Texas Tech University
United States of America
;
_audit_update_record             
;
2021-12-10 deposited with the CCDC.	2022-07-22 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT601_6                   
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .         31 Ang**3
RESPONSE: After applying PLATON/SQUEEZE on the final structure, there was only
          1 electron found in the void space. The details of the squeezed data
          analysis is listed in the Constraints and Restraints section.
;
_vrf_PLAT911_6                   
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         39 Report
RESPONSE: These reflections were omitted during the absorption correction.
;
# end Validation Reply Form

_audit_creation_date             2020-02-14T08:50:38-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C30 H45 B F3 N3 O5 S Si'
_chemical_formula_weight         655.65

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.02498(14)
_cell_length_b                   12.9384(3)
_cell_length_c                   17.0652(3)
_cell_angle_alpha                86.1005(17)
_cell_angle_beta                 80.4534(15)
_cell_angle_gamma                80.8641(17)
_cell_volume                     1723.60(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    32861
_cell_measurement_theta_min      2.598
_cell_measurement_theta_max      76.756

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       blade
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_size_max          0.276
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.042
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_F_000             696
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 7 -5 0.0463
-5 1 -1 0.1215
0 -7 5 0.0357
1 -7 5 0.0414
5 1 0 0.1379
0 -5 -9 0.0209
0 5 9 0.0209
-3 4 6 0.0649
0 2 -11 0.0376
-1 -2 10 0.04
3 -2 9 0.0868
2 -7 -4 0.0498
1 8 5 0.0378
0 7 6 0.029
-1 -7 -6 0.0468
2 -4 -7 0.0587
0 -4 9 0.0394
-4 4 -4 0.1072
4 3 -6 0.1171
0 7 6 0.0268


#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.652
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.40.70a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
                        a multifaceted crystal model
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.564
_exptl_absorpt_correction_T_max  1
_shelx_estimated_absorpt_T_min   0.658
_shelx_estimated_absorpt_T_max   0.934

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_ambient_temperature      100(2)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_detector_area_resol_mean 10
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_ub_11      -0.0294134
_diffrn_orient_matrix_ub_12      -0.0275285
_diffrn_orient_matrix_ub_13      0.0899966
_diffrn_orient_matrix_ub_21      0.0123113
_diffrn_orient_matrix_ub_22      0.1137107
_diffrn_orient_matrix_ub_23      0.0170825
_diffrn_orient_matrix_ub_31      -0.1942927
_diffrn_orient_matrix_ub_32      0.0297109
_diffrn_orient_matrix_ub_33      0.0020739
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_unetI/netI     0.0604
_diffrn_reflns_number            59003
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.628
_diffrn_reflns_theta_max         77.288
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.963
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.963
_reflns_Friedel_coverage         0
_reflns_number_total             7042
_reflns_number_gt                6358
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrysAlisPro 1.171.40.70a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.70a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.70a (Rigaku OD, 2020)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_shelx_SHELXL_version_number     2018/3
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0480P)²+0.6486P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         7042
_refine_ls_number_parameters     404
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.036
_refine_ls_wR_factor_ref         0.0979
_refine_ls_wR_factor_gt          0.0958
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.49
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.044

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 The results of the use of PLATON/SQUEEZE on the final data set.

 loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.062  0.320  0.256        31         1 ' '
   2 -0.062  0.680  0.744        32         1 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?
;

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.009 0.0039 '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 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.81485(4) 0.28431(2) 0.50458(2) 0.02658(9) Uani 1 1 d . . . . .
Si1 Si 0.49432(5) 0.50594(3) 0.22880(2) 0.02438(10) Uani 1 1 d . . . . .
F1 F 1.00187(14) 0.13772(8) 0.41563(7) 0.0512(3) Uani 1 1 d . . . . .
F2 F 0.76842(12) 0.09346(7) 0.47935(6) 0.0402(2) Uani 1 1 d . . . . .
F3 F 0.97895(13) 0.10052(7) 0.54115(6) 0.0438(2) Uani 1 1 d . . . . .
O1 O 0.74182(13) 0.65596(7) 0.14519(5) 0.0260(2) Uani 1 1 d . . . . .
O2 O 0.59718(12) 0.60048(7) 0.25932(6) 0.0257(2) Uani 1 1 d . . . . .
O3 O 0.72622(14) 0.32134(8) 0.43880(6) 0.0320(2) Uani 1 1 d . . . . .
O4 O 0.96737(14) 0.32852(8) 0.50691(8) 0.0376(3) Uani 1 1 d . . . . .
O5 O 0.70493(15) 0.27673(9) 0.58008(7) 0.0374(3) Uani 1 1 d . . . . .
N1 N 0.78529(14) 0.70903(9) 0.26424(6) 0.0230(2) Uani 1 1 d . . . . .
N2 N 0.65304(14) 0.79280(9) 0.38010(7) 0.0235(2) Uani 1 1 d . . . . .
N3 N 0.77795(14) 0.61673(9) 0.38766(7) 0.0227(2) Uani 1 1 d . . . . .
C1 C 0.70898(17) 0.65436(10) 0.21921(8) 0.0230(3) Uani 1 1 d . . . . .
C2 C 0.92254(17) 0.76715(10) 0.22992(8) 0.0241(3) Uani 1 1 d . . . . .
C3 C 0.95302(18) 0.78586(10) 0.14740(8) 0.0245(3) Uani 1 1 d . . . . .
C4 C 1.08935(19) 0.84195(11) 0.12074(9) 0.0292(3) Uani 1 1 d . . . . .
H4 H 1.117062 0.857217 0.06529 0.035 Uiso 1 1 calc R U . . .
C5 C 1.18551(19) 0.87613(12) 0.17162(9) 0.0328(3) Uani 1 1 d . . . . .
H5 H 1.274621 0.915439 0.150852 0.039 Uiso 1 1 calc R U . . .
C6 C 1.15181(19) 0.85308(13) 0.25241(9) 0.0328(3) Uani 1 1 d . . . . .
H6 H 1.218347 0.875566 0.287297 0.039 Uiso 1 1 calc R U . . .
C7 C 1.01991(19) 0.79678(12) 0.28212(9) 0.0297(3) Uani 1 1 d . . . . .
H7 H 0.996654 0.778815 0.337339 0.036 Uiso 1 1 calc R U . . .
C8 C 0.68805(18) 0.83120(11) 0.06237(8) 0.0246(3) Uani 1 1 d . . . . .
H8 H 0.624178 0.867825 0.110578 0.03 Uiso 1 1 calc R U . . .
C9 C 0.77298(19) 0.91206(11) 0.00504(8) 0.0269(3) Uani 1 1 d . . . . .
H9A H 0.682534 0.966158 -0.01182 0.032 Uiso 1 1 calc R U . . .
H9AB H 0.843834 0.947222 0.033982 0.032 Uiso 1 1 calc R U . . .
C10 C 0.8853(2) 0.86448(12) -0.06915(8) 0.0303(3) Uani 1 1 d . . . . .
H10A H 0.95392 0.917473 -0.096315 0.036 Uiso 1 1 calc R U . . .
H10B H 0.8101 0.849069 -0.105975 0.036 Uiso 1 1 calc R U . . .
C11 C 1.0075(2) 0.76366(12) -0.05344(9) 0.0311(3) Uani 1 1 d . . . . .
H11A H 1.110529 0.783674 -0.037255 0.037 Uiso 1 1 calc R U . . .
H11B H 1.044502 0.727388 -0.10405 0.037 Uiso 1 1 calc R U . . .
C12 C 0.93455(19) 0.68501(11) 0.01053(8) 0.0284(3) Uani 1 1 d . . . . .
H12 H 1.031303 0.632553 0.02518 0.034 Uiso 1 1 calc R U . . .
C13 C 0.8072(2) 0.62642(12) -0.02031(9) 0.0329(3) Uani 1 1 d . . . . .
H13A H 0.864704 0.592085 -0.069783 0.039 Uiso 1 1 calc R U . . .
H13B H 0.776156 0.570626 0.019564 0.039 Uiso 1 1 calc R U . . .
C14 C 0.6424(2) 0.69621(12) -0.03739(9) 0.0337(3) Uani 1 1 d . . . . .
H14A H 0.556784 0.650561 -0.042042 0.04 Uiso 1 1 calc R U . . .
H14B H 0.667325 0.733796 -0.089488 0.04 Uiso 1 1 calc R U . . .
C15 C 0.56212(19) 0.77783(12) 0.02555(9) 0.0292(3) Uani 1 1 d . . . . .
H15A H 0.484893 0.833073 0.000701 0.035 Uiso 1 1 calc R U . . .
H15B H 0.490924 0.742827 0.069129 0.035 Uiso 1 1 calc R U . . .
C16 C 0.73455(16) 0.70528(10) 0.34830(8) 0.0219(3) Uani 1 1 d . . . . .
C17 C 0.65448(19) 0.81716(11) 0.46267(8) 0.0276(3) Uani 1 1 d . . . . .
H17A H 0.749326 0.77191 0.482969 0.041 Uiso 1 1 calc R U . . .
H17B H 0.546249 0.805158 0.49539 0.041 Uiso 1 1 calc R U . . .
H17C H 0.668827 0.890679 0.46482 0.041 Uiso 1 1 calc R U . . .
C18 C 0.56474(19) 0.87728(11) 0.33328(9) 0.0300(3) Uani 1 1 d . . . . .
H18A H 0.635107 0.933331 0.320397 0.045 Uiso 1 1 calc R U . . .
H18B H 0.45461 0.905213 0.364239 0.045 Uiso 1 1 calc R U . . .
H18C H 0.54559 0.849645 0.283987 0.045 Uiso 1 1 calc R U . . .
C19 C 0.68495(18) 0.58717(11) 0.46542(8) 0.0267(3) Uani 1 1 d . . . . .
H19A H 0.574677 0.632941 0.475551 0.04 Uiso 1 1 calc R U . . .
H19B H 0.752319 0.594633 0.507075 0.04 Uiso 1 1 calc R U . . .
H19C H 0.665784 0.514218 0.46551 0.04 Uiso 1 1 calc R U . . .
C20 C 0.91490(19) 0.53516(11) 0.35419(9) 0.0299(3) Uani 1 1 d . . . . .
H20A H 0.864716 0.478209 0.336555 0.045 Uiso 1 1 calc R U . . .
H20B H 0.985268 0.507698 0.394897 0.045 Uiso 1 1 calc R U . . .
H20C H 0.986185 0.565101 0.30878 0.045 Uiso 1 1 calc R U . . .
C21 C 0.38957(19) 0.46040(11) 0.32665(9) 0.0299(3) Uani 1 1 d . . . . .
H21A H 0.314294 0.410388 0.319225 0.045 Uiso 1 1 calc R U . . .
H21B H 0.322039 0.520434 0.354931 0.045 Uiso 1 1 calc R U . . .
H21C H 0.476693 0.426189 0.3578 0.045 Uiso 1 1 calc R U . . .
C22 C 0.3415(2) 0.56800(12) 0.16363(10) 0.0351(3) Uani 1 1 d . . . . .
H22A H 0.40384 0.584601 0.111065 0.053 Uiso 1 1 calc R U . . .
H22B H 0.277577 0.632601 0.186884 0.053 Uiso 1 1 calc R U . . .
H22C H 0.261753 0.519766 0.15833 0.053 Uiso 1 1 calc R U . . .
C23 C 0.6628(2) 0.40713(12) 0.17918(10) 0.0363(3) Uani 1 1 d . . . . .
H23A H 0.611373 0.34808 0.16585 0.054 Uiso 1 1 calc R U . . .
H23B H 0.745861 0.38215 0.21491 0.054 Uiso 1 1 calc R U . . .
H23C H 0.720662 0.438611 0.130398 0.054 Uiso 1 1 calc R U . . .
C24 C 0.89576(19) 0.14698(11) 0.48364(10) 0.0312(3) Uani 1 1 d . . . . .
C25 C 0.4975(2) 0.08073(12) 0.18759(9) 0.0334(3) Uani 1 1 d . . . . .
H25 H 0.466767 0.05034 0.143903 0.04 Uiso 1 1 calc R U . . .
C26 C 0.6663(2) 0.08760(12) 0.18913(10) 0.0367(3) Uani 1 1 d . . . . .
H26 H 0.751973 0.061342 0.146874 0.044 Uiso 1 1 calc R U . . .
C27 C 0.7113(2) 0.13291(13) 0.25245(11) 0.0414(4) Uani 1 1 d . . . . .
H27 H 0.827834 0.137356 0.253776 0.05 Uiso 1 1 calc R U . . .
C28 C 0.5860(3) 0.17169(13) 0.31377(10) 0.0410(4) Uani 1 1 d . . . . .
H28 H 0.616418 0.20366 0.356782 0.049 Uiso 1 1 calc R U . . .
C29 C 0.4168(2) 0.16390(13) 0.31241(10) 0.0392(4) Uani 1 1 d . . . . .
H29 H 0.331026 0.190079 0.354655 0.047 Uiso 1 1 calc R U . . .
C30 C 0.3720(2) 0.11788(13) 0.24938(10) 0.0364(3) Uani 1 1 d . . . . .
H30 H 0.255877 0.111857 0.248578 0.044 Uiso 1 1 calc R U . . .
B1 B 0.8397(2) 0.74561(12) 0.08911(9) 0.0241(3) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O4 1.4382(11) . ?
S1 O3 1.4418(11) . ?
S1 O5 1.4426(12) . ?
S1 C24 1.8302(15) . ?
Si1 O2 1.7316(10) . ?
Si1 C23 1.8433(16) . ?
Si1 C21 1.8440(15) . ?
Si1 C22 1.8452(16) . ?
F1 C24 1.3210(19) . ?
F2 C24 1.3362(17) . ?
F3 C24 1.3341(18) . ?
O1 C1 1.2462(17) . ?
O1 B1 1.6637(17) . ?
O2 C1 1.2999(16) . ?
N1 C1 1.3541(17) . ?
N1 C16 1.4244(17) . ?
N1 C2 1.4529(16) . ?
N2 C16 1.3173(18) . ?
N2 C17 1.4669(17) . ?
N2 C18 1.4691(17) . ?
N3 C16 1.3158(17) . ?
N3 C20 1.4674(18) . ?
N3 C19 1.4687(16) . ?
C2 C7 1.387(2) . ?
C2 C3 1.3999(19) . ?
C3 C4 1.4045(19) . ?
C3 B1 1.615(2) . ?
C4 C5 1.389(2) . ?
C4 H4 0.95 . ?
C5 C6 1.382(2) . ?
C5 H5 0.95 . ?
C6 C7 1.387(2) . ?
C6 H6 0.95 . ?
C7 H7 0.95 . ?
C8 C9 1.5434(18) . ?
C8 C15 1.5441(19) . ?
C8 B1 1.614(2) . ?
C8 H8 1 . ?
C9 C10 1.532(2) . ?
C9 H9A 0.99 . ?
C9 H9AB 0.99 . ?
C10 C11 1.539(2) . ?
C10 H10A 0.99 . ?
C10 H10B 0.99 . ?
C11 C12 1.548(2) . ?
C11 H11A 0.99 . ?
C11 H11B 0.99 . ?
C12 C13 1.541(2) . ?
C12 B1 1.615(2) . ?
C12 H12 1 . ?
C13 C14 1.537(2) . ?
C13 H13A 0.99 . ?
C13 H13B 0.99 . ?
C14 C15 1.547(2) . ?
C14 H14A 0.99 . ?
C14 H14B 0.99 . ?
C15 H15A 0.99 . ?
C15 H15B 0.99 . ?
C17 H17A 0.98 . ?
C17 H17B 0.98 . ?
C17 H17C 0.98 . ?
C18 H18A 0.98 . ?
C18 H18B 0.98 . ?
C18 H18C 0.98 . ?
C19 H19A 0.98 . ?
C19 H19B 0.98 . ?
C19 H19C 0.98 . ?
C20 H20A 0.98 . ?
C20 H20B 0.98 . ?
C20 H20C 0.98 . ?
C21 H21A 0.98 . ?
C21 H21B 0.98 . ?
C21 H21C 0.98 . ?
C22 H22A 0.98 . ?
C22 H22B 0.98 . ?
C22 H22C 0.98 . ?
C23 H23A 0.98 . ?
C23 H23B 0.98 . ?
C23 H23C 0.98 . ?
C25 C26 1.377(2) . ?
C25 C30 1.385(2) . ?
C25 H25 0.95 . ?
C26 C27 1.387(2) . ?
C26 H26 0.95 . ?
C27 C28 1.386(3) . ?
C27 H27 0.95 . ?
C28 C29 1.382(3) . ?
C28 H28 0.95 . ?
C29 C30 1.387(2) . ?
C29 H29 0.95 . ?
C30 H30 0.95 . ?

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
O4 S1 O3 115.34(7) . . ?
O4 S1 O5 115.04(7) . . ?
O3 S1 O5 114.43(7) . . ?
O4 S1 C24 103.38(7) . . ?
O3 S1 C24 103.51(7) . . ?
O5 S1 C24 102.75(7) . . ?
O2 Si1 C23 106.54(7) . . ?
O2 Si1 C21 99.21(6) . . ?
C23 Si1 C21 113.80(7) . . ?
O2 Si1 C22 109.47(6) . . ?
C23 Si1 C22 113.36(8) . . ?
C21 Si1 C22 113.20(7) . . ?
C1 O1 B1 124.81(10) . . ?
C1 O2 Si1 130.23(9) . . ?
C1 N1 C16 118.78(11) . . ?
C1 N1 C2 122.09(11) . . ?
C16 N1 C2 119.07(11) . . ?
C16 N2 C17 122.98(11) . . ?
C16 N2 C18 122.10(12) . . ?
C17 N2 C18 114.76(11) . . ?
C16 N3 C20 122.44(11) . . ?
C16 N3 C19 123.15(11) . . ?
C20 N3 C19 114.21(11) . . ?
O1 C1 O2 122.44(12) . . ?
O1 C1 N1 122.94(12) . . ?
O2 C1 N1 114.62(12) . . ?
C7 C2 C3 124.29(13) . . ?
C7 C2 N1 116.68(12) . . ?
C3 C2 N1 118.98(12) . . ?
C2 C3 C4 114.12(13) . . ?
C2 C3 B1 122.14(12) . . ?
C4 C3 B1 123.74(12) . . ?
C5 C4 C3 123.07(13) . . ?
C5 C4 H4 118.5 . . ?
C3 C4 H4 118.5 . . ?
C6 C5 C4 120.11(13) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C7 119.39(14) . . ?
C5 C6 H6 120.3 . . ?
C7 C6 H6 120.3 . . ?
C2 C7 C6 118.94(13) . . ?
C2 C7 H7 120.5 . . ?
C6 C7 H7 120.5 . . ?
C9 C8 C15 113.36(11) . . ?
C9 C8 B1 107.11(11) . . ?
C15 C8 B1 110.81(11) . . ?
C9 C8 H8 108.5 . . ?
C15 C8 H8 108.5 . . ?
B1 C8 H8 108.5 . . ?
C10 C9 C8 113.80(12) . . ?
C10 C9 H9A 108.8 . . ?
C8 C9 H9A 108.8 . . ?
C10 C9 H9AB 108.8 . . ?
C8 C9 H9AB 108.8 . . ?
H9A C9 H9AB 107.7 . . ?
C9 C10 C11 115.11(12) . . ?
C9 C10 H10A 108.5 . . ?
C11 C10 H10A 108.5 . . ?
C9 C10 H10B 108.5 . . ?
C11 C10 H10B 108.5 . . ?
H10A C10 H10B 107.5 . . ?
C10 C11 C12 116.01(12) . . ?
C10 C11 H11A 108.3 . . ?
C12 C11 H11A 108.3 . . ?
C10 C11 H11B 108.3 . . ?
C12 C11 H11B 108.3 . . ?
H11A C11 H11B 107.4 . . ?
C13 C12 C11 111.58(12) . . ?
C13 C12 B1 109.14(12) . . ?
C11 C12 B1 110.10(11) . . ?
C13 C12 H12 108.7 . . ?
C11 C12 H12 108.7 . . ?
B1 C12 H12 108.7 . . ?
C14 C13 C12 114.47(12) . . ?
C14 C13 H13A 108.6 . . ?
C12 C13 H13A 108.6 . . ?
C14 C13 H13B 108.6 . . ?
C12 C13 H13B 108.6 . . ?
H13A C13 H13B 107.6 . . ?
C13 C14 C15 115.37(12) . . ?
C13 C14 H14A 108.4 . . ?
C15 C14 H14A 108.4 . . ?
C13 C14 H14B 108.4 . . ?
C15 C14 H14B 108.4 . . ?
H14A C14 H14B 107.5 . . ?
C8 C15 C14 116.37(12) . . ?
C8 C15 H15A 108.2 . . ?
C14 C15 H15A 108.2 . . ?
C8 C15 H15B 108.2 . . ?
C14 C15 H15B 108.2 . . ?
H15A C15 H15B 107.3 . . ?
N3 C16 N2 125.68(12) . . ?
N3 C16 N1 117.73(12) . . ?
N2 C16 N1 116.53(11) . . ?
N2 C17 H17A 109.5 . . ?
N2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 H19A 109.5 . . ?
N3 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N3 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N3 C20 H20A 109.5 . . ?
N3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si1 C21 H21A 109.5 . . ?
Si1 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si1 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si1 C22 H22A 109.5 . . ?
Si1 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si1 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si1 C23 H23A 109.5 . . ?
Si1 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Si1 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
F1 C24 F3 107.94(12) . . ?
F1 C24 F2 107.64(13) . . ?
F3 C24 F2 107.34(12) . . ?
F1 C24 S1 111.75(10) . . ?
F3 C24 S1 110.69(10) . . ?
F2 C24 S1 111.30(10) . . ?
C26 C25 C30 120.38(15) . . ?
C26 C25 H25 119.8 . . ?
C30 C25 H25 119.8 . . ?
C25 C26 C27 119.93(16) . . ?
C25 C26 H26 120 . . ?
C27 C26 H26 120 . . ?
C28 C27 C26 119.89(16) . . ?
C28 C27 H27 120.1 . . ?
C26 C27 H27 120.1 . . ?
C29 C28 C27 120.06(15) . . ?
C29 C28 H28 120 . . ?
C27 C28 H28 120 . . ?
C28 C29 C30 120.01(16) . . ?
C28 C29 H29 120 . . ?
C30 C29 H29 120 . . ?
C25 C30 C29 119.72(16) . . ?
C25 C30 H30 120.1 . . ?
C29 C30 H30 120.1 . . ?
C8 B1 C12 106.98(11) . . ?
C8 B1 C3 115.83(12) . . ?
C12 B1 C3 119.35(12) . . ?
C8 B1 O1 105.21(11) . . ?
C12 B1 O1 104.30(10) . . ?
C3 B1 O1 103.54(10) . . ?


####################################################################### 
# 
# 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_8
_database_code_depnum_ccdc_archive 'CCDC 2127870'
loop_
_audit_author_name
_audit_author_address
'Daniel Unruh'
;Texas Tech University
United States of America
;
_audit_update_record             
;
2021-12-10 deposited with the CCDC.	2022-07-22 downloaded from the CCDC.
;

_audit_creation_date             2021-03-31
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C21 H30 B F3 N3 O4 S, C F3 O3 S, 0.5(C6 H5 Cl)'
_chemical_formula_sum            'C25 H32.50 B Cl0.50 F6 N3 O7 S2'
_chemical_formula_weight         693.69
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C54  H62  F12  N8  O14  S4  '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   8.15130(10)
_cell_length_b                   12.7879(2)
_cell_length_c                   15.9378(3)
_cell_angle_alpha                70.1030(10)
_cell_angle_beta                 80.3630(10)
_cell_angle_gamma                89.3920(10)
_cell_volume                     1538.18(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    28500
_cell_measurement_temperature    99.9(4)
_cell_measurement_theta_max      77.1860
_cell_measurement_theta_min      2.9790
_shelx_estimated_absorpt_T_max   0.887
_shelx_estimated_absorpt_T_min   0.655
_exptl_absorpt_coefficient_mu    2.731
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.569
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.99a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             718
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 -2 -6 0.0680
1 -4 -10 0.0585
-3 -5 -9 0.0635
-5 -1 0 0.0912
2 5 10 0.0093
0 2 -8 0.0345
1 -7 3 0.0243
-1 7 -3 0.0150
-2 6 7 0.0344
-3 2 -8 0.0361
-1 -8 -2 0.0540

_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.045
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
3.8849 -1.7540 -5.6511 -0.1210 -0.5004 0.8573
0.9242 -4.3338 -9.5183 0.0306 0.1335 0.9906
-2.5376 -4.9801 -9.0933 0.1719 0.7218 0.6704
-5.0819 -1.1040 0.2998 0.2098 0.8737 -0.4389
1.6815 5.0442 9.6657 -0.1404 -0.5907 -0.7946
0.0763 2.3634 -8.1603 -0.7325 0.1762 0.6576
1.2826 -6.5505 3.0173 0.9725 -0.2329 -0.0090
-0.7663 6.8440 -2.5744 -0.9915 0.1299 0.0090
-1.7793 6.3161 7.3633 -0.3859 0.0494 -0.9212
-3.0886 1.8559 -7.6659 -0.6082 0.7105 0.3540
-1.3891 -7.9050 -2.1394 0.8979 0.3729 0.2338

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            42844
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.069
_diffrn_reflns_theta_max         67.069
_diffrn_reflns_theta_min         2.994
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(4)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -119.00 -35.00   0.50    1.08    --  -47.95 -46.00-100.00  168
  2  ω    -50.00  25.00   0.50    1.08    --  -47.95  46.00  48.00  150
  3  ω    -23.00  54.00   0.50    1.08    --   47.95 -46.00-100.00  154
  4  ω     35.00 119.00   0.50    1.08    --   47.95  46.00  48.00  168
  5  ω    -50.00 -14.00   0.50    4.31    --  -86.25  46.00  48.00   72
  6  ω   -159.00 -73.00   0.50    4.31    --  -86.25 -46.00-100.00  172
  7  ω     95.00 178.00   0.50    4.31    --  107.74  46.00  48.00  166
  8  ω    -20.00  18.00   0.50    1.08    --   14.00 101.00 -45.36   76
  9  ω     -1.00  31.00   0.50    1.08    --   30.00  95.00  19.59   64
 10  ω      1.00  27.00   0.50    1.08    --   34.00  98.00-152.31   52
 11  ω     11.00  43.00   0.50    1.08    --   38.00  86.00  53.06   64
 12  ω     13.00  43.00   0.50    1.08    --   42.00  90.00-105.09   60
 13  ω     12.00  39.00   0.50    1.08    --   42.00  92.00-158.78   54
 14  ω     17.00  43.00   0.50    1.08    --   46.00  90.00  73.95   52
 15  ω    -71.00  25.00   0.50    1.08    --  -47.95  77.00 150.00  192
 16  ω   -121.00 -36.00   0.50    1.08    --  -47.95 -38.00-180.00  170
 17  ω   -121.00 -36.00   0.50    1.08    --  -47.95 -38.00 -30.00  170
 18  ω   -121.00 -36.00   0.50    1.08    --  -47.95 -38.00 120.00  170
 19  ω   -120.00 -25.00   0.50    1.08    --  -47.95 -77.00 -90.00  190
 20  ω     34.00  96.00   0.50    1.08    --   47.95-125.00  60.00  124
 21  ω     25.00 120.00   0.50    1.08    --   47.95  77.00  30.00  190
 22  ω     27.00 122.00   0.50    1.08    --   50.00  77.00 135.72  190
 23  ω     32.00 126.00   0.50    1.08    --   54.00  75.00 -28.49  188
 24  ω     33.00 126.00   0.50    1.08    --   54.00  74.00-144.39  186
 25  ω     37.00 131.00   0.50    1.08    --   58.00  74.00  10.64  188
 26  ω     37.00 131.00   0.50    1.08    --   58.00  72.00 101.08  188
 27  ω     36.00 131.00   0.50    1.08    --   58.00  76.00 154.31  190
 28  ω   -135.00 -40.00   0.50    1.08    --  -62.00 -75.00 141.18  190
 29  ω     40.00  65.00   0.50    1.08    --   62.00  75.00-107.78   50
 30  ω     41.00  66.00   0.50    1.08    --   62.00  73.00 -43.79   50
 31  ω     40.00  83.00   0.50    1.08    --   62.00  76.00 120.02   86
 32  ω     40.00  67.00   0.50    1.08    --   62.00  76.00-134.48   54
 33  ω    -70.00 -45.00   0.50    1.08    --  -66.00 -73.00  44.88   50
 34  ω    -72.00 -46.00   0.50    1.08    --  -66.00 -71.00 -92.60   52
 35  ω    -73.00 -47.00   0.50    1.08    --  -66.00 -68.00 -60.49   52
 36  ω    -72.00 -46.00   0.50    1.08    --  -66.00 -71.00 122.34   52
 37  ω   -134.00-109.00   0.50    1.08    --  -66.00 -69.00 -38.16   50
 38  ω    -74.00 -47.00   0.50    1.08    --  -66.00 -69.00 -38.16   54
 39  ω    103.00 129.00   0.50    1.08    --   66.00  76.00 -97.93   52
 40  ω     44.00  69.00   0.50    1.08    --   66.00  76.00 -97.93   50
 41  ω    -77.00 -51.00   0.50    4.31    --  -70.00 -68.00 129.11   52
 42  ω    -78.00 -52.00   0.50    4.31    --  -70.00 -66.00 164.30   52
 43  ω   -139.00-113.00   0.50    4.31    --  -74.00 -68.00   5.22   52
 44  ω    -80.00 -54.00   0.50    4.31    --  -74.00 -72.00  -3.23   52
 45  ω    -81.00 -55.00   0.50    4.31    --  -74.00 -68.00   5.22   52
 46  ω    -81.00 -56.00   0.50    4.31    --  -74.00 -64.00 -73.23   50
 47  ω    -79.00 -53.00   0.50    4.31    --  -74.00 -74.00 117.41   52
 48  ω    -80.00 -54.00   0.50    4.31    --  -74.00 -70.00 -99.59   52
 49  ω    -96.00 -60.00   0.50    4.31    --  -78.00 -64.00  46.27   72
 50  ω    -87.00 -60.00   0.50    4.31    --  -78.00 -64.00-156.32   54
 51  ω     55.00  81.00   0.50    4.31    --   78.00  77.00-158.07   52
 52  ω    -80.00 -55.00   0.50    4.31    --  -78.00 -76.00  40.82   50
 53  ω    -89.00 -63.00   0.50    4.31    --  -82.00 -68.00 105.21   52
 54  ω    -90.00 -64.00   0.50    4.31    --  -82.00 -65.00-137.14   52
 55  ω    -86.00 -60.00   0.50    4.31    --  -82.00 -76.00-139.01   52
 56  ω    -93.00 -59.00   0.50    4.31    --  -82.00 -76.00 101.58   68
 57  ω    -90.00 -65.00   0.50    4.31    --  -86.25 -72.00 122.19   50
 58  ω    -40.00 -13.00   0.50    4.31    --  -86.25  38.00  90.00   54
 59  ω   -123.00 -97.00   0.50    4.31    --  -86.25 -77.00-150.00   52
 60  ω    -94.00 -66.00   0.50    4.31    --  -86.25 -70.00-118.59   56
 61  ω   -159.00-108.00   0.50    4.31    --  -86.25 -77.00  41.73  102
 62  ω    -89.00 -63.00   0.50    4.31    --  -86.25 -77.00  60.00   52
 63  ω   -100.00 -65.00   0.50    4.31    --  -86.25 -75.00 -14.07   70
 64  ω   -110.00 -63.00   0.50    4.31    --  -86.25 -77.00  90.00   94
 65  ω   -101.00 -65.00   0.50    4.31    --  -86.25 -74.00  19.85   72
 66  ω    -88.00 -63.00   0.50    4.31    --  -86.25 -77.00-180.00   50
 67  ω   -159.00-110.00   0.50    4.31    --  -86.25 -77.00-180.00   98
 68  ω    -91.00 -65.00   0.50    4.31    --  -86.25 -77.00   0.00   52
 69  ω   -102.00 -63.00   0.50    4.31    --  -86.25 -77.00 -30.00   78
 70  ω   -145.00-119.00   0.50    4.31    --  -86.25 -77.00   0.00   52
 71  ω   -104.00 -66.00   0.50    4.31    --  -86.25 -77.00 -90.00   76
 72  ω   -152.00-119.00   0.50    4.31    --  -86.25 -57.00 120.00   66
 73  ω   -138.00 -66.00   0.50    4.31    --  -86.25 -74.00-174.01  144
 74  ω    -92.00 -63.00   0.50    4.31    --  -86.25 -77.00 150.00   58
 75  ω    -92.00 -66.00   0.50    4.31    --  -86.25 -73.00   5.29   52
 76  ω    -97.00 -67.00   0.50    4.31    --  -86.25 -68.00 158.49   60
 77  ω   -154.00-128.00   0.50    4.31    --  -86.25 -77.00 150.00   52
 78  ω    -98.00 -68.00   0.50    4.31    --  -86.25 -68.00 -59.90   60
 79  ω    -63.00 -30.00   0.50    4.31    --  -86.25  57.00-150.00   66
 80  ω    -88.00 -63.00   0.50    4.31    --  -86.25 -77.00  41.73   50
 81  ω    -96.00 -66.00   0.50    4.31    --  -86.25 -72.00 -83.77   60
 82  ω    -90.00 -63.00   0.50    4.31    --  -86.25 -77.00-150.00   54
 83  ω    -90.00 -64.00   0.50    4.31    --  -86.25 -75.00 -59.93   52
 84  ω     72.00 155.00   0.50    4.31    --   90.00  69.00  43.11  166
 85  ω     97.00 178.00   0.50    4.31    --  107.74  38.00-120.00  162
 86  ω     85.00 128.00   0.50    4.31    --  107.74  77.00 120.00   86
 87  ω     70.00 106.00   0.50    4.31    --  107.74 -99.00  30.00   72
 88  ω     38.00  68.00   0.50    4.31    --  107.74 -57.00-150.00   60
 89  ω     35.00  65.00   0.50    4.31    --  107.74 -57.00  30.00   60
 90  ω     86.00 157.00   0.50    4.31    --  107.74  77.00  60.00  142
 91  ω     36.00  61.00   0.50    4.31    --  107.74 -99.00  30.00   50
 92  ω     66.00 106.00   0.50    4.31    --  107.74 -99.00-120.00   80
 93  ω     39.00  65.00   0.50    4.31    --  107.74 -99.00-120.00   52
 94  ω    102.00 168.00   0.50    4.31    --  107.74  38.00 120.00  132
 95  ω     35.00  74.00   0.50    4.31    --  107.74 -99.00 -60.00   78
 96  ω     88.00 175.00   0.50    4.31    --  107.74  77.00  30.00  174
 97  ω     96.00 178.00   0.50    4.31    --  107.74  38.00 -60.00  164
 98  ω     75.00 105.00   0.50    4.31    --  107.74 -99.00  90.00   60
 99  ω     35.00  71.00   0.50    4.31    --  107.74 -99.00  90.00   72
100  ω    106.00 176.00   0.50    4.31    --  107.74  38.00-150.00  140
101  ω     88.00 174.00   0.50    4.31    --  107.74  77.00 -90.00  172
102  ω     77.00 106.00   0.50    4.31    --  107.74 -99.00 120.00   58
103  ω     95.00 175.00   0.50    4.31    --  107.74 125.00 -30.00  160
104  ω     46.00  72.00   0.50    4.31    --  107.74 -99.00 120.00   52
105  ω     35.00 109.00   0.50    4.31    --  107.74-125.00  30.00  148
106  ω    112.00 160.00   0.50    4.31    --  107.74  77.00 150.00   96
107  ω     39.00  68.00   0.50    4.31    --  107.74 -57.00 -90.00   58
108  ω    102.00 155.00   0.50    4.31    --  107.74  38.00   0.00  106
109  ω     39.00  64.00   0.50    4.31    --  107.74 -57.00   0.00   50
110  ω    121.00 173.00   0.50    4.31    --  107.74  38.00 -30.00  104
111  ω     37.00 107.00   0.50    4.31    --  107.74 -77.00 120.00  140
112  ω     77.00 103.00   0.50    4.31    --  107.74 -99.00 -60.00   52
113  ω     35.00  65.00   0.50    4.31    --  107.74 -57.00  60.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0107558000
_diffrn_orient_matrix_UB_12      -0.1260833000
_diffrn_orient_matrix_UB_13      0.0531454000
_diffrn_orient_matrix_UB_21      -0.1712932000
_diffrn_orient_matrix_UB_22      -0.0100106000
_diffrn_orient_matrix_UB_23      -0.0260945000
_diffrn_orient_matrix_UB_31      0.0859345000
_diffrn_orient_matrix_UB_32      -0.0214079000
_diffrn_orient_matrix_UB_33      -0.0859803000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4650
_reflns_number_total             5438
_reflns_odcompleteness_completeness 99.14
_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 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.00104(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         5438
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0390
_refine_ls_restrained_S_all      1.061
_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)+(0.0435P)²+0.8547P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1013
_refine_special_details          
'The interstitial chlorobenzene molecule was positionally disordered about an inversion site. Atoms Cl1 and C23 < C28 had their site occupancies constrained to 0.5.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: Cl1(0.5) C23(0.5) C28(0.5) H28(0.5) C27(0.5) H27(0.5) C26(0.5)
 H26(0.5) C25(0.5) H25(0.5) C24(0.5) H24(0.5)
3.a Ternary CH refined with riding coordinates:
 C13(H13), C17(H17)
3.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C18(H18A,H18B), C19(H19A,
 H19B), C20(H20A,H20B)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C28(H28), C27(H27), C26(H26), C25(H25),
 C24(H24)
3.d Fitted hexagon refined as free rotating group:
 C23(C28,C27,C26,C25,C24)
3.e Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.20570(8) 0.52090(4) 0.56791(4) 0.04709(18) Uani 1 1 d . . . . .
F1 F 0.09329(18) 0.69383(12) 0.60386(10) 0.0566(4) Uani 1 1 d . . . . .
F2 F 0.0677(2) 0.69119(12) 0.47318(12) 0.0769(5) Uani 1 1 d . . . . .
F3 F 0.30592(18) 0.72864(11) 0.50005(10) 0.0577(4) Uani 1 1 d . . . . .
O1 O 0.38794(19) 0.35077(11) 0.67981(10) 0.0402(4) Uani 1 1 d . . . . .
O2 O 0.32467(19) 0.53181(11) 0.63625(10) 0.0379(4) Uani 1 1 d . . . . .
O3 O 0.3024(3) 0.50007(18) 0.49424(14) 0.0801(7) Uani 1 1 d . . . . .
O4 O 0.0578(3) 0.46025(15) 0.61678(16) 0.0795(7) Uani 1 1 d . . . . .
N1 N 0.4784(2) 0.46637(12) 0.74628(10) 0.0274(3) Uani 1 1 d . . . . .
N2 N 0.52704(18) 0.66082(12) 0.69435(10) 0.0246(3) Uani 1 1 d . . . . .
N3 N 0.37124(19) 0.56785(13) 0.83822(10) 0.0278(4) Uani 1 1 d . . . . .
C1 C 0.3998(3) 0.44123(16) 0.68810(14) 0.0330(5) Uani 1 1 d . . . . .
C2 C 0.5786(2) 0.38401(15) 0.80204(12) 0.0281(4) Uani 1 1 d . . . . .
C3 C 0.5561(3) 0.27182(15) 0.81256(13) 0.0315(4) Uani 1 1 d . . . . .
C4 C 0.6593(3) 0.20154(17) 0.86789(14) 0.0374(5) Uani 1 1 d . . . . .
H4 H 0.651252 0.123959 0.878195 0.045 Uiso 1 1 calc R U . . .
C5 C 0.7719(3) 0.24037(17) 0.90797(14) 0.0374(5) Uani 1 1 d . . . . .
H5 H 0.836556 0.189225 0.945997 0.045 Uiso 1 1 calc R U . . .
C6 C 0.7911(2) 0.35296(17) 0.89311(13) 0.0333(4) Uani 1 1 d . . . . .
H6 H 0.870028 0.379630 0.919615 0.040 Uiso 1 1 calc R U . . .
C7 C 0.6934(2) 0.42631(16) 0.83894(13) 0.0297(4) Uani 1 1 d . . . . .
H7 H 0.704800 0.504072 0.827311 0.036 Uiso 1 1 calc R U . . .
C8 C 0.4569(2) 0.57085(15) 0.76008(12) 0.0251(4) Uani 1 1 d . . . . .
C9 C 0.6693(2) 0.65769(16) 0.62572(13) 0.0317(4) Uani 1 1 d . . . . .
H9A H 0.633408 0.675578 0.566931 0.047 Uiso 1 1 calc R U . . .
H9B H 0.713046 0.583061 0.642972 0.047 Uiso 1 1 calc R U . . .
H9C H 0.756612 0.712322 0.621361 0.047 Uiso 1 1 calc R U . . .
C10 C 0.4650(2) 0.77218(15) 0.68298(14) 0.0309(4) Uani 1 1 d . . . . .
H10A H 0.538206 0.813273 0.705137 0.046 Uiso 1 1 calc R U . . .
H10B H 0.351855 0.765192 0.717538 0.046 Uiso 1 1 calc R U . . .
H10C H 0.463595 0.812388 0.618659 0.046 Uiso 1 1 calc R U . . .
C11 C 0.2536(3) 0.47412(18) 0.89477(15) 0.0418(5) Uani 1 1 d . . . . .
H11A H 0.155889 0.502359 0.923609 0.063 Uiso 1 1 calc R U . . .
H11B H 0.308103 0.422338 0.941558 0.063 Uiso 1 1 calc R U . . .
H11C H 0.218545 0.435287 0.856788 0.063 Uiso 1 1 calc R U . . .
C12 C 0.3981(3) 0.65094(18) 0.88053(14) 0.0349(5) Uani 1 1 d . . . . .
H12A H 0.305333 0.700805 0.875609 0.052 Uiso 1 1 calc R U . . .
H12B H 0.502574 0.694415 0.849508 0.052 Uiso 1 1 calc R U . . .
H12C H 0.404334 0.612839 0.944581 0.052 Uiso 1 1 calc R U . . .
C13 C 0.4814(3) 0.14327(17) 0.71202(14) 0.0378(5) Uani 1 1 d . . . . .
H13 H 0.594261 0.169687 0.674781 0.045 Uiso 1 1 calc R U . . .
C14 C 0.3575(3) 0.14648(19) 0.64832(15) 0.0431(5) Uani 1 1 d . . . . .
H14A H 0.365049 0.221933 0.602070 0.052 Uiso 1 1 calc R U . . .
H14B H 0.391207 0.093419 0.616350 0.052 Uiso 1 1 calc R U . . .
C15 C 0.1754(3) 0.11790(19) 0.69584(17) 0.0461(6) Uani 1 1 d . . . . .
H15A H 0.102957 0.139413 0.649228 0.055 Uiso 1 1 calc R U . . .
H15B H 0.160296 0.036234 0.726562 0.055 Uiso 1 1 calc R U . . .
C16 C 0.1170(3) 0.17444(19) 0.76581(17) 0.0448(5) Uani 1 1 d . . . . .
H16A H 0.014539 0.133591 0.805708 0.054 Uiso 1 1 calc R U . . .
H16B H 0.086810 0.250970 0.733173 0.054 Uiso 1 1 calc R U . . .
C17 C 0.2434(3) 0.18150(17) 0.82603(15) 0.0389(5) Uani 1 1 d . . . . .
H17 H 0.203739 0.234658 0.857900 0.047 Uiso 1 1 calc R U . . .
C18 C 0.2687(3) 0.06755(18) 0.89794(15) 0.0442(5) Uani 1 1 d . . . . .
H18A H 0.342906 0.079840 0.937289 0.053 Uiso 1 1 calc R U . . .
H18B H 0.159684 0.037310 0.936568 0.053 Uiso 1 1 calc R U . . .
C19 C 0.3435(3) -0.01970(18) 0.85759(16) 0.0481(6) Uani 1 1 d . . . . .
H19A H 0.379424 -0.082203 0.906545 0.058 Uiso 1 1 calc R U . . .
H19B H 0.255292 -0.049619 0.834990 0.058 Uiso 1 1 calc R U . . .
C20 C 0.4922(3) 0.02434(17) 0.78011(16) 0.0446(5) Uani 1 1 d . . . . .
H20A H 0.506655 -0.027773 0.745872 0.053 Uiso 1 1 calc R U . . .
H20B H 0.593648 0.023015 0.806971 0.053 Uiso 1 1 calc R U . . .
C21 C 0.1653(3) 0.66933(18) 0.53375(15) 0.0397(5) Uani 1 1 d . . . . .
B1 B 0.4254(3) 0.22391(18) 0.76809(16) 0.0342(5) Uani 1 1 d . . . . .
S2 S 0.08505(6) 0.28226(4) 1.16997(3) 0.03233(14) Uani 1 1 d . . . . .
F4 F 0.04707(18) 0.20840(13) 1.04100(10) 0.0605(4) Uani 1 1 d . . . . .
F5 F 0.30073(15) 0.21512(10) 1.05991(9) 0.0437(3) Uani 1 1 d . . . . .
F6 F 0.12931(19) 0.08641(11) 1.15481(11) 0.0633(4) Uani 1 1 d . . . . .
O5 O 0.0988(2) 0.39191(13) 1.10289(12) 0.0568(5) Uani 1 1 d . . . . .
O6 O -0.08087(17) 0.24003(15) 1.21589(10) 0.0474(4) Uani 1 1 d . . . . .
O7 O 0.20821(18) 0.26372(15) 1.22746(10) 0.0473(4) Uani 1 1 d . . . . .
C22 C 0.1433(3) 0.19289(17) 1.10377(14) 0.0351(5) Uani 1 1 d . . . . .
Cl1 Cl 0.32021(16) 0.98029(11) 0.47668(9) 0.0476(3) Uani 0.5 1 d . . P A -1
C23 C 0.1097(3) 0.9947(3) 0.4934(2) 0.0297(9) Uani 0.5 1 d G . P A -1
C28 C 0.0274(4) 1.0412(3) 0.42066(17) 0.0342(14) Uani 0.5 1 d G . P A -1
H28 H 0.088298 1.066096 0.360537 0.041 Uiso 0.5 1 calc R U P A -1
C27 C -0.1440(4) 1.0514(2) 0.4359(2) 0.0423(11) Uani 0.5 1 d G . P A -1
H27 H -0.200260 1.083235 0.386118 0.051 Uiso 0.5 1 calc R U P A -1
C26 C -0.2331(3) 1.0151(3) 0.5238(2) 0.0477(14) Uani 0.5 1 d G . P A -1
H26 H -0.350253 1.022011 0.534220 0.057 Uiso 0.5 1 calc R U P A -1
C25 C -0.1508(4) 0.9685(3) 0.59661(17) 0.0408(10) Uani 0.5 1 d G . P A -1
H25 H -0.211689 0.943645 0.656741 0.049 Uiso 0.5 1 calc R U P A -1
C24 C 0.0206(4) 0.9583(3) 0.58142(19) 0.0407(17) Uani 0.5 1 d G . P A -1
H24 H 0.076870 0.926504 0.631162 0.049 Uiso 0.5 1 calc R U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O2 1.6145(14) . ?
S1 O3 1.403(2) . ?
S1 O4 1.398(2) . ?
S1 C21 1.831(2) . ?
F1 C21 1.306(3) . ?
F2 C21 1.308(2) . ?
F3 C21 1.309(3) . ?
O1 C1 1.215(2) . ?
O1 B1 1.812(3) . ?
O2 C1 1.379(2) . ?
N1 C1 1.334(2) . ?
N1 C2 1.468(2) . ?
N1 C8 1.430(2) . ?
N2 C8 1.319(2) . ?
N2 C9 1.465(2) . ?
N2 C10 1.468(2) . ?
N3 C8 1.310(2) . ?
N3 C11 1.472(2) . ?
N3 C12 1.474(3) . ?
C2 C3 1.397(3) . ?
C2 C7 1.388(3) . ?
C3 C4 1.409(3) . ?
C3 B1 1.605(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.385(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.383(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.387(3) . ?
C7 H7 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13 1.0000 . ?
C13 C14 1.538(3) . ?
C13 C20 1.551(3) . ?
C13 B1 1.597(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.536(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.535(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.544(3) . ?
C17 H17 1.0000 . ?
C17 C18 1.554(3) . ?
C17 B1 1.602(3) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.541(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.533(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
S2 O5 1.4369(16) . ?
S2 O6 1.4393(15) . ?
S2 O7 1.4348(15) . ?
S2 C22 1.813(2) . ?
F4 C22 1.334(2) . ?
F5 C22 1.337(2) . ?
F6 C22 1.322(2) . ?
Cl1 C23 1.710(3) . ?
C23 C28 1.3900 . ?
C23 C24 1.3900 . ?
C28 H28 0.9500 . ?
C28 C27 1.3900 . ?
C27 H27 0.9500 . ?
C27 C26 1.3900 . ?
C26 H26 0.9500 . ?
C26 C25 1.3900 . ?
C25 H25 0.9500 . ?
C25 C24 1.3900 . ?
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
O2 S1 C21 91.92(8) . . ?
O3 S1 O2 109.45(11) . . ?
O3 S1 C21 108.74(12) . . ?
O4 S1 O2 110.28(11) . . ?
O4 S1 O3 123.46(15) . . ?
O4 S1 C21 108.38(12) . . ?
C1 O1 B1 121.46(16) . . ?
C1 O2 S1 121.90(12) . . ?
C1 N1 C2 120.43(16) . . ?
C1 N1 C8 120.62(15) . . ?
C8 N1 C2 118.80(15) . . ?
C8 N2 C9 123.05(16) . . ?
C8 N2 C10 122.27(16) . . ?
C9 N2 C10 114.66(14) . . ?
C8 N3 C11 122.00(17) . . ?
C8 N3 C12 122.79(16) . . ?
C11 N3 C12 114.90(17) . . ?
O1 C1 O2 121.11(18) . . ?
O1 C1 N1 126.89(18) . . ?
N1 C1 O2 111.98(16) . . ?
C3 C2 N1 119.24(17) . . ?
C7 C2 N1 115.73(16) . . ?
C7 C2 C3 125.01(18) . . ?
C2 C3 C4 113.56(18) . . ?
C2 C3 B1 124.68(17) . . ?
C4 C3 B1 121.75(18) . . ?
C3 C4 H4 118.5 . . ?
C5 C4 C3 123.03(19) . . ?
C5 C4 H4 118.5 . . ?
C4 C5 H5 119.7 . . ?
C6 C5 C4 120.59(19) . . ?
C6 C5 H5 119.7 . . ?
C5 C6 H6 120.5 . . ?
C5 C6 C7 119.01(19) . . ?
C7 C6 H6 120.5 . . ?
C2 C7 H7 120.6 . . ?
C6 C7 C2 118.76(18) . . ?
C6 C7 H7 120.6 . . ?
N2 C8 N1 117.60(16) . . ?
N3 C8 N1 116.49(16) . . ?
N3 C8 N2 125.90(17) . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 H12A 109.5 . . ?
N3 C12 H12B 109.5 . . ?
N3 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 H13 108.8 . . ?
C14 C13 C20 112.04(18) . . ?
C14 C13 B1 109.81(18) . . ?
C20 C13 H13 108.8 . . ?
C20 C13 B1 108.40(17) . . ?
B1 C13 H13 108.8 . . ?
C13 C14 H14A 108.6 . . ?
C13 C14 H14B 108.6 . . ?
H14A C14 H14B 107.6 . . ?
C15 C14 C13 114.51(19) . . ?
C15 C14 H14A 108.6 . . ?
C15 C14 H14B 108.6 . . ?
C14 C15 H15A 108.6 . . ?
C14 C15 H15B 108.6 . . ?
H15A C15 H15B 107.6 . . ?
C16 C15 C14 114.76(18) . . ?
C16 C15 H15A 108.6 . . ?
C16 C15 H15B 108.6 . . ?
C15 C16 H16A 108.3 . . ?
C15 C16 H16B 108.3 . . ?
C15 C16 C17 116.01(19) . . ?
H16A C16 H16B 107.4 . . ?
C17 C16 H16A 108.3 . . ?
C17 C16 H16B 108.3 . . ?
C16 C17 H17 108.8 . . ?
C16 C17 C18 113.46(18) . . ?
C16 C17 B1 112.01(18) . . ?
C18 C17 H17 108.8 . . ?
C18 C17 B1 104.95(18) . . ?
B1 C17 H17 108.8 . . ?
C17 C18 H18A 108.7 . . ?
C17 C18 H18B 108.7 . . ?
H18A C18 H18B 107.6 . . ?
C19 C18 C17 114.19(19) . . ?
C19 C18 H18A 108.7 . . ?
C19 C18 H18B 108.7 . . ?
C18 C19 H19A 108.6 . . ?
C18 C19 H19B 108.6 . . ?
H19A C19 H19B 107.6 . . ?
C20 C19 C18 114.61(17) . . ?
C20 C19 H19A 108.6 . . ?
C20 C19 H19B 108.6 . . ?
C13 C20 H20A 108.2 . . ?
C13 C20 H20B 108.2 . . ?
C19 C20 C13 116.46(19) . . ?
C19 C20 H20A 108.2 . . ?
C19 C20 H20B 108.2 . . ?
H20A C20 H20B 107.3 . . ?
F1 C21 S1 110.12(15) . . ?
F1 C21 F2 109.8(2) . . ?
F1 C21 F3 108.34(18) . . ?
F2 C21 S1 108.29(15) . . ?
F2 C21 F3 110.46(19) . . ?
F3 C21 S1 109.83(16) . . ?
C3 B1 O1 99.93(14) . . ?
C13 B1 O1 102.07(16) . . ?
C13 B1 C3 121.20(19) . . ?
C13 B1 C17 108.13(17) . . ?
C17 B1 O1 103.50(16) . . ?
C17 B1 C3 118.44(18) . . ?
O5 S2 O6 116.12(11) . . ?
O5 S2 C22 103.50(10) . . ?
O6 S2 C22 102.78(10) . . ?
O7 S2 O5 113.56(11) . . ?
O7 S2 O6 115.02(9) . . ?
O7 S2 C22 103.53(10) . . ?
F4 C22 S2 110.42(15) . . ?
F4 C22 F5 106.87(17) . . ?
F5 C22 S2 111.67(13) . . ?
F6 C22 S2 111.95(15) . . ?
F6 C22 F4 108.27(17) . . ?
F6 C22 F5 107.45(17) . . ?
C28 C23 Cl1 121.0(2) . . ?
C28 C23 C24 120.0 . . ?
C24 C23 Cl1 119.0(2) . . ?
C23 C28 H28 120.0 . . ?
C27 C28 C23 120.0 . . ?
C27 C28 H28 120.0 . . ?
C28 C27 H27 120.0 . . ?
C26 C27 C28 120.0 . . ?
C26 C27 H27 120.0 . . ?
C27 C26 H26 120.0 . . ?
C27 C26 C25 120.0 . . ?
C25 C26 H26 120.0 . . ?
C26 C25 H25 120.0 . . ?
C24 C25 C26 120.0 . . ?
C24 C25 H25 120.0 . . ?
C23 C24 H24 120.0 . . ?
C25 C24 C23 120.0 . . ?
C25 C24 H24 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
S1 O2 C1 O1 4.9(3) . . . . ?
S1 O2 C1 N1 -173.59(14) . . . . ?
O2 S1 C21 F1 -60.92(16) . . . . ?
O2 S1 C21 F2 179.01(17) . . . . ?
O2 S1 C21 F3 58.31(16) . . . . ?
O3 S1 O2 C1 -70.12(19) . . . . ?
O3 S1 C21 F1 -172.22(16) . . . . ?
O3 S1 C21 F2 67.7(2) . . . . ?
O3 S1 C21 F3 -52.99(19) . . . . ?
O4 S1 O2 C1 68.81(19) . . . . ?
O4 S1 C21 F1 51.20(19) . . . . ?
O4 S1 C21 F2 -68.9(2) . . . . ?
O4 S1 C21 F3 170.44(16) . . . . ?
N1 C2 C3 C4 -179.76(17) . . . . ?
N1 C2 C3 B1 -0.4(3) . . . . ?
N1 C2 C7 C6 179.37(17) . . . . ?
C1 O1 B1 C3 -28.8(2) . . . . ?
C1 O1 B1 C13 -153.89(19) . . . . ?
C1 O1 B1 C17 93.9(2) . . . . ?
C1 N1 C2 C3 -17.2(3) . . . . ?
C1 N1 C2 C7 161.28(18) . . . . ?
C1 N1 C8 N2 -71.9(2) . . . . ?
C1 N1 C8 N3 109.3(2) . . . . ?
C2 N1 C1 O1 7.0(3) . . . . ?
C2 N1 C1 O2 -174.59(16) . . . . ?
C2 N1 C8 N2 112.47(19) . . . . ?
C2 N1 C8 N3 -66.3(2) . . . . ?
C2 C3 C4 C5 0.1(3) . . . . ?
C2 C3 B1 O1 18.9(2) . . . . ?
C2 C3 B1 C13 129.6(2) . . . . ?
C2 C3 B1 C17 -92.5(2) . . . . ?
C3 C2 C7 C6 -2.2(3) . . . . ?
C3 C4 C5 C6 -1.6(3) . . . . ?
C4 C3 B1 O1 -161.85(18) . . . . ?
C4 C3 B1 C13 -51.1(3) . . . . ?
C4 C3 B1 C17 86.8(3) . . . . ?
C4 C5 C6 C7 1.3(3) . . . . ?
C5 C6 C7 C2 0.5(3) . . . . ?
C7 C2 C3 C4 1.9(3) . . . . ?
C7 C2 C3 B1 -178.79(19) . . . . ?
C8 N1 C1 O1 -168.5(2) . . . . ?
C8 N1 C1 O2 9.9(3) . . . . ?
C8 N1 C2 C3 158.38(17) . . . . ?
C8 N1 C2 C7 -23.1(2) . . . . ?
C9 N2 C8 N1 -22.8(2) . . . . ?
C9 N2 C8 N3 155.88(18) . . . . ?
C10 N2 C8 N1 155.54(16) . . . . ?
C10 N2 C8 N3 -25.8(3) . . . . ?
C11 N3 C8 N1 -21.6(3) . . . . ?
C11 N3 C8 N2 159.72(18) . . . . ?
C12 N3 C8 N1 151.60(16) . . . . ?
C12 N3 C8 N2 -27.1(3) . . . . ?
C13 C14 C15 C16 44.9(3) . . . . ?
C14 C13 C20 C19 -73.5(2) . . . . ?
C14 C13 B1 O1 -48.7(2) . . . . ?
C14 C13 B1 C3 -158.30(18) . . . . ?
C14 C13 B1 C17 60.1(2) . . . . ?
C14 C15 C16 C17 -40.1(3) . . . . ?
C15 C16 C17 C18 -72.1(2) . . . . ?
C15 C16 C17 B1 46.5(3) . . . . ?
C16 C17 C18 C19 63.6(3) . . . . ?
C16 C17 B1 O1 52.0(2) . . . . ?
C16 C17 B1 C3 161.43(18) . . . . ?
C16 C17 B1 C13 -55.7(2) . . . . ?
C17 C18 C19 C20 45.4(3) . . . . ?
C18 C17 B1 O1 175.58(15) . . . . ?
C18 C17 B1 C3 -75.0(2) . . . . ?
C18 C17 B1 C13 67.8(2) . . . . ?
C18 C19 C20 C13 -39.2(3) . . . . ?
C20 C13 C14 C15 64.8(2) . . . . ?
C20 C13 B1 O1 -171.39(16) . . . . ?
C20 C13 B1 C3 79.0(2) . . . . ?
C20 C13 B1 C17 -62.6(2) . . . . ?
C21 S1 O2 C1 179.22(17) . . . . ?
B1 O1 C1 O2 -160.06(17) . . . . ?
B1 O1 C1 N1 18.2(3) . . . . ?
B1 C3 C4 C5 -179.3(2) . . . . ?
B1 C13 C14 C15 -55.7(2) . . . . ?
B1 C13 C20 C19 47.8(3) . . . . ?
B1 C17 C18 C19 -59.0(2) . . . . ?
O5 S2 C22 F4 -56.00(17) . . . . ?
O5 S2 C22 F5 62.76(16) . . . . ?
O5 S2 C22 F6 -176.71(15) . . . . ?
O6 S2 C22 F4 65.24(16) . . . . ?
O6 S2 C22 F5 -176.00(14) . . . . ?
O6 S2 C22 F6 -55.47(16) . . . . ?
O7 S2 C22 F4 -174.72(14) . . . . ?
O7 S2 C22 F5 -55.96(16) . . . . ?
O7 S2 C22 F6 64.57(16) . . . . ?
Cl1 C23 C28 C27 179.6(3) . . . . ?
Cl1 C23 C24 C25 -179.6(3) . . . . ?
C23 C28 C27 C26 0.0 . . . . ?
C28 C23 C24 C25 0.0 . . . . ?
C28 C27 C26 C25 0.0 . . . . ?
C27 C26 C25 C24 0.0 . . . . ?
C26 C25 C24 C23 0.0 . . . . ?
C24 C23 C28 C27 0.0 . . . . ?

_olex2_exptl_crystal_mounting_method 'Hampton Reserach 20 micron nylon CryoLoop'
_olex2_submission_original_sample_id kre21_10
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   6138
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.871
_oxdiff_exptl_absorpt_empirical_full_min 0.476
# start Validation Reply Form
_vrf_PLAT230_8                   
;
PROBLEM: Hirshfeld Test Diff for    N1       --C1       .        5.5 s.u.  
RESPONSE: The correct atom assignments for these positions were confirmed by 
          NMR spectroscopy.
;
_vrf_PLAT410_8                   
;
PROBLEM: Short Intra H...H Contact  H15B     ..H19B     .       1.98 Ang.  
RESPONSE: This is a typically distance for hydrogen atoms across from each 
          other when the bicyclo(3.3.1)nonan-9-ane moiety is in the
          boat-boat configuration.
;
_vrf_PLAT906_8                   
;
PROBLEM: Large K Value in the Analysis of Variance ......      2.423 Check 
RESPONSE: The crystals were weak diffractors at high angles.
;
_vrf_PLAT911_8                   
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.597         46 Report
RESPONSE: These reflections were omitted during the absorption correction.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_11
_database_code_depnum_ccdc_archive 'CCDC 2127872'
loop_
_audit_author_name
_audit_author_address
'Daniel Unruh'
;Texas Tech University
United States of America
;
_audit_update_record             
;
2021-12-10 deposited with the CCDC.	2022-07-22 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT230_11                  
;
PROBLEM: Hirshfeld Test Diff for    O3       --C2       .        5.7 s.u.  
RESPONSE: This is due to slight rotation that elongates the ADP for the O3
          atom. In both cases the atom identies were both confirmed by other 
          technique or through the synthesis method.
;
_vrf_PLAT410_11                  
;
PROBLEM: Short Intra H...H Contact  H17B     ..H21B     .       1.96 Ang.  
RESPONSE: This is a typical distance between hydrogen atoms when the 
          9-Borabicyclo(3.3.1)nonane is in the boat-boat configuration.
;
_vrf_PLAT911_11                  
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         56 Report
RESPONSE: These reflections were omitted during the absorption correction.
;
# end Validation Reply Form


_audit_creation_date             2021-03-01
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C40 H60 B2 N6 O3, 2(C F3 O3 S), C H2 Cl2'
_chemical_formula_sum            'C43 H62 B2 Cl2 F6 N6 O9 S2'
_chemical_formula_weight         1077.62
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C88  H124  B2  Cl4  F12  N12  O18  S4  '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   12.96610(10)
_cell_length_b                   13.2799(2)
_cell_length_c                   15.5932(2)
_cell_angle_alpha                74.5510(10)
_cell_angle_beta                 83.6470(10)
_cell_angle_gamma                75.3530(10)
_cell_volume                     2501.15(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    30378
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      77.2980
_cell_measurement_theta_min      2.9320
_shelx_estimated_absorpt_T_max   0.738
_shelx_estimated_absorpt_T_min   0.644
_exptl_absorpt_coefficient_mu    2.652
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.581
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.99a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1128
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 0 -1 0.0635
5 6 -3 0.0737
8 0 3 0.0873
0 -6 5 0.0804
-8 -4 0 0.0711
4 -3 -8 0.0443
-3 -7 -8 0.0611
-2 5 9 0.0664
7 2 -3 0.0663
5 7 6 0.0886
-6 0 6 0.0809
0 -2 9 0.0613
-6 -2 -7 0.0613
-7 3 3 0.0613
1 9 3 0.0670
-2 7 3 0.0636
-1 -8 -3 0.0775
2 -2 -9 0.0550
-4 -5 -9 0.0594
5 -5 -4 0.0778

_exptl_crystal_recrystallization_method 'Slow evaporation from dichloromethane'
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.122
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
-1.9988 0.0001 -0.9995 0.0266 0.1787 0.1895
4.8824 6.4471 -2.9326 0.1352 0.5602 -0.8172
7.6530 -0.3555 3.3174 -0.1602 -0.6731 -0.7220
0.1765 -6.1365 4.7128 -0.2217 -0.9242 0.3108
-8.0283 -4.1553 -0.0544 0.0070 0.0347 0.9994
3.9438 -2.9181 -7.9287 -0.8656 0.2067 -0.4560
-2.8898 -6.7755 -8.0331 -0.8887 0.2133 0.4058
-1.6297 4.7310 8.7509 0.9600 -0.2297 0.1601
7.4962 1.9480 -3.4315 -0.3648 0.0862 -0.9271
5.3218 6.9462 6.2036 0.6915 -0.1665 -0.7029
-6.2447 0.3211 5.8774 0.6360 -0.1513 0.7567
0.3667 -1.7140 9.0119 0.3753 -0.9040 0.2049
-6.4989 -1.9983 -7.1406 -0.3010 0.7273 0.6168
-6.5710 3.1962 2.6706 0.6918 0.3753 0.6169
1.0628 8.5427 2.9779 0.8116 0.4418 -0.3822
-2.2028 7.4144 3.2826 0.8785 0.4777 0.0091
-0.6005 -8.4639 -3.0515 -0.8293 -0.4514 0.3293
2.0082 -2.1171 -9.4697 -0.8094 0.4958 -0.3147
-3.6494 -5.0988 -9.0463 -0.7817 0.4778 0.4007
4.9437 -5.0556 -3.9557 -0.8463 -0.3517 -0.4001

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            41852
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.464
_diffrn_reflns_theta_min         2.943
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -83.00  -3.00   0.50    0.20    --  -47.95 112.00 171.00  160
  2  ω     25.00  89.00   0.50    0.20    --   47.95-112.00  79.00  128
  3  ω    -82.00 -13.00   0.50    0.81    --  -86.25 112.00 171.00  138
  4  ω   -159.00 -81.00   0.50    0.81    --  -86.25-112.00  79.00  156
  5  ω    103.00 178.00   0.50    0.81    --  107.74 112.00 171.00  150
  6  ω     35.00 108.00   0.50    0.81    --  107.74-112.00  79.00  146
  7  ω    -71.00  25.00   0.50    0.20    --  -47.95  77.00 -60.00  192
  8  ω   -120.00 -73.00   0.50    0.20    --  -47.95-125.00   0.00   94
  9  ω    -24.00  28.00   0.50    0.20    --  -47.95  19.00-120.00  104
 10  ω   -120.00 -73.00   0.50    0.20    --  -47.95-125.00-120.00   94
 11  ω    -86.00 -13.00   0.50    0.20    --  -47.95 125.00  90.00  146
 12  ω   -120.00 -73.00   0.50    0.20    --  -47.95-125.00 -90.00   94
 13  ω    -24.00  28.00   0.50    0.20    --  -47.95  19.00   0.00  104
 14  ω    -25.00  45.00   0.50    0.20    --   47.95 -38.00 150.00  140
 15  ω    -41.00 -13.00   0.50    0.81    --  -86.25  38.00  90.00   56
 16  ω   -159.00 -73.00   0.50    0.81    --  -86.25 -38.00 -30.00  172
 17  ω    -41.00 -13.00   0.50    0.81    --  -86.25  38.00 120.00   56
 18  ω    -41.00 -13.00   0.50    0.81    --  -86.25  38.00 -60.00   56
 19  ω    -41.00 -13.00   0.50    0.81    --  -86.25  38.00 -30.00   56
 20  ω    -41.00 -13.00   0.50    0.81    --  -86.25  38.00  30.00   56
 21  ω   -162.00 -73.00   0.50    0.81    --  -86.25 -19.00 120.00  178
 22  ω     95.00 178.00   0.50    0.81    --  107.74 125.00 -60.00  166
 23  ω     35.00  68.00   0.50    0.81    --  107.74 -57.00-120.00   66
 24  ω     35.00  68.00   0.50    0.81    --  107.74 -57.00-150.00   66
 25  ω     35.00 111.00   0.50    0.81    --  107.74-125.00  60.00  152
 26  ω     95.00 178.00   0.50    0.81    --  107.74  38.00 -90.00  166
 27  ω     35.00  68.00   0.50    0.81    --  107.74 -57.00 -90.00   66
 28  ω     35.00 111.00   0.50    0.81    --  107.74-125.00   0.00  152
 29  ω     35.00 106.00   0.50    0.81    --  107.74 -99.00 120.00  142
 30  ω     35.00 106.00   0.50    0.81    --  107.74 -99.00 150.00  142
 31  ω     95.00 178.00   0.50    0.81    --  107.74  38.00-150.00  166
 32  ω     35.00 111.00   0.50    0.81    --  107.74-125.00  30.00  152
 33  ω     35.00 106.00   0.50    0.81    --  107.74 -99.00 -90.00  142
 34  ω     35.00  68.00   0.50    0.81    --  107.74 -57.00 -30.00   66
 35  ω     35.00 111.00   0.50    0.81    --  107.74-125.00 -60.00  152
 36  ω     93.00 178.00   0.50    0.81    --  107.74  57.00  30.00  170
 37  ω     35.00 106.00   0.50    0.81    --  107.74 -99.00-150.00  142
 38  ω     95.00 149.50   0.50    0.81    --  107.74  38.00 150.00  109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0426137000
_diffrn_orient_matrix_UB_12      0.0798902000
_diffrn_orient_matrix_UB_13      0.0585774000
_diffrn_orient_matrix_UB_21      -0.0484318000
_diffrn_orient_matrix_UB_22      0.0863045000
_diffrn_orient_matrix_UB_23      -0.0819227000
_diffrn_orient_matrix_UB_31      -0.1046523000
_diffrn_orient_matrix_UB_32      -0.0385678000
_diffrn_orient_matrix_UB_33      0.0196571000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9322
_reflns_number_total             10180
_reflns_odcompleteness_completeness 99.47
_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 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0.00088(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         10180
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0342
_refine_ls_restrained_S_all      0.949
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0482P)²+1.6300P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0913
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C15(H15), C19(H19), C34(H34), C38(H38)
2.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C20(H20A,H20B), C21(H21A,
 H21B), C22(H22A,H22B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B),
 C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C44(H44A,H44B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C25(H25), C26(H26), C27(H27), C28(H28)
2.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.76365(8) 0.44964(8) 0.77669(7) 0.0167(2) Uani 1 1 d . . . . .
O2 O 0.71260(8) 0.62234(8) 0.70129(6) 0.0158(2) Uani 1 1 d . . . . .
O3 O 0.75860(9) 0.63999(9) 0.83178(7) 0.0238(2) Uani 1 1 d . . . . .
N1 N 0.59758(9) 0.51372(9) 0.72029(8) 0.0144(2) Uani 1 1 d . . . . .
N2 N 0.43973(9) 0.63159(9) 0.75257(8) 0.0169(2) Uani 1 1 d . . . . .
N7 N 0.52272(9) 0.66583(9) 0.60953(8) 0.0165(2) Uani 1 1 d . . . . .
N4 N 0.83370(9) 0.72011(9) 0.70031(8) 0.0144(2) Uani 1 1 d . . . . .
N5 N 0.82494(10) 0.83708(9) 0.55868(8) 0.0167(2) Uani 1 1 d . . . . .
N6 N 0.88184(10) 0.65213(9) 0.57298(8) 0.0164(2) Uani 1 1 d . . . . .
C1 C 0.69404(11) 0.52181(11) 0.73665(9) 0.0150(3) Uani 1 1 d . . . . .
C2 C 0.77111(11) 0.65806(11) 0.75180(10) 0.0165(3) Uani 1 1 d . . . . .
C3 C 0.57324(11) 0.40823(11) 0.73920(9) 0.0152(3) Uani 1 1 d . . . . .
C4 C 0.63995(11) 0.31997(11) 0.79324(9) 0.0171(3) Uani 1 1 d . . . . .
C5 C 0.60872(13) 0.22319(12) 0.80486(11) 0.0231(3) Uani 1 1 d . . . . .
H5 H 0.649428 0.159966 0.841929 0.028 Uiso 1 1 calc R U . . .
C6 C 0.52182(13) 0.21488(12) 0.76523(11) 0.0243(3) Uani 1 1 d . . . . .
H6 H 0.504325 0.147226 0.775519 0.029 Uiso 1 1 calc R U . . .
C7 C 0.46036(12) 0.30500(12) 0.71063(10) 0.0199(3) Uani 1 1 d . . . . .
H7 H 0.401251 0.299426 0.682679 0.024 Uiso 1 1 calc R U . . .
C8 C 0.48593(11) 0.40328(11) 0.69719(10) 0.0176(3) Uani 1 1 d . . . . .
H8 H 0.444752 0.466121 0.660054 0.021 Uiso 1 1 calc R U . . .
C9 C 0.51601(11) 0.60860(11) 0.69217(10) 0.0152(3) Uani 1 1 d . . . . .
C10 C 0.44963(13) 0.57870(13) 0.84801(10) 0.0231(3) Uani 1 1 d . . . . .
H10A H 0.417146 0.516738 0.862845 0.035 Uiso 1 1 calc R U . . .
H10B H 0.413081 0.629667 0.883135 0.035 Uiso 1 1 calc R U . . .
H10C H 0.525262 0.554476 0.861636 0.035 Uiso 1 1 calc R U . . .
C11 C 0.33332(12) 0.69999(12) 0.72797(11) 0.0225(3) Uani 1 1 d . . . . .
H11A H 0.330933 0.774006 0.729007 0.034 Uiso 1 1 calc R U . . .
H11B H 0.279024 0.673229 0.770575 0.034 Uiso 1 1 calc R U . . .
H11C H 0.319263 0.698189 0.667993 0.034 Uiso 1 1 calc R U . . .
C13 C 0.57793(12) 0.61846(12) 0.53716(10) 0.0218(3) Uani 1 1 d . . . . .
H13A H 0.608960 0.541857 0.561195 0.033 Uiso 1 1 calc R U . . .
H13B H 0.634775 0.654827 0.509621 0.033 Uiso 1 1 calc R U . . .
H13C H 0.526931 0.627055 0.492339 0.033 Uiso 1 1 calc R U . . .
C14 C 0.47771(13) 0.78255(12) 0.58294(11) 0.0244(3) Uani 1 1 d . . . . .
H14A H 0.408136 0.796562 0.557523 0.037 Uiso 1 1 calc R U . . .
H14B H 0.526086 0.816583 0.538374 0.037 Uiso 1 1 calc R U . . .
H14C H 0.468944 0.812162 0.635242 0.037 Uiso 1 1 calc R U . . .
C15 C 0.85774(12) 0.24580(12) 0.81930(10) 0.0214(3) Uani 1 1 d . . . . .
H15 H 0.864660 0.242561 0.755525 0.026 Uiso 1 1 calc R U . . .
C16 C 0.86097(13) 0.13174(12) 0.87913(12) 0.0260(3) Uani 1 1 d . . . . .
H16A H 0.814169 0.099121 0.854299 0.031 Uiso 1 1 calc R U . . .
H16B H 0.934653 0.087655 0.875981 0.031 Uiso 1 1 calc R U . . .
C17 C 0.82657(14) 0.12529(13) 0.97794(12) 0.0283(4) Uani 1 1 d . . . . .
H17A H 0.807152 0.055660 1.004386 0.034 Uiso 1 1 calc R U . . .
H17B H 0.888495 0.126103 1.009414 0.034 Uiso 1 1 calc R U . . .
C18 C 0.73248(13) 0.21574(13) 0.99479(11) 0.0259(3) Uani 1 1 d . . . . .
H18A H 0.728915 0.215484 1.058591 0.031 Uiso 1 1 calc R U . . .
H18B H 0.665632 0.200059 0.982557 0.031 Uiso 1 1 calc R U . . .
C19 C 0.73778(12) 0.32976(12) 0.93834(10) 0.0200(3) Uani 1 1 d . . . . .
H19 H 0.669819 0.381333 0.949475 0.024 Uiso 1 1 calc R U . . .
C20 C 0.83204(14) 0.36820(13) 0.96064(11) 0.0272(3) Uani 1 1 d . . . . .
H20A H 0.821491 0.446080 0.932630 0.033 Uiso 1 1 calc R U . . .
H20B H 0.830349 0.358565 1.025923 0.033 Uiso 1 1 calc R U . . .
C21 C 0.94317(14) 0.31071(14) 0.93055(13) 0.0313(4) Uani 1 1 d . . . . .
H21A H 0.994415 0.354525 0.931165 0.038 Uiso 1 1 calc R U . . .
H21B H 0.965768 0.241008 0.974397 0.038 Uiso 1 1 calc R U . . .
C22 C 0.94964(12) 0.29002(13) 0.83810(12) 0.0271(3) Uani 1 1 d . . . . .
H22A H 1.017928 0.238348 0.830762 0.033 Uiso 1 1 calc R U . . .
H22B H 0.950773 0.358168 0.792931 0.033 Uiso 1 1 calc R U . . .
C23 C 0.89762(11) 0.76964(11) 0.74108(9) 0.0153(3) Uani 1 1 d . . . . .
C24 C 0.86409(11) 0.79429(11) 0.82282(9) 0.0159(3) Uani 1 1 d . . . . .
C25 C 0.92931(12) 0.84686(12) 0.85271(10) 0.0204(3) Uani 1 1 d . . . . .
H25 H 0.910490 0.865714 0.907984 0.024 Uiso 1 1 calc R U . . .
C26 C 1.02017(13) 0.87241(13) 0.80477(11) 0.0231(3) Uani 1 1 d . . . . .
H26 H 1.060452 0.910370 0.826352 0.028 Uiso 1 1 calc R U . . .
C27 C 1.05197(12) 0.84251(12) 0.72554(10) 0.0206(3) Uani 1 1 d . . . . .
H27 H 1.114825 0.858451 0.693235 0.025 Uiso 1 1 calc R U . . .
C28 C 0.99132(11) 0.78917(11) 0.69384(10) 0.0172(3) Uani 1 1 d . . . . .
H28 H 1.013275 0.766175 0.640596 0.021 Uiso 1 1 calc R U . . .
C29 C 0.84608(11) 0.73620(11) 0.60644(9) 0.0149(3) Uani 1 1 d . . . . .
C30 C 0.89329(13) 0.87301(12) 0.48063(10) 0.0226(3) Uani 1 1 d . . . . .
H30A H 0.954847 0.814012 0.475496 0.034 Uiso 1 1 calc R U . . .
H30B H 0.918162 0.934097 0.487554 0.034 Uiso 1 1 calc R U . . .
H30C H 0.852431 0.894890 0.426793 0.034 Uiso 1 1 calc R U . . .
C31 C 0.74982(12) 0.92245(11) 0.59253(10) 0.0207(3) Uani 1 1 d . . . . .
H31A H 0.695087 0.892273 0.632114 0.031 Uiso 1 1 calc R U . . .
H31B H 0.715820 0.978618 0.542433 0.031 Uiso 1 1 calc R U . . .
H31C H 0.788461 0.953402 0.625613 0.031 Uiso 1 1 calc R U . . .
C32 C 0.93785(12) 0.54633(11) 0.62463(10) 0.0194(3) Uani 1 1 d . . . . .
H32A H 0.948972 0.551063 0.684450 0.029 Uiso 1 1 calc R U . . .
H32B H 1.007050 0.523428 0.594698 0.029 Uiso 1 1 calc R U . . .
H32C H 0.894862 0.493953 0.629187 0.029 Uiso 1 1 calc R U . . .
C33 C 0.86796(12) 0.65708(13) 0.47967(10) 0.0214(3) Uani 1 1 d . . . . .
H33A H 0.813562 0.721625 0.454783 0.032 Uiso 1 1 calc R U . . .
H33B H 0.845288 0.593196 0.476483 0.032 Uiso 1 1 calc R U . . .
H33C H 0.935751 0.659719 0.445458 0.032 Uiso 1 1 calc R U . . .
C34 C 0.76227(12) 0.71355(12) 0.98372(10) 0.0204(3) Uani 1 1 d . . . . .
H34 H 0.833985 0.664592 0.998039 0.024 Uiso 1 1 calc R U . . .
C35 C 0.67564(13) 0.64871(12) 1.01330(10) 0.0224(3) Uani 1 1 d . . . . .
H35A H 0.696026 0.584764 0.988469 0.027 Uiso 1 1 calc R U . . .
H35B H 0.674173 0.622891 1.079031 0.027 Uiso 1 1 calc R U . . .
C36 C 0.56321(13) 0.71057(13) 0.98518(10) 0.0228(3) Uani 1 1 d . . . . .
H36A H 0.532956 0.757864 1.025722 0.027 Uiso 1 1 calc R U . . .
H36B H 0.518133 0.658408 0.993044 0.027 Uiso 1 1 calc R U . . .
C37 C 0.55617(12) 0.77972(14) 0.88862(10) 0.0244(3) Uani 1 1 d . . . . .
H37A H 0.556177 0.732672 0.848901 0.029 Uiso 1 1 calc R U . . .
H37B H 0.486921 0.833207 0.883354 0.029 Uiso 1 1 calc R U . . .
C38 C 0.64562(12) 0.83992(12) 0.85474(10) 0.0189(3) Uani 1 1 d . . . . .
H38 H 0.643605 0.867744 0.788566 0.023 Uiso 1 1 calc R U . . .
C39 C 0.63808(14) 0.93449(12) 0.89789(12) 0.0270(3) Uani 1 1 d . . . . .
H39A H 0.694312 0.972664 0.869567 0.032 Uiso 1 1 calc R U . . .
H39B H 0.568244 0.985729 0.884768 0.032 Uiso 1 1 calc R U . . .
C40 C 0.64985(15) 0.90161(14) 0.99917(12) 0.0312(4) Uani 1 1 d . . . . .
H40A H 0.658974 0.964046 1.018330 0.037 Uiso 1 1 calc R U . . .
H40B H 0.583022 0.883297 1.028643 0.037 Uiso 1 1 calc R U . . .
C41 C 0.74363(14) 0.80605(15) 1.03123(11) 0.0286(4) Uani 1 1 d . . . . .
H41A H 0.731662 0.776215 1.095843 0.034 Uiso 1 1 calc R U . . .
H41B H 0.809545 0.832926 1.023159 0.034 Uiso 1 1 calc R U . . .
B1 B 0.74551(13) 0.32531(12) 0.83623(11) 0.0168(3) Uani 1 1 d . . . . .
B2 B 0.75975(13) 0.76680(13) 0.87993(11) 0.0168(3) Uani 1 1 d . . . . .
S2 S 0.36205(3) 1.03796(3) 0.65080(2) 0.02115(9) Uani 1 1 d . . . . .
F4 F 0.28205(11) 0.95427(10) 0.80701(8) 0.0510(3) Uani 1 1 d . . . . .
F5 F 0.32010(10) 1.10553(12) 0.79666(8) 0.0509(3) Uani 1 1 d . . . . .
F6 F 0.18148(9) 1.10093(10) 0.73605(8) 0.0407(3) Uani 1 1 d . . . . .
O7 O 0.46821(10) 0.98780(10) 0.68038(9) 0.0335(3) Uani 1 1 d . . . . .
O8 O 0.34575(10) 1.14749(10) 0.59822(8) 0.0331(3) Uani 1 1 d . . . . .
O9 O 0.31094(10) 0.97150(9) 0.61809(8) 0.0313(3) Uani 1 1 d . . . . .
C43 C 0.28268(14) 1.05045(14) 0.75295(11) 0.0267(3) Uani 1 1 d . . . . .
S1 S 0.77927(3) 0.35658(3) 0.50981(2) 0.01739(9) Uani 1 1 d . . . . .
F1 F 0.79543(9) 0.16427(8) 0.48979(7) 0.0339(2) Uani 1 1 d . . . . .
F2 F 0.68621(9) 0.20218(9) 0.59703(8) 0.0388(3) Uani 1 1 d . . . . .
F3 F 0.85568(9) 0.16506(8) 0.61282(7) 0.0344(2) Uani 1 1 d . . . . .
O4 O 0.88206(9) 0.35024(9) 0.46257(8) 0.0267(2) Uani 1 1 d . . . . .
O5 O 0.76854(9) 0.40057(9) 0.58641(7) 0.0242(2) Uani 1 1 d . . . . .
O6 O 0.68931(9) 0.39568(9) 0.45329(8) 0.0268(2) Uani 1 1 d . . . . .
C42 C 0.77861(13) 0.21492(12) 0.55582(11) 0.0231(3) Uani 1 1 d . . . . .
Cl1 Cl 1.17419(3) 0.37504(3) 0.72317(3) 0.03085(10) Uani 1 1 d . . . . .
Cl2 Cl 1.10770(4) 0.53368(3) 0.82948(3) 0.03622(11) Uani 1 1 d . . . . .
C44 C 1.19528(15) 0.49238(15) 0.74392(12) 0.0320(4) Uani 1 1 d . . . . .
H44A H 1.184935 0.550878 0.688660 0.038 Uiso 1 1 calc R U . . .
H44B H 1.269845 0.478818 0.760856 0.038 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.2212(18) . ?
O1 B1 1.7248(18) . ?
O2 C1 1.3730(16) . ?
O2 C2 1.3908(17) . ?
O3 C2 1.2061(18) . ?
O3 B2 2.0220(19) . ?
N1 C1 1.3395(18) . ?
N1 C3 1.4601(16) . ?
N1 C9 1.4258(18) . ?
N2 C9 1.3239(19) . ?
N2 C10 1.4713(19) . ?
N2 C11 1.4743(19) . ?
N7 C9 1.3162(19) . ?
N7 C13 1.4675(19) . ?
N7 C14 1.4726(18) . ?
N4 C2 1.3505(18) . ?
N4 C23 1.4626(17) . ?
N4 C29 1.4186(18) . ?
N5 C29 1.3238(18) . ?
N5 C30 1.4697(18) . ?
N5 C31 1.4694(18) . ?
N6 C29 1.3149(18) . ?
N6 C32 1.4700(18) . ?
N6 C33 1.4678(18) . ?
C3 C4 1.398(2) . ?
C3 C8 1.393(2) . ?
C4 C5 1.404(2) . ?
C4 B1 1.614(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.385(2) . ?
C6 H6 0.9500 . ?
C6 C7 1.385(2) . ?
C7 H7 0.9500 . ?
C7 C8 1.384(2) . ?
C8 H8 0.9500 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15 1.0000 . ?
C15 C16 1.546(2) . ?
C15 C22 1.541(2) . ?
C15 B1 1.609(2) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.542(2) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.535(2) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.550(2) . ?
C19 H19 1.0000 . ?
C19 C20 1.542(2) . ?
C19 B1 1.600(2) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.538(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.528(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.396(2) . ?
C23 C28 1.395(2) . ?
C24 C25 1.407(2) . ?
C24 B2 1.602(2) . ?
C25 H25 0.9500 . ?
C25 C26 1.391(2) . ?
C26 H26 0.9500 . ?
C26 C27 1.386(2) . ?
C27 H27 0.9500 . ?
C27 C28 1.385(2) . ?
C28 H28 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34 1.0000 . ?
C34 C35 1.542(2) . ?
C34 C41 1.553(2) . ?
C34 B2 1.584(2) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.528(2) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C37 1.539(2) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.540(2) . ?
C38 H38 1.0000 . ?
C38 C39 1.553(2) . ?
C38 B2 1.577(2) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.536(2) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40 C41 1.535(3) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
S2 O7 1.4368(13) . ?
S2 O8 1.4423(12) . ?
S2 O9 1.4452(13) . ?
S2 C43 1.8209(17) . ?
F4 C43 1.331(2) . ?
F5 C43 1.324(2) . ?
F6 C43 1.333(2) . ?
S1 O4 1.4440(11) . ?
S1 O5 1.4426(11) . ?
S1 O6 1.4437(12) . ?
S1 C42 1.8279(16) . ?
F1 C42 1.3436(18) . ?
F2 C42 1.3233(19) . ?
F3 C42 1.3325(19) . ?
Cl1 C44 1.7640(19) . ?
Cl2 C44 1.7636(19) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O1 B1 124.56(11) . . ?
C1 O2 C2 116.48(11) . . ?
C2 O3 B2 113.18(10) . . ?
C1 N1 C3 119.95(11) . . ?
C1 N1 C9 119.73(11) . . ?
C9 N1 C3 120.07(11) . . ?
C9 N2 C10 122.31(12) . . ?
C9 N2 C11 122.26(12) . . ?
C10 N2 C11 114.87(12) . . ?
C9 N7 C13 122.45(12) . . ?
C9 N7 C14 122.69(12) . . ?
C13 N7 C14 114.85(12) . . ?
C2 N4 C23 120.22(12) . . ?
C2 N4 C29 123.10(12) . . ?
C29 N4 C23 116.59(11) . . ?
C29 N5 C30 121.09(12) . . ?
C29 N5 C31 121.34(12) . . ?
C30 N5 C31 115.96(12) . . ?
C29 N6 C32 123.63(12) . . ?
C29 N6 C33 121.91(12) . . ?
C33 N6 C32 114.46(11) . . ?
O1 C1 O2 119.91(12) . . ?
O1 C1 N1 126.42(13) . . ?
N1 C1 O2 113.65(12) . . ?
O3 C2 O2 121.56(12) . . ?
O3 C2 N4 126.21(13) . . ?
N4 C2 O2 112.02(12) . . ?
C4 C3 N1 119.23(12) . . ?
C8 C3 N1 115.88(12) . . ?
C8 C3 C4 124.81(13) . . ?
C3 C4 C5 113.48(13) . . ?
C3 C4 B1 124.38(12) . . ?
C5 C4 B1 122.11(13) . . ?
C4 C5 H5 118.2 . . ?
C6 C5 C4 123.57(14) . . ?
C6 C5 H5 118.2 . . ?
C5 C6 H6 119.9 . . ?
C5 C6 C7 120.11(14) . . ?
C7 C6 H6 119.9 . . ?
C6 C7 H7 120.3 . . ?
C8 C7 C6 119.31(14) . . ?
C8 C7 H7 120.3 . . ?
C3 C8 H8 120.7 . . ?
C7 C8 C3 118.68(13) . . ?
C7 C8 H8 120.7 . . ?
N2 C9 N1 116.39(12) . . ?
N7 C9 N1 117.98(12) . . ?
N7 C9 N2 125.62(13) . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
N2 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N7 C13 H13A 109.5 . . ?
N7 C13 H13B 109.5 . . ?
N7 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N7 C14 H14A 109.5 . . ?
N7 C14 H14B 109.5 . . ?
N7 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 H15 108.8 . . ?
C16 C15 B1 109.70(12) . . ?
C22 C15 H15 108.8 . . ?
C22 C15 C16 111.28(13) . . ?
C22 C15 B1 109.40(13) . . ?
B1 C15 H15 108.8 . . ?
C15 C16 H16A 108.3 . . ?
C15 C16 H16B 108.3 . . ?
H16A C16 H16B 107.4 . . ?
C17 C16 C15 115.78(13) . . ?
C17 C16 H16A 108.3 . . ?
C17 C16 H16B 108.3 . . ?
C16 C17 H17A 108.5 . . ?
C16 C17 H17B 108.5 . . ?
H17A C17 H17B 107.5 . . ?
C18 C17 C16 115.07(13) . . ?
C18 C17 H17A 108.5 . . ?
C18 C17 H17B 108.5 . . ?
C17 C18 H18A 108.5 . . ?
C17 C18 H18B 108.5 . . ?
C17 C18 C19 114.93(13) . . ?
H18A C18 H18B 107.5 . . ?
C19 C18 H18A 108.5 . . ?
C19 C18 H18B 108.5 . . ?
C18 C19 H19 108.6 . . ?
C18 C19 B1 106.54(12) . . ?
C20 C19 C18 112.94(13) . . ?
C20 C19 H19 108.6 . . ?
C20 C19 B1 111.39(12) . . ?
B1 C19 H19 108.6 . . ?
C19 C20 H20A 108.4 . . ?
C19 C20 H20B 108.4 . . ?
H20A C20 H20B 107.5 . . ?
C21 C20 C19 115.35(14) . . ?
C21 C20 H20A 108.4 . . ?
C21 C20 H20B 108.4 . . ?
C20 C21 H21A 108.6 . . ?
C20 C21 H21B 108.6 . . ?
H21A C21 H21B 107.6 . . ?
C22 C21 C20 114.77(13) . . ?
C22 C21 H21A 108.6 . . ?
C22 C21 H21B 108.6 . . ?
C15 C22 H22A 108.6 . . ?
C15 C22 H22B 108.6 . . ?
C21 C22 C15 114.84(13) . . ?
C21 C22 H22A 108.6 . . ?
C21 C22 H22B 108.6 . . ?
H22A C22 H22B 107.5 . . ?
C24 C23 N4 120.19(12) . . ?
C28 C23 N4 116.13(12) . . ?
C28 C23 C24 123.68(13) . . ?
C23 C24 C25 114.77(13) . . ?
C23 C24 B2 124.05(13) . . ?
C25 C24 B2 121.18(13) . . ?
C24 C25 H25 118.6 . . ?
C26 C25 C24 122.78(14) . . ?
C26 C25 H25 118.6 . . ?
C25 C26 H26 120.0 . . ?
C27 C26 C25 120.01(14) . . ?
C27 C26 H26 120.0 . . ?
C26 C27 H27 120.3 . . ?
C28 C27 C26 119.44(14) . . ?
C28 C27 H27 120.3 . . ?
C23 C28 H28 120.4 . . ?
C27 C28 C23 119.17(13) . . ?
C27 C28 H28 120.4 . . ?
N5 C29 N4 116.52(12) . . ?
N6 C29 N4 118.87(12) . . ?
N6 C29 N5 124.54(13) . . ?
N5 C30 H30A 109.5 . . ?
N5 C30 H30B 109.5 . . ?
N5 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N5 C31 H31A 109.5 . . ?
N5 C31 H31B 109.5 . . ?
N5 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N6 C32 H32A 109.5 . . ?
N6 C32 H32B 109.5 . . ?
N6 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N6 C33 H33A 109.5 . . ?
N6 C33 H33B 109.5 . . ?
N6 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 H34 109.3 . . ?
C35 C34 C41 111.15(12) . . ?
C35 C34 B2 110.48(12) . . ?
C41 C34 H34 109.3 . . ?
C41 C34 B2 107.14(12) . . ?
B2 C34 H34 109.3 . . ?
C34 C35 H35A 108.5 . . ?
C34 C35 H35B 108.5 . . ?
H35A C35 H35B 107.5 . . ?
C36 C35 C34 114.93(12) . . ?
C36 C35 H35A 108.5 . . ?
C36 C35 H35B 108.5 . . ?
C35 C36 H36A 108.5 . . ?
C35 C36 H36B 108.5 . . ?
C35 C36 C37 115.17(12) . . ?
H36A C36 H36B 107.5 . . ?
C37 C36 H36A 108.5 . . ?
C37 C36 H36B 108.5 . . ?
C36 C37 H37A 108.3 . . ?
C36 C37 H37B 108.3 . . ?
H37A C37 H37B 107.4 . . ?
C38 C37 C36 115.93(13) . . ?
C38 C37 H37A 108.3 . . ?
C38 C37 H37B 108.3 . . ?
C37 C38 H38 109.4 . . ?
C37 C38 C39 113.20(13) . . ?
C37 C38 B2 112.55(12) . . ?
C39 C38 H38 109.4 . . ?
C39 C38 B2 102.80(12) . . ?
B2 C38 H38 109.4 . . ?
C38 C39 H39A 108.6 . . ?
C38 C39 H39B 108.6 . . ?
H39A C39 H39B 107.5 . . ?
C40 C39 C38 114.85(13) . . ?
C40 C39 H39A 108.6 . . ?
C40 C39 H39B 108.6 . . ?
C39 C40 H40A 108.7 . . ?
C39 C40 H40B 108.7 . . ?
H40A C40 H40B 107.6 . . ?
C41 C40 C39 114.42(13) . . ?
C41 C40 H40A 108.7 . . ?
C41 C40 H40B 108.7 . . ?
C34 C41 H41A 108.4 . . ?
C34 C41 H41B 108.4 . . ?
C40 C41 C34 115.55(13) . . ?
C40 C41 H41A 108.4 . . ?
C40 C41 H41B 108.4 . . ?
H41A C41 H41B 107.5 . . ?
C4 B1 O1 101.32(10) . . ?
C15 B1 O1 102.97(11) . . ?
C15 B1 C4 119.41(13) . . ?
C19 B1 O1 104.80(11) . . ?
C19 B1 C4 118.37(12) . . ?
C19 B1 C15 107.47(12) . . ?
C24 B2 O3 95.81(10) . . ?
C34 B2 O3 101.27(10) . . ?
C34 B2 C24 121.60(13) . . ?
C38 B2 O3 100.60(10) . . ?
C38 B2 C24 120.54(12) . . ?
C38 B2 C34 110.43(12) . . ?
O7 S2 O8 115.98(8) . . ?
O7 S2 O9 115.21(7) . . ?
O7 S2 C43 104.01(8) . . ?
O8 S2 O9 114.22(8) . . ?
O8 S2 C43 103.15(8) . . ?
O9 S2 C43 101.63(8) . . ?
F4 C43 S2 111.02(12) . . ?
F4 C43 F6 107.28(14) . . ?
F5 C43 S2 111.56(12) . . ?
F5 C43 F4 108.01(14) . . ?
F5 C43 F6 107.44(15) . . ?
F6 C43 S2 111.34(11) . . ?
O4 S1 O6 114.56(7) . . ?
O4 S1 C42 102.16(7) . . ?
O5 S1 O4 114.64(7) . . ?
O5 S1 O6 115.30(7) . . ?
O5 S1 C42 104.83(7) . . ?
O6 S1 C42 103.06(7) . . ?
F1 C42 S1 109.71(10) . . ?
F2 C42 S1 112.10(11) . . ?
F2 C42 F1 107.39(13) . . ?
F2 C42 F3 108.39(13) . . ?
F3 C42 S1 111.87(11) . . ?
F3 C42 F1 107.17(13) . . ?
Cl1 C44 Cl2 112.04(9) . . ?
Cl1 C44 H44A 109.2 . . ?
Cl1 C44 H44B 109.2 . . ?
Cl2 C44 H44A 109.2 . . ?
Cl2 C44 H44B 109.2 . . ?
H44A C44 H44B 107.9 . . ?

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
N1 C3 C4 C5 -178.96(13) . . . . ?
N1 C3 C4 B1 -1.0(2) . . . . ?
N1 C3 C8 C7 178.40(13) . . . . ?
N4 C23 C24 C25 -176.73(12) . . . . ?
N4 C23 C24 B2 3.0(2) . . . . ?
N4 C23 C28 C27 175.65(13) . . . . ?
C1 O1 B1 C4 20.39(17) . . . . ?
C1 O1 B1 C15 144.44(13) . . . . ?
C1 O1 B1 C19 -103.26(14) . . . . ?
C1 O2 C2 O3 -39.05(19) . . . . ?
C1 O2 C2 N4 145.95(12) . . . . ?
C1 N1 C3 C4 15.28(19) . . . . ?
C1 N1 C3 C8 -161.73(13) . . . . ?
C1 N1 C9 N2 -104.83(15) . . . . ?
C1 N1 C9 N7 74.84(17) . . . . ?
C2 O2 C1 O1 -38.41(18) . . . . ?
C2 O2 C1 N1 143.22(12) . . . . ?
C2 N4 C23 C24 -27.90(19) . . . . ?
C2 N4 C23 C28 151.87(13) . . . . ?
C2 N4 C29 N5 125.01(14) . . . . ?
C2 N4 C29 N6 -58.05(19) . . . . ?
C3 N1 C1 O1 -9.4(2) . . . . ?
C3 N1 C1 O2 168.87(11) . . . . ?
C3 N1 C9 N2 69.46(16) . . . . ?
C3 N1 C9 N7 -110.87(14) . . . . ?
C3 C4 C5 C6 1.4(2) . . . . ?
C3 C4 B1 O1 -13.65(17) . . . . ?
C3 C4 B1 C15 -125.70(15) . . . . ?
C3 C4 B1 C19 100.19(16) . . . . ?
C4 C3 C8 C7 1.6(2) . . . . ?
C4 C5 C6 C7 0.1(3) . . . . ?
C5 C4 B1 O1 164.11(13) . . . . ?
C5 C4 B1 C15 52.1(2) . . . . ?
C5 C4 B1 C19 -82.06(18) . . . . ?
C5 C6 C7 C8 -0.9(2) . . . . ?
C6 C7 C8 C3 0.1(2) . . . . ?
C8 C3 C4 C5 -2.2(2) . . . . ?
C8 C3 C4 B1 175.70(14) . . . . ?
C9 N1 C1 O1 164.92(13) . . . . ?
C9 N1 C1 O2 -16.83(18) . . . . ?
C9 N1 C3 C4 -158.99(13) . . . . ?
C9 N1 C3 C8 23.99(18) . . . . ?
C10 N2 C9 N1 13.82(19) . . . . ?
C10 N2 C9 N7 -165.82(13) . . . . ?
C11 N2 C9 N1 -157.19(12) . . . . ?
C11 N2 C9 N7 23.2(2) . . . . ?
C13 N7 C9 N1 26.66(19) . . . . ?
C13 N7 C9 N2 -153.70(14) . . . . ?
C14 N7 C9 N1 -151.86(13) . . . . ?
C14 N7 C9 N2 27.8(2) . . . . ?
C15 C16 C17 C18 38.5(2) . . . . ?
C16 C15 C22 C21 -66.23(17) . . . . ?
C16 C15 B1 O1 172.11(11) . . . . ?
C16 C15 B1 C4 -76.73(16) . . . . ?
C16 C15 B1 C19 61.79(15) . . . . ?
C16 C17 C18 C19 -43.7(2) . . . . ?
C17 C18 C19 C20 -65.30(18) . . . . ?
C17 C18 C19 B1 57.30(17) . . . . ?
C18 C19 C20 C21 70.63(18) . . . . ?
C18 C19 B1 O1 -174.61(11) . . . . ?
C18 C19 B1 C4 73.47(16) . . . . ?
C18 C19 B1 C15 -65.56(14) . . . . ?
C19 C20 C21 C22 41.5(2) . . . . ?
C20 C19 B1 O1 -51.04(15) . . . . ?
C20 C19 B1 C4 -162.96(13) . . . . ?
C20 C19 B1 C15 58.02(15) . . . . ?
C20 C21 C22 C15 -44.85(19) . . . . ?
C22 C15 C16 C17 73.21(17) . . . . ?
C22 C15 B1 O1 49.79(14) . . . . ?
C22 C15 B1 C4 160.94(13) . . . . ?
C22 C15 B1 C19 -60.53(15) . . . . ?
C23 N4 C2 O2 177.08(11) . . . . ?
C23 N4 C2 O3 2.4(2) . . . . ?
C23 N4 C29 N5 -58.42(16) . . . . ?
C23 N4 C29 N6 118.52(14) . . . . ?
C23 C24 C25 C26 0.0(2) . . . . ?
C23 C24 B2 O3 26.56(16) . . . . ?
C23 C24 B2 C34 133.60(15) . . . . ?
C23 C24 B2 C38 -79.39(18) . . . . ?
C24 C23 C28 C27 -4.6(2) . . . . ?
C24 C25 C26 C27 -2.4(2) . . . . ?
C25 C24 B2 O3 -153.76(12) . . . . ?
C25 C24 B2 C34 -46.7(2) . . . . ?
C25 C24 B2 C38 100.30(17) . . . . ?
C25 C26 C27 C28 1.3(2) . . . . ?
C26 C27 C28 C23 2.0(2) . . . . ?
C28 C23 C24 C25 3.5(2) . . . . ?
C28 C23 C24 B2 -176.78(13) . . . . ?
C29 N4 C2 O2 -6.47(18) . . . . ?
C29 N4 C2 O3 178.80(14) . . . . ?
C29 N4 C23 C24 155.43(13) . . . . ?
C29 N4 C23 C28 -24.81(17) . . . . ?
C30 N5 C29 N4 138.24(13) . . . . ?
C30 N5 C29 N6 -38.5(2) . . . . ?
C31 N5 C29 N4 -26.77(19) . . . . ?
C31 N5 C29 N6 156.48(14) . . . . ?
C32 N6 C29 N4 -17.8(2) . . . . ?
C32 N6 C29 N5 158.87(13) . . . . ?
C33 N6 C29 N4 161.86(12) . . . . ?
C33 N6 C29 N5 -21.5(2) . . . . ?
C34 C35 C36 C37 43.71(19) . . . . ?
C35 C34 C41 C40 -72.89(17) . . . . ?
C35 C34 B2 O3 -49.19(14) . . . . ?
C35 C34 B2 C24 -153.29(13) . . . . ?
C35 C34 B2 C38 56.74(16) . . . . ?
C35 C36 C37 C38 -39.7(2) . . . . ?
C36 C37 C38 C39 -70.99(18) . . . . ?
C36 C37 C38 B2 45.05(19) . . . . ?
C37 C38 C39 C40 62.75(18) . . . . ?
C37 C38 B2 O3 52.99(14) . . . . ?
C37 C38 B2 C24 156.28(13) . . . . ?
C37 C38 B2 C34 -53.38(16) . . . . ?
C38 C39 C40 C41 46.8(2) . . . . ?
C39 C38 B2 O3 175.11(10) . . . . ?
C39 C38 B2 C24 -81.60(15) . . . . ?
C39 C38 B2 C34 68.74(14) . . . . ?
C39 C40 C41 C34 -40.2(2) . . . . ?
C41 C34 C35 C36 66.35(17) . . . . ?
C41 C34 B2 O3 -170.40(11) . . . . ?
C41 C34 B2 C24 85.50(16) . . . . ?
C41 C34 B2 C38 -64.48(15) . . . . ?
B1 O1 C1 O2 171.32(11) . . . . ?
B1 O1 C1 N1 -10.5(2) . . . . ?
B1 C4 C5 C6 -176.59(15) . . . . ?
B1 C15 C16 C17 -47.99(18) . . . . ?
B1 C15 C22 C21 55.14(17) . . . . ?
B1 C19 C20 C21 -49.22(18) . . . . ?
B2 O3 C2 O2 -138.88(12) . . . . ?
B2 O3 C2 N4 35.4(2) . . . . ?
B2 C24 C25 C26 -179.72(14) . . . . ?
B2 C34 C35 C36 -52.45(17) . . . . ?
B2 C34 C41 C40 47.90(17) . . . . ?
B2 C38 C39 C40 -58.93(16) . . . . ?
O7 S2 C43 F4 -63.51(14) . . . . ?
O7 S2 C43 F5 57.02(15) . . . . ?
O7 S2 C43 F6 177.04(11) . . . . ?
O8 S2 C43 F4 175.03(12) . . . . ?
O8 S2 C43 F5 -64.44(14) . . . . ?
O8 S2 C43 F6 55.58(13) . . . . ?
O9 S2 C43 F4 56.47(13) . . . . ?
O9 S2 C43 F5 176.99(13) . . . . ?
O9 S2 C43 F6 -62.99(13) . . . . ?
O4 S1 C42 F1 -56.04(12) . . . . ?
O4 S1 C42 F2 -175.25(12) . . . . ?
O4 S1 C42 F3 62.76(12) . . . . ?
O5 S1 C42 F1 -175.92(11) . . . . ?
O5 S1 C42 F2 64.87(13) . . . . ?
O5 S1 C42 F3 -57.12(12) . . . . ?
O6 S1 C42 F1 63.07(12) . . . . ?
O6 S1 C42 F2 -56.14(13) . . . . ?
O6 S1 C42 F3 -178.14(11) . . . . ?

_olex2_exptl_crystal_mounting_method 'MiTeGen 50 micron MicroLoop'
_olex2_submission_original_sample_id kre21_07
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.383
_oxdiff_exptl_absorpt_empirical_full_min 0.612
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_9
_database_code_depnum_ccdc_archive 'CCDC 2127871'
loop_
_audit_author_name
_audit_author_address
'Daniel Unruh'
;Texas Tech University
United States of America
;
_audit_update_record             
;
2021-12-10 deposited with the CCDC.	2022-07-22 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT430_9                   
;
PROBLEM: Short Inter D...A Contact  O1       ..O3       .       2.82 Ang.  
RESPONSE: This is a cation-anion interaction between the two molecules.
;
_vrf_PLAT243_9                   
;
PROBLEM: High   'Solvent' Ueq as Compared to Neighbors of         F3 Check 
RESPONSE: Due to the disordered triflate molecule.
;
_vrf_PLAT250_9                   
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.1 Note  
RESPONSE: Due to the disordered triflate molecule.
;
_vrf_PLAT410_9                   
;
PROBLEM: Short Intra H...H Contact  H15B     ..H19B     .       1.99 Ang.  
RESPONSE: This is a typical H...H contact distance in the boat configuration of
          the 9-Borabicyclo[3.3.1]nonane molecule.
;
_vrf_PLAT911_9                   
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         95 Report
RESPONSE: Due to an issue with the initial data collection strategy for the 
          experiment.
;
# end Validation Reply Form

_audit_creation_date             2020-06-23T14:53:08-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C37 H54 B F6 N3 O8 P S2'
_chemical_formula_weight         888.73

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.7942(2)
_cell_length_b                   13.2589(2)
_cell_length_c                   18.7602(3)
_cell_angle_alpha                90.2410(10)
_cell_angle_beta                 101.395(2)
_cell_angle_gamma                90.355(2)
_cell_volume                     2144.27(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    21518
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      76.97

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       irregular
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.049
_exptl_crystal_size_min          0.025
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_F_000             934
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 -2 -8 0.0289
4 -6 -2 0.0062
-4 6 1 0.0114
2 4 9 0.037
-4 -5 5 0.0255
2 5 -10 0.0289
-2 -4 11 0.0362
4 5 -5 0.0231


#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    2.16
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
        a multifaceted crystal model
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_T_max  1
_shelx_estimated_absorpt_T_min   0.846
_shelx_estimated_absorpt_T_max   0.948

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_ambient_temperature      100(2)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_detector_area_resol_mean 10
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_ub_11      0.0962223
_diffrn_orient_matrix_ub_12      -0.0853113
_diffrn_orient_matrix_ub_13      -0.0247303
_diffrn_orient_matrix_ub_21      -0.07304
_diffrn_orient_matrix_ub_22      -0.0759458
_diffrn_orient_matrix_ub_23      0.0455616
_diffrn_orient_matrix_ub_31      -0.1316899
_diffrn_orient_matrix_ub_32      -0.0213415
_diffrn_orient_matrix_ub_33      -0.065804
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_unetI/netI     0.0782
_diffrn_reflns_number            41829
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.402
_diffrn_reflns_theta_max         77.486
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.961
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.961
_reflns_Friedel_coverage         0
_reflns_number_total             8758
_reflns_number_gt                7388
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_shelx_SHELXL_version_number     2018/3
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0426P)²+0.9779P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         8758
_refine_ls_number_parameters     570
_refine_ls_number_restraints     589
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0377
_refine_ls_wR_factor_ref         0.0985
_refine_ls_wR_factor_gt          0.0942
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.02
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.052

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 The triflate molecule (S1, O3 < O5, F1 < F3, and C27) was positionally 
 disordered over two sites. Atoms S1, O5, C27, and F1 were split into parts A 
 and B with refined occupancies of 0.94 and 0.06, respectively. To help 
 maintain reasonable ADP values and bond lengths of the disordered sites, RIGU,
 SIMU, and free variable DFIX restraints were applied. The inconsistent 
 reflections -9 -4 15 and -6 14 0 were omitted.
;

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.009 0.0039 '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 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
S1A S 0.34579(5) 0.32562(4) 0.37483(2) 0.02289(13) Uani 0.9367(15) 1 d D U P A
1
O5A O 0.34729(15) 0.43336(10) 0.38442(8) 0.0324(3) Uani 0.9367(15) 1 d D U P A
1
C27A C 0.4022(2) 0.27870(16) 0.46805(11) 0.0263(4) Uani 0.9367(15) 1 d D U P A
1
F1A F 0.41441(13) 0.17835(8) 0.46949(6) 0.0304(3) Uani 0.9367(15) 1 d D U P A 1
S1B S 0.3454(7) 0.2575(6) 0.3621(4) 0.0259(16) Uani 0.0633(15) 1 d D U P A 2
O5B O 0.370(2) 0.1566(12) 0.3764(12) 0.034(4) Uani 0.0633(15) 1 d D U P A 2
C27B C 0.390(2) 0.3129(17) 0.4547(10) 0.028(2) Uani 0.0633(15) 1 d D U P A 2
F1B F 0.373(2) 0.4164(13) 0.4506(10) 0.037(3) Uani 0.0633(15) 1 d D U P A 2
S2 S -0.01487(5) 0.75235(3) 0.40112(2) 0.02257(10) Uani 1 1 d . . . . .
P1 P 0.85273(5) 0.12054(3) 0.35423(2) 0.01858(10) Uani 1 1 d . . . . .
F2 F 0.29581(15) 0.30191(10) 0.50664(6) 0.0425(3) Uani 1 1 d D . . . .
F3 F 0.53774(14) 0.31600(10) 0.50064(6) 0.0445(3) Uani 1 1 d D . . . .
F4 F 0.26512(13) 0.81485(9) 0.39192(6) 0.0366(3) Uani 1 1 d . . . . .
F5 F 0.11013(15) 0.79332(9) 0.28847(6) 0.0389(3) Uani 1 1 d . . . . .
F6 F 0.21008(14) 0.66462(9) 0.35059(7) 0.0413(3) Uani 1 1 d . . . . .
O1 O 0.96647(13) 0.21781(8) 0.23013(6) 0.0204(2) Uani 1 1 d . . . . .
O2 O 0.85076(13) 0.23717(8) 0.32605(6) 0.0195(2) Uani 1 1 d . . . . .
O3 O 0.19423(14) 0.28164(9) 0.34997(7) 0.0293(3) Uani 1 1 d D U . . .
O4 O 0.46555(15) 0.28821(11) 0.33893(7) 0.0318(3) Uani 1 1 d D U . . .
O6 O 0.05149(16) 0.71479(10) 0.47247(7) 0.0320(3) Uani 1 1 d . . . . .
O7 O -0.06325(16) 0.85603(9) 0.39937(7) 0.0324(3) Uani 1 1 d . . . . .
O8 O -0.12066(15) 0.68387(9) 0.35587(7) 0.0285(3) Uani 1 1 d . . . . .
N1 N 0.88141(16) 0.37290(10) 0.25941(7) 0.0181(3) Uani 1 1 d . . . . .
N2 N 0.83245(15) 0.44977(10) 0.36593(7) 0.0177(3) Uani 1 1 d . . . . .
N3 N 0.64263(16) 0.44964(10) 0.25880(7) 0.0219(3) Uani 1 1 d . . . . .
C1 C 0.90666(18) 0.27395(12) 0.26921(8) 0.0181(3) Uani 1 1 d . . . . .
C2 C 0.95514(19) 0.42916(12) 0.20895(8) 0.0205(3) Uani 1 1 d . . . . .
C3 C 1.0313(2) 0.37684(13) 0.16138(8) 0.0224(3) Uani 1 1 d . . . . .
C4 C 1.1065(2) 0.43978(14) 0.11888(9) 0.0286(4) Uani 1 1 d . . . . .
H4 H 1.161341 0.409176 0.085726 0.034 Uiso 1 1 calc R U . . .
C5 C 1.1049(2) 0.54427(15) 0.12287(10) 0.0315(4) Uani 1 1 d . . . . .
H5 H 1.157539 0.583257 0.092801 0.038 Uiso 1 1 calc R U . . .
C6 C 1.0267(2) 0.59177(13) 0.17056(10) 0.0292(4) Uani 1 1 d . . . . .
H6 H 1.024095 0.663301 0.173003 0.035 Uiso 1 1 calc R U . . .
C7 C 0.9522(2) 0.53386(13) 0.21468(9) 0.0244(3) Uani 1 1 d . . . . .
H7 H 0.89975 0.565173 0.248458 0.029 Uiso 1 1 calc R U . . .
C8 C 0.77984(19) 0.42549(11) 0.29783(9) 0.0190(3) Uani 1 1 d . . . . .
C9 C 0.7319(2) 0.47209(14) 0.41796(9) 0.0250(3) Uani 1 1 d . . . . .
H9A H 0.737109 0.544386 0.429326 0.037 Uiso 1 1 calc R U . . .
H9B H 0.766872 0.433697 0.462651 0.037 Uiso 1 1 calc R U . . .
H9C H 0.624685 0.453042 0.396549 0.037 Uiso 1 1 calc R U . . .
C10 C 0.99898(18) 0.45450(12) 0.39817(9) 0.0208(3) Uani 1 1 d . . . . .
H10A H 1.059127 0.451944 0.359452 0.031 Uiso 1 1 calc R U . . .
H10B H 1.026553 0.397134 0.430841 0.031 Uiso 1 1 calc R U . . .
H10C H 1.022229 0.517566 0.425708 0.031 Uiso 1 1 calc R U . . .
C11 C 0.5571(2) 0.53953(13) 0.27445(11) 0.0289(4) Uani 1 1 d . . . . .
H11A H 0.515287 0.574488 0.228937 0.043 Uiso 1 1 calc R U . . .
H11B H 0.627369 0.584944 0.306987 0.043 Uiso 1 1 calc R U . . .
H11C H 0.471622 0.518997 0.297855 0.043 Uiso 1 1 calc R U . . .
C12 C 0.5653(2) 0.38992(14) 0.19562(10) 0.0290(4) Uani 1 1 d . . . . .
H12A H 0.543991 0.433105 0.15258 0.044 Uiso 1 1 calc R U . . .
H12B H 0.467482 0.362399 0.205024 0.044 Uiso 1 1 calc R U . . .
H12C H 0.632773 0.334444 0.187147 0.044 Uiso 1 1 calc R U . . .
C13 C 0.9023(2) 0.21022(14) 0.08625(9) 0.0265(4) Uani 1 1 d . . . . .
H13 H 0.800187 0.24337 0.085429 0.032 Uiso 1 1 calc R U . . .
C14 C 0.8814(2) 0.09509(14) 0.09241(9) 0.0294(4) Uani 1 1 d . . . . .
H14A H 0.823267 0.082055 0.131597 0.035 Uiso 1 1 calc R U . . .
H14B H 0.816823 0.070085 0.046361 0.035 Uiso 1 1 calc R U . . .
C15 C 1.0316(2) 0.03362(14) 0.10810(10) 0.0312(4) Uani 1 1 d . . . . .
H15A H 1.007643 -0.03455 0.124396 0.037 Uiso 1 1 calc R U . . .
H15B H 1.070606 0.025735 0.062394 0.037 Uiso 1 1 calc R U . . .
C16 C 1.1600(2) 0.08125(14) 0.16596(9) 0.0282(4) Uani 1 1 d . . . . .
H16A H 1.258249 0.045469 0.165458 0.034 Uiso 1 1 calc R U . . .
H16B H 1.133767 0.070842 0.214363 0.034 Uiso 1 1 calc R U . . .
C17 C 1.1864(2) 0.19472(13) 0.15588(9) 0.0247(3) Uani 1 1 d . . . . .
H17 H 1.265121 0.219855 0.198249 0.03 Uiso 1 1 calc R U . . .
C18 C 1.2483(2) 0.21441(15) 0.08538(10) 0.0302(4) Uani 1 1 d . . . . .
H18A H 1.294695 0.282899 0.088456 0.036 Uiso 1 1 calc R U . . .
H18B H 1.332204 0.165775 0.083111 0.036 Uiso 1 1 calc R U . . .
C19 C 1.1263(3) 0.20606(16) 0.01382(10) 0.0349(4) Uani 1 1 d . . . . .
H19A H 1.163707 0.246092 -0.023776 0.042 Uiso 1 1 calc R U . . .
H19B H 1.120293 0.134734 -0.002385 0.042 Uiso 1 1 calc R U . . .
C20 C 0.9619(2) 0.24104(15) 0.01724(9) 0.0328(4) Uani 1 1 d . . . . .
H20A H 0.889366 0.213537 -0.025697 0.039 Uiso 1 1 calc R U . . .
H20B H 0.958999 0.315493 0.013565 0.039 Uiso 1 1 calc R U . . .
C21 C 0.7224(2) 0.12877(12) 0.41503(9) 0.0219(3) Uani 1 1 d . . . . .
H21A H 0.773638 0.165689 0.459365 0.026 Uiso 1 1 calc R U . . .
H21B H 0.630501 0.167939 0.391866 0.026 Uiso 1 1 calc R U . . .
C22 C 0.6688(2) 0.02478(14) 0.43685(11) 0.0304(4) Uani 1 1 d . . . . .
H22A H 0.599262 -0.006282 0.395154 0.046 Uiso 1 1 calc R U . . .
H22B H 0.613603 0.032729 0.477072 0.046 Uiso 1 1 calc R U . . .
H22C H 0.759257 -0.018386 0.452235 0.046 Uiso 1 1 calc R U . . .
C23 C 1.0405(2) 0.08635(13) 0.40351(9) 0.0248(3) Uani 1 1 d . . . . .
H23A H 1.086265 0.146022 0.43194 0.03 Uiso 1 1 calc R U . . .
H23B H 1.026402 0.03348 0.438793 0.03 Uiso 1 1 calc R U . . .
C24 C 1.1576(2) 0.04825(14) 0.36034(10) 0.0274(4) Uani 1 1 d . . . . .
H24A H 1.111312 -0.006872 0.32814 0.041 Uiso 1 1 calc R U . . .
H24B H 1.249685 0.023664 0.393845 0.041 Uiso 1 1 calc R U . . .
H24C H 1.187564 0.103359 0.331175 0.041 Uiso 1 1 calc R U . . .
C25 C 0.7783(2) 0.03935(13) 0.27964(9) 0.0246(3) Uani 1 1 d . . . . .
H25A H 0.852353 0.03763 0.246182 0.03 Uiso 1 1 calc R U . . .
H25B H 0.768914 -0.029905 0.297884 0.03 Uiso 1 1 calc R U . . .
C26 C 0.6197(2) 0.07326(15) 0.23769(10) 0.0330(4) Uani 1 1 d . . . . .
H26A H 0.630871 0.138159 0.214369 0.049 Uiso 1 1 calc R U . . .
H26B H 0.548317 0.080563 0.271382 0.049 Uiso 1 1 calc R U . . .
H26C H 0.578487 0.022778 0.20046 0.049 Uiso 1 1 calc R U . . .
C28 C 0.1513(2) 0.75595(14) 0.35597(10) 0.0289(4) Uani 1 1 d . . . . .
C29 C 0.6452(3) 0.79706(15) 0.21649(12) 0.0438(5) Uani 1 1 d . . . . .
H29 H 0.720518 0.773594 0.256289 0.053 Uiso 1 1 calc R U . . .
C30 C 0.4896(3) 0.79987(17) 0.22132(13) 0.0474(5) Uani 1 1 d . . . . .
H30 H 0.458078 0.778535 0.264489 0.057 Uiso 1 1 calc R U . . .
C31 C 0.3809(3) 0.83393(17) 0.16289(15) 0.0475(6) Uani 1 1 d . . . . .
H31 H 0.274271 0.835635 0.165705 0.057 Uiso 1 1 calc R U . . .
C32 C 0.4270(3) 0.86494(17) 0.10149(13) 0.0476(6) Uani 1 1 d . . . . .
H32 H 0.351921 0.88854 0.061614 0.057 Uiso 1 1 calc R U . . .
C33 C 0.5801(3) 0.86265(17) 0.09629(12) 0.0458(5) Uani 1 1 d . . . . .
H33 H 0.610731 0.884643 0.053068 0.055 Uiso 1 1 calc R U . . .
C34 C 0.6895(3) 0.82842(16) 0.15380(13) 0.0422(5) Uani 1 1 d . . . . .
H34 H 0.795662 0.826453 0.150174 0.051 Uiso 1 1 calc R U . . .
C35 C 0.5881(3) 0.57560(16) 0.03905(11) 0.0378(5) Uani 1 1 d . . . . .
H35 H 0.648672 0.627602 0.066105 0.045 Uiso 1 1 calc R U . . .
C36 C 0.6584(3) 0.48692(17) 0.02432(11) 0.0383(5) Uani 1 1 d . . . . .
H36 H 0.766811 0.478285 0.040853 0.046 Uiso 1 1 calc R U . . .
C37 C 0.5696(3) 0.41061(16) -0.01476(11) 0.0378(5) Uani 1 1 d . . . . .
H37 H 0.616802 0.349279 -0.024794 0.045 Uiso 1 1 calc R U . . .
B1 B 1.0272(2) 0.25525(14) 0.15368(9) 0.0219(4) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
S1A O5A 1.4387(14) . ?
S1A O3 1.4410(13) . ?
S1A O4 1.4465(13) . ?
S1A C27A 1.834(2) . ?
C27A F3 1.320(2) . ?
C27A F2 1.328(2) . ?
C27A F1A 1.335(2) . ?
S1B O4 1.284(7) . ?
S1B O3 1.345(6) . ?
S1B O5B 1.375(16) . ?
S1B C27B 1.85(2) . ?
C27B F1B 1.382(19) . ?
C27B F2 1.406(18) . ?
C27B F3 1.411(18) . ?
S2 O7 1.4401(13) . ?
S2 O6 1.4424(13) . ?
S2 O8 1.4427(12) . ?
S2 C28 1.829(2) . ?
P1 O2 1.6354(12) . ?
P1 C21 1.7731(17) . ?
P1 C25 1.7781(16) . ?
P1 C23 1.7877(17) . ?
F4 C28 1.336(2) . ?
F5 C28 1.344(2) . ?
F6 C28 1.331(2) . ?
O1 C1 1.2332(19) . ?
O1 B1 1.701(2) . ?
O2 C1 1.351(2) . ?
N1 C1 1.339(2) . ?
N1 C8 1.436(2) . ?
N1 C2 1.454(2) . ?
N2 C8 1.308(2) . ?
N2 C10 1.471(2) . ?
N2 C9 1.471(2) . ?
N3 C8 1.324(2) . ?
N3 C12 1.470(2) . ?
N3 C11 1.473(2) . ?
C2 C7 1.393(2) . ?
C2 C3 1.401(2) . ?
C3 C4 1.406(3) . ?
C3 B1 1.617(2) . ?
C4 C5 1.387(3) . ?
C4 H4 0.95 . ?
C5 C6 1.383(3) . ?
C5 H5 0.95 . ?
C6 C7 1.384(3) . ?
C6 H6 0.95 . ?
C7 H7 0.95 . ?
C9 H9A 0.98 . ?
C9 H9B 0.98 . ?
C9 H9C 0.98 . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 H11A 0.98 . ?
C11 H11B 0.98 . ?
C11 H11C 0.98 . ?
C12 H12A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C13 C14 1.544(3) . ?
C13 C20 1.545(3) . ?
C13 B1 1.612(2) . ?
C13 H13 1 . ?
C14 C15 1.535(3) . ?
C14 H14A 0.99 . ?
C14 H14B 0.99 . ?
C15 C16 1.534(2) . ?
C15 H15A 0.99 . ?
C15 H15B 0.99 . ?
C16 C17 1.539(3) . ?
C16 H16A 0.99 . ?
C16 H16B 0.99 . ?
C17 C18 1.549(2) . ?
C17 B1 1.612(3) . ?
C17 H17 1 . ?
C18 C19 1.547(3) . ?
C18 H18A 0.99 . ?
C18 H18B 0.99 . ?
C19 C20 1.535(3) . ?
C19 H19A 0.99 . ?
C19 H19B 0.99 . ?
C20 H20A 0.99 . ?
C20 H20B 0.99 . ?
C21 C22 1.537(2) . ?
C21 H21A 0.99 . ?
C21 H21B 0.99 . ?
C22 H22A 0.98 . ?
C22 H22B 0.98 . ?
C22 H22C 0.98 . ?
C23 C24 1.518(2) . ?
C23 H23A 0.99 . ?
C23 H23B 0.99 . ?
C24 H24A 0.98 . ?
C24 H24B 0.98 . ?
C24 H24C 0.98 . ?
C25 C26 1.531(3) . ?
C25 H25A 0.99 . ?
C25 H25B 0.99 . ?
C26 H26A 0.98 . ?
C26 H26B 0.98 . ?
C26 H26C 0.98 . ?
C29 C34 1.375(4) . ?
C29 C30 1.389(4) . ?
C29 H29 0.95 . ?
C30 C31 1.384(3) . ?
C30 H30 0.95 . ?
C31 C32 1.359(4) . ?
C31 H31 0.95 . ?
C32 C33 1.370(4) . ?
C32 H32 0.95 . ?
C33 C34 1.377(3) . ?
C33 H33 0.95 . ?
C34 H34 0.95 . ?
C35 C36 1.384(3) . ?
C35 C37 1.385(3) 2_665 ?
C35 H35 0.95 . ?
C36 C37 1.389(3) . ?
C36 H36 0.95 . ?
C37 H37 0.95 . ?

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
O5A S1A O3 114.84(8) . . ?
O5A S1A O4 114.30(9) . . ?
O3 S1A O4 115.08(8) . . ?
O5A S1A C27A 103.24(9) . . ?
O3 S1A C27A 103.30(9) . . ?
O4 S1A C27A 103.90(8) . . ?
F3 C27A F2 109.31(16) . . ?
F3 C27A F1A 107.16(16) . . ?
F2 C27A F1A 106.53(17) . . ?
F3 C27A S1A 111.38(14) . . ?
F2 C27A S1A 110.64(14) . . ?
F1A C27A S1A 111.64(13) . . ?
O4 S1B O3 135.9(6) . . ?
O4 S1B O5B 105.4(10) . . ?
O3 S1B O5B 112.4(10) . . ?
O4 S1B C27B 99.1(7) . . ?
O3 S1B C27B 94.7(7) . . ?
O5B S1B C27B 101.7(12) . . ?
F1B C27B F2 94.0(15) . . ?
F1B C27B F3 95.1(15) . . ?
F2 C27B F3 100.1(12) . . ?
F1B C27B S1B 109.7(14) . . ?
F2 C27B S1B 124.5(12) . . ?
F3 C27B S1B 125.4(12) . . ?
O7 S2 O6 114.90(8) . . ?
O7 S2 O8 115.40(8) . . ?
O6 S2 O8 115.00(8) . . ?
O7 S2 C28 103.11(8) . . ?
O6 S2 C28 102.95(8) . . ?
O8 S2 C28 102.90(8) . . ?
O2 P1 C21 100.46(7) . . ?
O2 P1 C25 109.57(7) . . ?
C21 P1 C25 111.09(8) . . ?
O2 P1 C23 111.37(7) . . ?
C21 P1 C23 109.40(8) . . ?
C25 P1 C23 114.13(8) . . ?
C1 O1 B1 124.46(13) . . ?
C1 O2 P1 128.00(10) . . ?
C1 N1 C8 120.79(13) . . ?
C1 N1 C2 120.63(13) . . ?
C8 N1 C2 118.57(13) . . ?
C8 N2 C10 122.77(13) . . ?
C8 N2 C9 123.61(13) . . ?
C10 N2 C9 113.60(12) . . ?
C8 N3 C12 122.61(14) . . ?
C8 N3 C11 122.57(14) . . ?
C12 N3 C11 114.81(14) . . ?
O1 C1 N1 126.10(15) . . ?
O1 C1 O2 121.01(14) . . ?
N1 C1 O2 112.79(13) . . ?
C7 C2 C3 124.14(16) . . ?
C7 C2 N1 116.33(14) . . ?
C3 C2 N1 119.42(14) . . ?
C2 C3 C4 113.90(15) . . ?
C2 C3 B1 123.04(15) . . ?
C4 C3 B1 123.02(15) . . ?
C5 C4 C3 123.39(17) . . ?
C5 C4 H4 118.3 . . ?
C3 C4 H4 118.3 . . ?
C6 C5 C4 120.10(17) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C7 119.24(17) . . ?
C5 C6 H6 120.4 . . ?
C7 C6 H6 120.4 . . ?
C6 C7 C2 119.21(16) . . ?
C6 C7 H7 120.4 . . ?
C2 C7 H7 120.4 . . ?
N2 C8 N3 126.02(15) . . ?
N2 C8 N1 118.18(14) . . ?
N3 C8 N1 115.70(13) . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 H12A 109.5 . . ?
N3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C20 113.00(15) . . ?
C14 C13 B1 111.88(14) . . ?
C20 C13 B1 105.67(14) . . ?
C14 C13 H13 108.7 . . ?
C20 C13 H13 108.7 . . ?
B1 C13 H13 108.7 . . ?
C15 C14 C13 115.73(15) . . ?
C15 C14 H14A 108.3 . . ?
C13 C14 H14A 108.3 . . ?
C15 C14 H14B 108.3 . . ?
C13 C14 H14B 108.3 . . ?
H14A C14 H14B 107.4 . . ?
C16 C15 C14 113.82(14) . . ?
C16 C15 H15A 108.8 . . ?
C14 C15 H15A 108.8 . . ?
C16 C15 H15B 108.8 . . ?
C14 C15 H15B 108.8 . . ?
H15A C15 H15B 107.7 . . ?
C15 C16 C17 114.56(15) . . ?
C15 C16 H16A 108.6 . . ?
C17 C16 H16A 108.6 . . ?
C15 C16 H16B 108.6 . . ?
C17 C16 H16B 108.6 . . ?
H16A C16 H16B 107.6 . . ?
C16 C17 C18 110.97(14) . . ?
C16 C17 B1 110.12(15) . . ?
C18 C17 B1 110.04(14) . . ?
C16 C17 H17 108.5 . . ?
C18 C17 H17 108.5 . . ?
B1 C17 H17 108.5 . . ?
C19 C18 C17 115.43(16) . . ?
C19 C18 H18A 108.4 . . ?
C17 C18 H18A 108.4 . . ?
C19 C18 H18B 108.4 . . ?
C17 C18 H18B 108.4 . . ?
H18A C18 H18B 107.5 . . ?
C20 C19 C18 116.21(15) . . ?
C20 C19 H19A 108.2 . . ?
C18 C19 H19A 108.2 . . ?
C20 C19 H19B 108.2 . . ?
C18 C19 H19B 108.2 . . ?
H19A C19 H19B 107.4 . . ?
C19 C20 C13 115.55(16) . . ?
C19 C20 H20A 108.4 . . ?
C13 C20 H20A 108.4 . . ?
C19 C20 H20B 108.4 . . ?
C13 C20 H20B 108.4 . . ?
H20A C20 H20B 107.5 . . ?
C22 C21 P1 112.72(12) . . ?
C22 C21 H21A 109 . . ?
P1 C21 H21A 109 . . ?
C22 C21 H21B 109 . . ?
P1 C21 H21B 109 . . ?
H21A C21 H21B 107.8 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 P1 117.80(12) . . ?
C24 C23 H23A 107.9 . . ?
P1 C23 H23A 107.9 . . ?
C24 C23 H23B 107.9 . . ?
P1 C23 H23B 107.9 . . ?
H23A C23 H23B 107.2 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 P1 112.33(12) . . ?
C26 C25 H25A 109.1 . . ?
P1 C25 H25A 109.1 . . ?
C26 C25 H25B 109.1 . . ?
P1 C25 H25B 109.1 . . ?
H25A C25 H25B 107.9 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
F6 C28 F4 107.56(15) . . ?
F6 C28 F5 107.84(15) . . ?
F4 C28 F5 107.15(15) . . ?
F6 C28 S2 111.83(13) . . ?
F4 C28 S2 111.53(12) . . ?
F5 C28 S2 110.73(13) . . ?
C34 C29 C30 119.7(2) . . ?
C34 C29 H29 120.2 . . ?
C30 C29 H29 120.2 . . ?
C31 C30 C29 119.6(2) . . ?
C31 C30 H30 120.2 . . ?
C29 C30 H30 120.2 . . ?
C32 C31 C30 119.9(2) . . ?
C32 C31 H31 120.1 . . ?
C30 C31 H31 120.1 . . ?
C31 C32 C33 120.9(2) . . ?
C31 C32 H32 119.5 . . ?
C33 C32 H32 119.5 . . ?
C32 C33 C34 119.9(2) . . ?
C32 C33 H33 120.1 . . ?
C34 C33 H33 120.1 . . ?
C29 C34 C33 120.0(2) . . ?
C29 C34 H34 120 . . ?
C33 C34 H34 120 . . ?
C36 C35 C37 120.74(19) . 2_665 ?
C36 C35 H35 119.6 . . ?
C37 C35 H35 119.6 2_665 . ?
C35 C36 C37 119.6(2) . . ?
C35 C36 H36 120.2 . . ?
C37 C36 H36 120.2 . . ?
C35 C37 C36 119.7(2) 2_665 . ?
C35 C37 H37 120.2 2_665 . ?
C36 C37 H37 120.2 . . ?
C17 B1 C13 106.91(13) . . ?
C17 B1 C3 119.69(15) . . ?
C13 B1 C3 115.55(14) . . ?
C17 B1 O1 104.26(13) . . ?
C13 B1 O1 106.06(13) . . ?
C3 B1 O1 102.84(12) . . ?


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

data_5
_database_code_depnum_ccdc_archive 'CCDC 2127868'
loop_
_audit_author_name
_audit_author_address
'Daniel Unruh'
;Texas Tech University
United States of America
;
_audit_update_record             
;
2021-12-10 deposited with the CCDC.	2022-07-22 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT340_5                   
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01009 Ang.  
RESPONSE: Due to the poor diffraction quality of the crystals.
;
_vrf_PLAT410_5                   
;
PROBLEM: Short Intra H...H Contact  H15A     ..H19B     .       1.84 Ang.  
RESPONSE: This interaction is typically short in BBN molecules, but is more
          so than normal due to slight disorder about the entire molecule.
;
_vrf_PLAT082_5                   
;
PROBLEM: High R1 Value ..................................       0.11 Report
RESPONSE: Due to the poor diffraction quality of the crystals, especially
          at high angles.
;
_vrf_PLAT084_5                   
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.34 Report
RESPONSE: Due to the poor diffraction quality of the crystals.
;
_vrf_PLAT260_5                   
;
PROBLEM: Large Average Ueq of Residue Including       C57      0.121 Check 
RESPONSE: Due to disorder about the interstitial benzene molecule.
;
_vrf_PLAT331_5                   
;
PROBLEM: Small Aver Phenyl C-C Dist C57      --C57_a    .       1.37 Ang.  
RESPONSE: Due to disorder about the interstitial benzene molecule.
;
_vrf_PLAT334_5                   
;
PROBLEM: Small Aver. Benzene C-C Dist C45      -C50             1.37 Ang.  
RESPONSE: Due to slight disorder about the entire molecule.
;
_vrf_PLAT360_5                   
;
PROBLEM: Short  C(sp3)-C(sp3) Bond  C14      - C15      .       1.42 Ang.  
RESPONSE: Due to slight disorder about the entire molecule due to 
          suspected solvent loss prior to analysis.
;
_vrf_PLAT906_5                   
;
PROBLEM: Large K Value in the Analysis of Variance ......      8.965 Check 
RESPONSE: Due to poor high angle data.
;
_vrf_PLAT911_5                   
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         26 Report
RESPONSE: These reflections were omitted during the absorption correction.
;
_vrf_PLAT978_5                   
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info  
RESPONSE: The remaining residual electron density is located about the 
          fluorine atoms primarily.
;
# end Validation Reply Form

_audit_creation_date             2020-02-21T09:41:33-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C59 H33 Al2 B F30 N3 O2'
_chemical_formula_weight         1450.65

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_Int_Tables_number      60
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   18.30960(10)
_cell_length_b                   26.0399(3)
_cell_length_c                   27.5573(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     13138.8(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    30710
_cell_measurement_theta_min      2.895
_cell_measurement_theta_max      73.247

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       irregular
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_size_max          0.316
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.09
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_F_000             5800
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 2 1 0.0458
2 -15 -7 0.0412
-12 0 1 0.1471
0 6 -17 0.0393
1 -6 17 0.0376
11 0 8 0.1481
-12 -3 -1 0.1384
2 6 16 0.0408
-1 6 17 0.0561
7 6 13 0.098
4 16 0 0.0654
0 17 0 0.0458
2 -4 -17 0.045
9 -1 -12 0.1232
1 -13 11 0.0337


#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.575
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.40.70a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
                        a multifaceted crystal model
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.617
_exptl_absorpt_correction_T_max  1
_shelx_estimated_absorpt_T_min   0.636
_shelx_estimated_absorpt_T_max   0.871

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_ambient_temperature      100(2)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_detector_area_resol_mean 10
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_ub_11      0.0172275
_diffrn_orient_matrix_ub_12      -0.057666
_diffrn_orient_matrix_ub_13      -0.0052627
_diffrn_orient_matrix_ub_21      0.0026972
_diffrn_orient_matrix_ub_22      0.0060836
_diffrn_orient_matrix_ub_23      -0.055586
_diffrn_orient_matrix_ub_31      0.0822678
_diffrn_orient_matrix_ub_32      0.0118545
_diffrn_orient_matrix_ub_33      0.00292
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_unetI/netI     0.0837
_diffrn_reflns_number            89839
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.95
_diffrn_reflns_theta_max         77.552
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.978
_reflns_Friedel_coverage         0
_reflns_number_total             13677
_reflns_number_gt                10215
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrysAlisPro 1.171.40.70a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.70a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.70a (Rigaku OD, 2020)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#


_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom


#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_shelx_SHELXL_version_number     2018/3
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1869P)²+28.1401P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         13677
_refine_ls_number_parameters     878
_refine_ls_number_restraints     801
_refine_ls_R_factor_all          0.1268
_refine_ls_R_factor_gt           0.1077
_refine_ls_wR_factor_ref         0.3396
_refine_ls_wR_factor_gt          0.3191
_refine_ls_goodness_of_fit_ref   1.01
_refine_ls_restrained_S_all      0.987
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.097

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#

_refine_special_details          
;Due to the suspected loss and disorder of interstitial solvent molecules, 
 there is slight disorder about the whole structure. To help with maintaining
 reasonable ADP values the RIGU restraint was applied globally.
   
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.855  0.250       618       125 ' '
   2 -0.007  0.355  0.250       618       125 ' '
   3 -0.001  0.145  0.750       617       125 ' '
   4 -0.010  0.645  0.750       617       125 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?

  The unit cell contains 12 disordered benzene molecules in the interstitial 
  space which have been treated as a diffuse contribution to the overall 
  scattering without specific atoms positions by PLATON/SQUEEZE. The squeezed
  atoms were not included in the CIF.
  
  References:
  Spek, A.L. (2009). Acta Cryst. D65, 148-155.
  Spek, A.L. (2015). Acta Cryst. C71, 9-18.,SQUEEZE
;

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.213 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.009 0.0039 '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 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
Al1 Al 0.42884(7) 0.28164(5) 0.52265(5) 0.0494(3) Uani 1 1 d . . . . .
Al2 Al 0.25892(7) 0.38751(6) 0.45334(5) 0.0537(4) Uani 1 1 d . . . . .
F1 F 0.46787(19) 0.33926(14) 0.61703(13) 0.0768(9) Uani 1 1 d . . . . .
F2 F 0.5223(3) 0.3055(3) 0.70229(17) 0.138(2) Uani 1 1 d . . . . .
F3 F 0.5659(4) 0.2064(3) 0.71262(18) 0.152(2) Uani 1 1 d . . . . .
F4 F 0.5560(3) 0.14073(19) 0.6366(2) 0.1180(16) Uani 1 1 d . . . . .
F5 F 0.4984(2) 0.17210(14) 0.55322(15) 0.0873(10) Uani 1 1 d . . . . .
F6 F 0.45405(15) 0.40526(11) 0.51758(11) 0.0605(7) Uani 1 1 d . . . . .
F7 F 0.55773(18) 0.46010(12) 0.47208(14) 0.0762(9) Uani 1 1 d . . . . .
F8 F 0.6603(2) 0.41145(17) 0.4172(2) 0.1074(15) Uani 1 1 d . . . . .
F9 F 0.6577(2) 0.30763(19) 0.4096(2) 0.1238(19) Uani 1 1 d . . . . .
F10 F 0.55497(18) 0.25246(13) 0.45605(15) 0.0810(10) Uani 1 1 d . . . . .
F11 F 0.4172(2) 0.25872(15) 0.40740(11) 0.0768(9) Uani 1 1 d . . . . .
F12 F 0.3670(3) 0.17722(19) 0.35971(14) 0.1050(14) Uani 1 1 d . . . . .
F13 F 0.3082(2) 0.09635(17) 0.40912(17) 0.1045(14) Uani 1 1 d . . . . .
F14 F 0.2957(2) 0.10096(14) 0.50709(16) 0.0946(12) Uani 1 1 d . . . . .
F15 F 0.34275(18) 0.18382(12) 0.55539(11) 0.0694(8) Uani 1 1 d . . . . .
F16 F 0.1947(2) 0.47241(18) 0.38050(14) 0.0938(11) Uani 1 1 d . . . . .
F17 F 0.0606(3) 0.5132(2) 0.3752(2) 0.1322(19) Uani 1 1 d . . . . .
F18 F -0.0441(2) 0.4864(2) 0.4390(2) 0.134(2) Uani 1 1 d . . . . .
F19 F -0.0140(2) 0.4183(2) 0.51116(19) 0.1097(15) Uani 1 1 d . . . . .
F20 F 0.11893(18) 0.37592(16) 0.51703(14) 0.0815(9) Uani 1 1 d . . . . .
F21 F 0.2636(3) 0.34818(18) 0.34768(13) 0.1002(12) Uani 1 1 d . . . . .
F22 F 0.2258(4) 0.2579(3) 0.30741(18) 0.145(2) Uani 1 1 d . . . . .
F23 F 0.1759(3) 0.1789(2) 0.3653(2) 0.136(2) Uani 1 1 d . . . . .
F24 F 0.1700(2) 0.19164(16) 0.4617(2) 0.1021(13) Uani 1 1 d . . . . .
F25 F 0.21126(17) 0.28002(14) 0.50283(12) 0.0735(8) Uani 1 1 d . . . . .
F26 F 0.4041(2) 0.36756(18) 0.38889(14) 0.0899(11) Uani 1 1 d . . . . .
F27 F 0.5061(2) 0.4345(2) 0.3578(2) 0.1289(19) Uani 1 1 d . . . . .
F28 F 0.4951(2) 0.5374(2) 0.38178(19) 0.1182(17) Uani 1 1 d . . . . .
F29 F 0.3803(2) 0.57090(16) 0.43388(15) 0.0966(12) Uani 1 1 d . . . . .
F30 F 0.2827(2) 0.50306(14) 0.46672(13) 0.0826(9) Uani 1 1 d . . . . .
O1 O 0.35344(17) 0.32030(14) 0.54367(12) 0.0570(8) Uani 1 1 d . . . . .
O2 O 0.27825(17) 0.38156(14) 0.51742(11) 0.0554(8) Uani 1 1 d . . . . .
N1 N 0.2777(2) 0.36067(14) 0.59638(13) 0.0479(8) Uani 1 1 d . . . . .
N2 N 0.1607(2) 0.3898(2) 0.62012(17) 0.0682(11) Uani 1 1 d . . . . .
N3 N 0.2497(2) 0.44790(18) 0.59344(16) 0.0626(10) Uani 1 1 d . . . . .
C1 C 0.3053(2) 0.35365(18) 0.55016(16) 0.0470(9) Uani 1 1 d . . . . .
C2 C 0.2938(3) 0.3245(2) 0.63542(17) 0.0572(11) Uani 1 1 d . . . . .
C3 C 0.3185(3) 0.3420(2) 0.68093(19) 0.0689(13) Uani 1 1 d . . . . .
C4 C 0.3360(5) 0.3007(3) 0.7132(2) 0.086(2) Uani 1 1 d . . . . .
H4 H 0.353997 0.308877 0.744616 0.103 Uiso 1 1 calc R U . . .
C5 C 0.3281(5) 0.2501(3) 0.7010(2) 0.088(2) Uani 1 1 d . . . . .
H5 H 0.340753 0.22442 0.723948 0.106 Uiso 1 1 calc R U . . .
C6 C 0.3027(4) 0.2358(2) 0.6568(2) 0.0749(15) Uani 1 1 d . . . . .
H6 H 0.297237 0.200567 0.648697 0.09 Uiso 1 1 calc R U . . .
C7 C 0.2851(3) 0.2735(2) 0.6242(2) 0.0644(12) Uani 1 1 d . . . . .
H7 H 0.26646 0.264148 0.593241 0.077 Uiso 1 1 calc R U . . .
C8 C 0.2276(3) 0.4017(2) 0.60393(18) 0.0578(11) Uani 1 1 d . . . . .
C9 C 0.1119(3) 0.4266(3) 0.6436(2) 0.0838(18) Uani 1 1 d . . . . .
H9A H 0.140041 0.456509 0.654314 0.126 Uiso 1 1 calc R U . . .
H9B H 0.088693 0.410322 0.671743 0.126 Uiso 1 1 calc R U . . .
H9C H 0.074252 0.437515 0.620555 0.126 Uiso 1 1 calc R U . . .
C10 C 0.1290(3) 0.3379(3) 0.6153(3) 0.0808(17) Uani 1 1 d . . . . .
H10A H 0.082687 0.339934 0.597623 0.121 Uiso 1 1 calc R U . . .
H10B H 0.120326 0.323435 0.647663 0.121 Uiso 1 1 calc R U . . .
H10C H 0.163039 0.315751 0.597519 0.121 Uiso 1 1 calc R U . . .
C11 C 0.3268(3) 0.4610(2) 0.5907(2) 0.0690(13) Uani 1 1 d . . . . .
H11A H 0.341681 0.463212 0.556642 0.103 Uiso 1 1 calc R U . . .
H11B H 0.355572 0.434356 0.607078 0.103 Uiso 1 1 calc R U . . .
H11C H 0.335075 0.494098 0.606657 0.103 Uiso 1 1 calc R U . . .
C12 C 0.2021(4) 0.4888(3) 0.5762(2) 0.0810(17) Uani 1 1 d . . . . .
H12A H 0.226922 0.508105 0.550463 0.122 Uiso 1 1 calc R U . . .
H12B H 0.190473 0.512016 0.603116 0.122 Uiso 1 1 calc R U . . .
H12C H 0.156893 0.473954 0.563353 0.122 Uiso 1 1 calc R U . . .
C13 C 0.3962(4) 0.4171(3) 0.7286(3) 0.099(2) Uani 1 1 d . . . . .
H13 H 0.439446 0.397659 0.716146 0.119 Uiso 1 1 calc R U . . .
C14 C 0.3899(5) 0.4121(4) 0.7848(3) 0.107(2) Uani 1 1 d . . . . .
H14A H 0.397462 0.375545 0.793256 0.128 Uiso 1 1 calc R U . . .
H14B H 0.430775 0.431675 0.799335 0.128 Uiso 1 1 calc R U . . .
C15 C 0.3244(5) 0.4286(4) 0.8075(3) 0.107(2) Uani 1 1 d . . . . .
H15A H 0.323669 0.466581 0.808704 0.128 Uiso 1 1 calc R U . . .
H15B H 0.323443 0.415736 0.84132 0.128 Uiso 1 1 calc R U . . .
C16 C 0.2561(5) 0.4097(4) 0.7810(3) 0.103(2) Uani 1 1 d . . . . .
H16A H 0.212325 0.423828 0.797263 0.124 Uiso 1 1 calc R U . . .
H16B H 0.25374 0.371779 0.783366 0.124 Uiso 1 1 calc R U . . .
C17 C 0.2547(4) 0.4254(3) 0.7264(3) 0.0850(17) Uani 1 1 d . . . . .
H17 H 0.208857 0.412333 0.710945 0.102 Uiso 1 1 calc R U . . .
C18 C 0.2608(5) 0.4845(3) 0.7180(4) 0.106(2) Uani 1 1 d . . . . .
H18A H 0.246521 0.492235 0.684163 0.127 Uiso 1 1 calc R U . . .
H18B H 0.225632 0.502076 0.739688 0.127 Uiso 1 1 calc R U . . .
C19 C 0.3384(5) 0.5070(3) 0.7274(4) 0.114(3) Uani 1 1 d . . . . .
H19A H 0.342531 0.539558 0.709097 0.137 Uiso 1 1 calc R U . . .
H19B H 0.34213 0.51549 0.76228 0.137 Uiso 1 1 calc R U . . .
C20 C 0.4011(5) 0.4747(4) 0.7145(3) 0.107(2) Uani 1 1 d . . . . .
H20A H 0.445091 0.489345 0.730165 0.129 Uiso 1 1 calc R U . . .
H20B H 0.408437 0.476896 0.678999 0.129 Uiso 1 1 calc R U . . .
C21 C 0.4774(3) 0.2567(2) 0.58322(19) 0.0610(11) Uani 1 1 d . . . . .
C22 C 0.4872(3) 0.2896(2) 0.6215(2) 0.0682(13) Uani 1 1 d . . . . .
C23 C 0.5153(4) 0.2726(3) 0.6654(2) 0.094(2) Uani 1 1 d . . . . .
C24 C 0.5385(4) 0.2231(4) 0.6699(3) 0.104(2) Uani 1 1 d . . . . .
C25 C 0.5330(4) 0.1895(3) 0.6317(3) 0.0872(18) Uani 1 1 d . . . . .
C26 C 0.5023(3) 0.2069(3) 0.5897(2) 0.0725(14) Uani 1 1 d . . . . .
C27 C 0.4988(2) 0.3263(2) 0.48737(18) 0.0537(10) Uani 1 1 d . . . . .
C28 C 0.5035(2) 0.37937(19) 0.49050(19) 0.0554(10) Uani 1 1 d . . . . .
C29 C 0.5554(3) 0.4090(2) 0.4675(2) 0.0642(12) Uani 1 1 d . . . . .
C30 C 0.6079(3) 0.3834(3) 0.4399(3) 0.0792(17) Uani 1 1 d . . . . .
C31 C 0.6059(3) 0.3317(3) 0.4358(3) 0.0824(18) Uani 1 1 d . . . . .
C32 C 0.5523(3) 0.3044(2) 0.4596(2) 0.0658(13) Uani 1 1 d . . . . .
C33 C 0.3851(3) 0.22465(18) 0.48421(17) 0.0532(10) Uani 1 1 d . . . . .
C34 C 0.3892(3) 0.2205(2) 0.43375(19) 0.0626(12) Uani 1 1 d . . . . .
C35 C 0.3625(3) 0.1785(3) 0.4087(2) 0.0749(14) Uani 1 1 d . . . . .
C36 C 0.3330(3) 0.1384(2) 0.4325(2) 0.0745(14) Uani 1 1 d . . . . .
C37 C 0.3261(3) 0.1404(2) 0.4827(2) 0.0710(14) Uani 1 1 d . . . . .
C38 C 0.3516(3) 0.1835(2) 0.5066(2) 0.0602(11) Uani 1 1 d . . . . .
C39 C 0.1630(3) 0.4232(2) 0.4495(2) 0.0661(13) Uani 1 1 d . . . . .
C40 C 0.1448(4) 0.4590(2) 0.4135(2) 0.0748(14) Uani 1 1 d . . . . .
C41 C 0.0768(4) 0.4804(3) 0.4097(3) 0.0920(18) Uani 1 1 d . . . . .
C42 C 0.0236(4) 0.4656(3) 0.4426(3) 0.0952(19) Uani 1 1 d . . . . .
C43 C 0.0378(3) 0.4315(3) 0.4788(3) 0.0844(16) Uani 1 1 d . . . . .
C44 C 0.1063(3) 0.4111(2) 0.4809(2) 0.0684(13) Uani 1 1 d . . . . .
C45 C 0.2407(3) 0.3174(2) 0.42644(19) 0.0600(11) Uani 1 1 d . . . . .
C46 C 0.2416(4) 0.3084(3) 0.3778(2) 0.0742(14) Uani 1 1 d . . . . .
C47 C 0.2222(4) 0.2635(4) 0.3565(3) 0.0970(19) Uani 1 1 d . . . . .
C48 C 0.1968(4) 0.2252(3) 0.3854(3) 0.0932(18) Uani 1 1 d . . . . .
C49 C 0.1935(3) 0.2307(3) 0.4345(3) 0.0787(15) Uani 1 1 d . . . . .
C50 C 0.2154(3) 0.2763(2) 0.4537(2) 0.0651(12) Uani 1 1 d . . . . .
C51 C 0.3390(3) 0.4325(2) 0.42765(18) 0.0631(12) Uani 1 1 d . . . . .
C52 C 0.3953(3) 0.4188(3) 0.4004(2) 0.0737(14) Uani 1 1 d . . . . .
C53 C 0.4497(4) 0.4533(4) 0.3839(2) 0.0876(17) Uani 1 1 d . . . . .
C54 C 0.4432(4) 0.5034(3) 0.3958(3) 0.0876(17) Uani 1 1 d . . . . .
C55 C 0.3871(4) 0.5205(3) 0.4224(2) 0.0785(15) Uani 1 1 d . . . . .
C56 C 0.3357(3) 0.4853(2) 0.4396(2) 0.0672(12) Uani 1 1 d . . . . .
C57 C 0.0287(5) 0.5504(4) 0.2671(3) 0.110(2) Uani 1 1 d . . . . .
H57 H 0.04892 0.518865 0.27813 0.132 Uiso 1 1 calc R U . . .
C58 C 0.0546(5) 0.5950(5) 0.2840(3) 0.113(3) Uani 1 1 d . . . . .
H58 H 0.092638 0.595351 0.307439 0.136 Uiso 1 1 calc R U . . .
C59 C 0.0252(7) 0.6410(5) 0.2669(4) 0.139(4) Uani 1 1 d . . . . .
H59 H 0.041889 0.672728 0.279892 0.167 Uiso 1 1 calc R U . . .
B1 B 0.3218(4) 0.3944(3) 0.7067(2) 0.0734(16) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Al1 O1 1.804(4) . ?
Al1 C27 1.984(5) . ?
Al1 C33 1.991(5) . ?
Al1 C21 2.000(5) . ?
Al2 O2 1.808(3) . ?
Al2 C39 1.990(5) . ?
Al2 C45 2.000(6) . ?
Al2 C51 2.006(6) . ?
F1 C22 1.345(7) . ?
F2 C23 1.337(9) . ?
F3 C24 1.352(7) . ?
F4 C25 1.344(8) . ?
F5 C26 1.355(8) . ?
F6 C28 1.353(6) . ?
F7 C29 1.337(6) . ?
F8 C30 1.358(6) . ?
F9 C31 1.347(7) . ?
F10 C32 1.356(7) . ?
F11 C34 1.334(7) . ?
F12 C35 1.354(7) . ?
F13 C36 1.350(7) . ?
F14 C37 1.348(7) . ?
F15 C38 1.355(6) . ?
F16 C40 1.337(8) . ?
F17 C41 1.313(9) . ?
F18 C42 1.357(7) . ?
F19 C43 1.346(9) . ?
F20 C44 1.374(7) . ?
F21 C46 1.387(8) . ?
F22 C47 1.363(9) . ?
F23 C48 1.381(8) . ?
F24 C49 1.336(8) . ?
F25 C50 1.358(7) . ?
F26 C52 1.380(8) . ?
F27 C53 1.350(8) . ?
F28 C54 1.355(8) . ?
F29 C55 1.356(8) . ?
F30 C56 1.310(7) . ?
O1 C1 1.250(6) . ?
O2 C1 1.260(6) . ?
N1 C1 1.382(6) . ?
N1 C8 1.425(6) . ?
N1 C2 1.460(6) . ?
N2 C8 1.340(7) . ?
N2 C9 1.460(8) . ?
N2 C10 1.478(8) . ?
N3 C8 1.301(7) . ?
N3 C11 1.454(7) . ?
N3 C12 1.457(7) . ?
C2 C7 1.375(8) . ?
C2 C3 1.408(7) . ?
C3 C4 1.432(8) . ?
C3 B1 1.539(10) . ?
C4 C5 1.368(9) . ?
C4 H4 0.95 . ?
C5 C6 1.355(9) . ?
C5 H5 0.95 . ?
C6 C7 1.369(8) . ?
C6 H6 0.95 . ?
C7 H7 0.95 . ?
C9 H9A 0.98 . ?
C9 H9B 0.98 . ?
C9 H9C 0.98 . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 H11A 0.98 . ?
C11 H11B 0.98 . ?
C11 H11C 0.98 . ?
C12 H12A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C13 C20 1.552(12) . ?
C13 C14 1.558(13) . ?
C13 B1 1.603(10) . ?
C13 H13 1 . ?
C14 C15 1.421(13) . ?
C14 H14A 0.99 . ?
C14 H14B 0.99 . ?
C15 C16 1.529(12) . ?
C15 H15A 0.99 . ?
C15 H15B 0.99 . ?
C16 C17 1.560(11) . ?
C16 H16A 0.99 . ?
C16 H16B 0.99 . ?
C17 C18 1.559(11) . ?
C17 B1 1.568(11) . ?
C17 H17 1 . ?
C18 C19 1.557(12) . ?
C18 H18A 0.99 . ?
C18 H18B 0.99 . ?
C19 C20 1.467(13) . ?
C19 H19A 0.99 . ?
C19 H19B 0.99 . ?
C20 H20A 0.99 . ?
C20 H20B 0.99 . ?
C21 C22 1.371(8) . ?
C21 C26 1.386(8) . ?
C22 C23 1.388(9) . ?
C23 C24 1.361(12) . ?
C24 C25 1.373(12) . ?
C25 C26 1.364(8) . ?
C27 C32 1.368(7) . ?
C27 C28 1.387(7) . ?
C28 C29 1.378(7) . ?
C29 C30 1.396(9) . ?
C30 C31 1.350(9) . ?
C31 C32 1.379(8) . ?
C33 C38 1.380(7) . ?
C33 C34 1.397(7) . ?
C34 C35 1.383(8) . ?
C35 C36 1.344(10) . ?
C36 C37 1.390(9) . ?
C37 C38 1.382(8) . ?
C39 C44 1.388(8) . ?
C39 C40 1.400(8) . ?
C40 C41 1.367(9) . ?
C41 C42 1.384(12) . ?
C42 C43 1.361(12) . ?
C43 C44 1.363(8) . ?
C45 C46 1.360(8) . ?
C45 C50 1.387(8) . ?
C46 C47 1.356(10) . ?
C47 C48 1.357(12) . ?
C48 C49 1.363(11) . ?
C49 C50 1.359(8) . ?
C51 C52 1.325(8) . ?
C51 C56 1.415(9) . ?
C52 C53 1.417(10) . ?
C53 C54 1.351(12) . ?
C54 C55 1.339(11) . ?
C55 C56 1.395(9) . ?
C57 C58 1.337(13) . ?
C57 C57 1.414(19) 3 ?
C57 H57 0.95 . ?
C58 C59 1.396(15) . ?
C58 H58 0.95 . ?
C59 C59 1.31(2) 3 ?
C59 H59 0.95 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Al1 C27 108.91(19) . . ?
O1 Al1 C33 106.21(18) . . ?
C27 Al1 C33 115.8(2) . . ?
O1 Al1 C21 104.7(2) . . ?
C27 Al1 C21 108.2(2) . . ?
C33 Al1 C21 112.4(2) . . ?
O2 Al2 C39 105.4(2) . . ?
O2 Al2 C45 108.5(2) . . ?
C39 Al2 C45 105.0(2) . . ?
O2 Al2 C51 104.58(18) . . ?
C39 Al2 C51 110.7(3) . . ?
C45 Al2 C51 121.7(2) . . ?
C1 O1 Al1 166.7(3) . . ?
C1 O2 Al2 145.7(3) . . ?
C1 N1 C8 118.0(4) . . ?
C1 N1 C2 121.3(4) . . ?
C8 N1 C2 120.4(4) . . ?
C8 N2 C9 123.7(5) . . ?
C8 N2 C10 122.7(5) . . ?
C9 N2 C10 113.6(5) . . ?
C8 N3 C11 122.0(5) . . ?
C8 N3 C12 124.3(5) . . ?
C11 N3 C12 113.1(5) . . ?
O1 C1 O2 125.1(4) . . ?
O1 C1 N1 118.8(4) . . ?
O2 C1 N1 116.1(4) . . ?
C7 C2 C3 123.4(5) . . ?
C7 C2 N1 115.7(4) . . ?
C3 C2 N1 120.9(5) . . ?
C2 C3 C4 112.5(5) . . ?
C2 C3 B1 135.2(5) . . ?
C4 C3 B1 111.7(5) . . ?
C5 C4 C3 123.1(6) . . ?
C5 C4 H4 118.4 . . ?
C3 C4 H4 118.4 . . ?
C6 C5 C4 121.5(6) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C5 C6 C7 118.3(6) . . ?
C5 C6 H6 120.9 . . ?
C7 C6 H6 120.9 . . ?
C6 C7 C2 121.2(6) . . ?
C6 C7 H7 119.4 . . ?
C2 C7 H7 119.4 . . ?
N3 C8 N2 124.9(5) . . ?
N3 C8 N1 117.4(4) . . ?
N2 C8 N1 117.6(5) . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 H12A 109.5 . . ?
N3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C20 C13 C14 109.4(7) . . ?
C20 C13 B1 108.1(7) . . ?
C14 C13 B1 106.3(6) . . ?
C20 C13 H13 110.9 . . ?
C14 C13 H13 110.9 . . ?
B1 C13 H13 110.9 . . ?
C15 C14 C13 118.4(7) . . ?
C15 C14 H14A 107.7 . . ?
C13 C14 H14A 107.7 . . ?
C15 C14 H14B 107.7 . . ?
C13 C14 H14B 107.7 . . ?
H14A C14 H14B 107.1 . . ?
C14 C15 C16 112.5(7) . . ?
C14 C15 H15A 109.1 . . ?
C16 C15 H15A 109.1 . . ?
C14 C15 H15B 109.1 . . ?
C16 C15 H15B 109.1 . . ?
H15A C15 H15B 107.8 . . ?
C15 C16 C17 113.0(6) . . ?
C15 C16 H16A 109 . . ?
C17 C16 H16A 109 . . ?
C15 C16 H16B 109 . . ?
C17 C16 H16B 109 . . ?
H16A C16 H16B 107.8 . . ?
C18 C17 C16 113.6(7) . . ?
C18 C17 B1 113.6(6) . . ?
C16 C17 B1 100.6(6) . . ?
C18 C17 H17 109.5 . . ?
C16 C17 H17 109.5 . . ?
B1 C17 H17 109.5 . . ?
C19 C18 C17 114.3(6) . . ?
C19 C18 H18A 108.7 . . ?
C17 C18 H18A 108.7 . . ?
C19 C18 H18B 108.7 . . ?
C17 C18 H18B 108.7 . . ?
H18A C18 H18B 107.6 . . ?
C20 C19 C18 117.4(7) . . ?
C20 C19 H19A 108 . . ?
C18 C19 H19A 108 . . ?
C20 C19 H19B 108 . . ?
C18 C19 H19B 108 . . ?
H19A C19 H19B 107.2 . . ?
C19 C20 C13 116.6(7) . . ?
C19 C20 H20A 108.1 . . ?
C13 C20 H20A 108.1 . . ?
C19 C20 H20B 108.1 . . ?
C13 C20 H20B 108.1 . . ?
H20A C20 H20B 107.3 . . ?
C22 C21 C26 116.3(5) . . ?
C22 C21 Al1 119.7(4) . . ?
C26 C21 Al1 123.9(4) . . ?
F1 C22 C21 119.8(5) . . ?
F1 C22 C23 119.0(6) . . ?
C21 C22 C23 121.2(6) . . ?
F2 C23 C24 120.5(6) . . ?
F2 C23 C22 119.6(7) . . ?
C24 C23 C22 119.9(7) . . ?
F3 C24 C23 120.0(8) . . ?
F3 C24 C25 119.2(8) . . ?
C23 C24 C25 120.7(6) . . ?
F4 C25 C26 121.8(7) . . ?
F4 C25 C24 120.2(6) . . ?
C26 C25 C24 117.9(7) . . ?
F5 C26 C25 115.5(6) . . ?
F5 C26 C21 120.8(5) . . ?
C25 C26 C21 123.7(7) . . ?
C32 C27 C28 113.9(5) . . ?
C32 C27 Al1 119.4(4) . . ?
C28 C27 Al1 126.4(4) . . ?
F6 C28 C29 115.8(5) . . ?
F6 C28 C27 119.3(4) . . ?
C29 C28 C27 124.9(5) . . ?
F7 C29 C28 122.4(5) . . ?
F7 C29 C30 120.3(5) . . ?
C28 C29 C30 117.2(5) . . ?
C31 C30 F8 121.1(6) . . ?
C31 C30 C29 120.2(5) . . ?
F8 C30 C29 118.7(6) . . ?
F9 C31 C30 119.3(5) . . ?
F9 C31 C32 121.1(6) . . ?
C30 C31 C32 119.6(6) . . ?
F10 C32 C27 118.9(5) . . ?
F10 C32 C31 117.0(5) . . ?
C27 C32 C31 124.1(5) . . ?
C38 C33 C34 114.1(5) . . ?
C38 C33 Al1 121.3(4) . . ?
C34 C33 Al1 124.5(4) . . ?
F11 C34 C35 117.1(5) . . ?
F11 C34 C33 120.3(5) . . ?
C35 C34 C33 122.6(5) . . ?
C36 C35 F12 119.4(6) . . ?
C36 C35 C34 120.9(6) . . ?
F12 C35 C34 119.7(6) . . ?
C35 C36 F13 122.2(6) . . ?
C35 C36 C37 119.5(5) . . ?
F13 C36 C37 118.3(6) . . ?
F14 C37 C38 121.4(6) . . ?
F14 C37 C36 120.4(5) . . ?
C38 C37 C36 118.2(6) . . ?
F15 C38 C33 119.4(4) . . ?
F15 C38 C37 115.9(5) . . ?
C33 C38 C37 124.6(5) . . ?
C44 C39 C40 114.4(5) . . ?
C44 C39 Al2 121.4(4) . . ?
C40 C39 Al2 124.0(5) . . ?
F16 C40 C41 117.6(6) . . ?
F16 C40 C39 119.5(5) . . ?
C41 C40 C39 122.9(7) . . ?
F17 C41 C40 121.8(8) . . ?
F17 C41 C42 119.7(7) . . ?
C40 C41 C42 118.5(7) . . ?
F18 C42 C43 119.2(8) . . ?
F18 C42 C41 119.0(8) . . ?
C43 C42 C41 121.8(6) . . ?
F19 C43 C42 121.3(6) . . ?
F19 C43 C44 121.3(7) . . ?
C42 C43 C44 117.4(7) . . ?
C43 C44 F20 116.5(6) . . ?
C43 C44 C39 125.0(6) . . ?
F20 C44 C39 118.5(5) . . ?
C46 C45 C50 114.0(6) . . ?
C46 C45 Al2 121.3(5) . . ?
C50 C45 Al2 124.0(4) . . ?
C47 C46 C45 124.7(7) . . ?
C47 C46 F21 117.5(6) . . ?
C45 C46 F21 117.8(6) . . ?
C46 C47 C48 118.1(7) . . ?
C46 C47 F22 120.6(8) . . ?
C48 C47 F22 121.3(8) . . ?
C47 C48 C49 121.3(6) . . ?
C47 C48 F23 120.1(8) . . ?
C49 C48 F23 118.5(8) . . ?
F24 C49 C50 122.7(7) . . ?
F24 C49 C48 119.4(6) . . ?
C50 C49 C48 117.8(7) . . ?
F25 C50 C49 115.8(6) . . ?
F25 C50 C45 120.2(5) . . ?
C49 C50 C45 124.0(6) . . ?
C52 C51 C56 115.3(6) . . ?
C52 C51 Al2 127.7(5) . . ?
C56 C51 Al2 117.0(4) . . ?
C51 C52 F26 118.8(6) . . ?
C51 C52 C53 123.9(7) . . ?
F26 C52 C53 117.2(6) . . ?
F27 C53 C54 123.2(7) . . ?
F27 C53 C52 118.6(8) . . ?
C54 C53 C52 118.2(6) . . ?
C55 C54 C53 121.4(7) . . ?
C55 C54 F28 118.6(8) . . ?
C53 C54 F28 120.0(7) . . ?
C54 C55 F29 121.2(6) . . ?
C54 C55 C56 119.1(7) . . ?
F29 C55 C56 119.7(7) . . ?
F30 C56 C55 117.5(6) . . ?
F30 C56 C51 120.4(5) . . ?
C55 C56 C51 122.0(6) . . ?
C58 C57 C57 119.7(6) . 3 ?
C58 C57 H57 120.2 . . ?
C57 C57 H57 120.2 3 . ?
C57 C58 C59 119.5(10) . . ?
C57 C58 H58 120.3 . . ?
C59 C58 H58 120.3 . . ?
C59 C59 C58 120.7(6) 3 . ?
C59 C59 H59 119.6 3 . ?
C58 C59 H59 119.6 . . ?
C3 B1 C17 125.8(6) . . ?
C3 B1 C13 122.3(6) . . ?
C17 B1 C13 110.2(6) . . ?



