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

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

data_R-1
_database_code_depnum_ccdc_archive 'CCDC 2058920'
loop_
_audit_author_name
_audit_author_address
'Daniel Unruh'
;Texas Tech University
United States of America
;
_audit_update_record             
;
2021-02-01 deposited with the CCDC.	2021-03-23 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT089_R-1                 
;
PROBLEM: Poor Data / Parameter Ratio (Zmax < 18) ........       6.65 Note  
RESPONSE: Due to the disorder within the structure and the weak diffracting 
          nature of the crystals. Multiple attempts were made to produce 
          larger crystals, but were ultimately unsuccessful.
;
_vrf_PLAT340_R-1                 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.00531 Ang.  
RESPONSE: Due to the weak nature of the high angle data and the disordered
          interstitial THF molecule in the structure.
;
# end Validation Reply Form

_audit_creation_date             2021-01-20
_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         'C30 H20 B F5 O3, C4 H8 O'
_chemical_formula_sum            'C34 H28 B F5 O4'
_chemical_formula_weight         606.37
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C136  H108  B4  F20  O16  '
_chemical_oxdiff_usercomment     "Nick's structure"
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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   8.6846(2)
_cell_length_b                   11.2757(3)
_cell_length_c                   28.9903(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2838.87(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6412
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      75.3980
_cell_measurement_theta_min      3.0140
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.961
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.657
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (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_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1256
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 -2 0.0118
0 1 2 0.0058
-6 -1 3 0.0988
5 0 -5 0.1071
0 -6 9 0.0084
0 7 -7 0.0135
1 -5 14 0.0207
0 -7 6 0.0120
0 1 19 0.0053
3 -5 -8 0.0629
0 4 -16 0.0093

_exptl_crystal_size_max          0.213
_exptl_crystal_size_mid          0.019
_exptl_crystal_size_min          0.018
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0000 -1.0000 -2.0000 0.0214 0.0616 0.1604
-0.0000 1.0000 2.0000 -0.0214 -0.0616 -0.1604
-5.5232 -0.6037 3.4555 -0.2202 -0.9178 0.3304
5.4601 -0.0959 -4.6923 0.2275 0.9490 -0.2183
0.0666 -6.3849 9.1961 -0.8658 0.2079 0.4552
0.2206 6.7437 -7.2733 0.8041 -0.1932 -0.5622
0.9041 -4.7470 14.0043 -0.9677 0.2318 0.0995
-0.4191 -6.9326 5.8637 -0.7537 0.1813 0.6317
-0.0931 1.1063 18.5977 -0.7718 -0.2299 -0.5928
3.4686 -4.9198 -7.7493 0.0225 0.8578 0.5135
-0.0368 3.7504 -16.1613 0.9996 -0.0256 0.0091

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1073
_diffrn_reflns_av_unetI/netI     0.0764
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            25818
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.196
_diffrn_reflns_theta_min         3.049
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -24.00  27.00   0.50   12.00    --  -48.35  19.00  60.00  102
  2  ω    -53.00 -14.00   0.50   30.00    --  -86.25  49.00  41.00   78
  3  ω    -49.00 -14.00   0.50   30.00    --  -86.25  45.00  90.00   70
  4  ω   -120.00 -35.00   0.50   12.00    --  -48.35 -49.00-105.00  170
  5  ω   -120.00 -73.00   0.50   12.00    --  -48.35-125.00-120.00   94
  6  ω   -120.00 -73.00   0.50   12.00    --  -48.35-125.00 -90.00   94
  7  ω   -120.00 -73.00   0.50   12.00    --  -48.35-125.00  30.00   94
  8  ω   -120.00 -33.00   0.50   12.00    --  -48.35 -57.00  30.00  174
  9  ω   -120.00 -33.00   0.50   12.00    --  -48.35 -57.00 120.00  174
 10  ω   -159.00 -83.00   0.50   30.00    --  -86.25 -95.00  33.00  152
 11  ω    101.00 178.00   0.50   30.00    --  107.75  83.00-108.00  154
 12  ω     95.00 178.00   0.50   30.00    --  107.75  49.00  41.00  166
 13  ω     95.00 178.00   0.50   30.00    --  107.75 125.00 -60.00  166
 14  ω     95.00 178.00   0.50   30.00    --  107.75  45.00-150.00  166
 15  ω     35.00  73.00   0.50   30.00    --  107.75 -61.00-150.00   76
 16  ω     35.00 106.00   0.50   30.00    --  107.75 -94.00-120.00  142
 17  ω     35.00 106.00   0.50   30.00    --  107.75 -94.00   0.00  142
 18  ω     35.00  73.00   0.50   30.00    --  107.75 -61.00 120.00   76
 19  ω     35.00 105.00   0.50   30.00    --  107.75 -95.00  33.00  140
 20  ω     35.00  73.00   0.50   30.00    --  107.75 -61.00  30.00   76
 21  ω     35.00  73.00   0.50   30.00    --  107.75 -61.00 150.00   76
 22  ω     35.00  73.00   0.50   30.00    --  107.75 -61.00-120.00   76
 23  ω     35.00  49.50   0.50   30.00    --  107.75 -61.00-180.00   29
;
_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      0.0036716000
_diffrn_orient_matrix_UB_12      0.0698974000
_diffrn_orient_matrix_UB_13      -0.0456416000
_diffrn_orient_matrix_UB_21      0.1653549000
_diffrn_orient_matrix_UB_22      -0.0437012000
_diffrn_orient_matrix_UB_23      -0.0089356000
_diffrn_orient_matrix_UB_31      -0.0639981000
_diffrn_orient_matrix_UB_32      -0.1089959000
_diffrn_orient_matrix_UB_33      -0.0257107000
_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         0.749
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3966
_reflns_number_total             5188
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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         0.280
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.20(19)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         5188
_refine_ls_number_restraints     226
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0437
_refine_ls_restrained_S_all      0.984
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0445P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.1009
_refine_special_details          
'The interstitial tetrahydrofurn molecule (O4, C31 < C34) was positionally disordered and modeled as split sites (A and B). The refined site occupancies for the A and B sites were 0.16 and 0.84, respectively. To help maintain reasonable ADP values and bond lengths, SIMU, RIGU, and free variable DFIX restraints were applied to the disordered molecule.'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.80(19)
 0.20(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 C31A-C32A = C32A-C33A = C33A-C34A = C31B-C32B = C32B-C33B = C33B-C34B
 1.48317 with sigma of 0.02
 O4A-C31A = O4A-C34A = O4B-C31B = O4B-C34B
 1.44031 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O4B \\sim C31B \\sim C32B \\sim C33B \\sim C34B \\sim O4A \\sim C31A \\sim C32A
\\sim C33A \\sim C34A: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 2A
5. Rigid body (RIGU) restrains
 O4B, C31B, C32B, C33B, C34B, O4A, C31A, C32A, C33A, C34A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(O4B)=Sof(C31B)=Sof(H31C)=Sof(H31D)=Sof(C32B)=Sof(H32C)=Sof(H32D)=
 Sof(C33B)=Sof(H33C)=Sof(H33D)=Sof(C34B)=Sof(H34C)=Sof(H34D)=1-FVAR(3)
 Sof(O4A)=Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(C32A)=Sof(H32A)=Sof(H32B)=
 Sof(C33A)=Sof(H33A)=Sof(H33B)=Sof(C34A)=Sof(H34A)=Sof(H34B)=FVAR(3)
7.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31A(H31A,
 H31B), C32A(H32A,H32B), C33A(H33A,H33B), C34A(H34A,H34B), C31B(H31C,H31D),
 C32B(H32C,H32D), C33B(H33C,H33D), C34B(H34C,H34D)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C13(H13), C14(H14), C15(H15),
 C16(H16), C18(H18), C19(H19)
;
_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
F1 F 0.6567(3) 0.3237(2) 0.03094(7) 0.0352(5) Uani 1 1 d . . . . .
F2 F 0.4978(3) 0.3921(2) -0.04213(7) 0.0425(6) Uani 1 1 d . . . . .
F3 F 0.5425(3) 0.6087(2) -0.08011(7) 0.0463(7) Uani 1 1 d . . . . .
F4 F 0.7516(3) 0.7608(2) -0.04162(8) 0.0533(8) Uani 1 1 d . . . . .
F5 F 0.9094(3) 0.6959(2) 0.03284(8) 0.0439(6) Uani 1 1 d . . . . .
O1 O 0.8731(3) 0.5698(2) 0.11838(7) 0.0237(6) Uani 1 1 d . . . . .
O2 O 0.8495(3) 0.3606(2) 0.09972(7) 0.0237(6) Uani 1 1 d . . . . .
O3 O 1.0630(3) 0.4851(2) 0.07086(8) 0.0272(6) Uani 1 1 d . . . . .
C1 C 0.7390(4) 0.5704(3) 0.14330(11) 0.0221(8) Uani 1 1 d . . . . .
C2 C 0.6396(5) 0.6685(3) 0.13802(11) 0.0254(8) Uani 1 1 d . . . . .
H2 H 0.664706 0.728301 0.117233 0.030 Uiso 1 1 calc R U . . .
C3 C 0.5079(5) 0.6766(3) 0.16290(12) 0.0268(8) Uani 1 1 d . . . . .
H3 H 0.446535 0.743907 0.160406 0.032 Uiso 1 1 calc R U . . .
C4 C 0.4626(4) 0.5824(3) 0.19291(11) 0.0254(8) Uani 1 1 d . . . . .
C5 C 0.3213(5) 0.5852(4) 0.21703(12) 0.0295(9) Uani 1 1 d . . . . .
H5 H 0.259058 0.652123 0.214932 0.035 Uiso 1 1 calc R U . . .
C6 C 0.2742(5) 0.4916(4) 0.24337(13) 0.0329(9) Uani 1 1 d . . . . .
H6 H 0.180837 0.494534 0.259053 0.039 Uiso 1 1 calc R U . . .
C7 C 0.3691(5) 0.3901(4) 0.24650(12) 0.0287(9) Uani 1 1 d . . . . .
H7 H 0.336178 0.325388 0.263785 0.034 Uiso 1 1 calc R U . . .
C8 C 0.5079(5) 0.3853(3) 0.22466(11) 0.0258(8) Uani 1 1 d . . . . .
H8 H 0.568533 0.317753 0.227615 0.031 Uiso 1 1 calc R U . . .
C9 C 0.5616(4) 0.4817(3) 0.19743(11) 0.0224(8) Uani 1 1 d . . . . .
C10 C 0.7073(4) 0.4805(3) 0.17420(11) 0.0212(8) Uani 1 1 d . . . . .
C11 C 0.8233(4) 0.3857(3) 0.18161(11) 0.0204(7) Uani 1 1 d . . . . .
C12 C 0.8778(4) 0.3536(3) 0.22724(11) 0.0202(8) Uani 1 1 d . . . . .
C13 C 0.8304(4) 0.4143(3) 0.26768(11) 0.0215(8) Uani 1 1 d . . . . .
H13 H 0.760463 0.476467 0.265182 0.026 Uiso 1 1 calc R U . . .
C14 C 0.8854(4) 0.3834(3) 0.31040(12) 0.0245(8) Uani 1 1 d . . . . .
H14 H 0.853179 0.425061 0.336364 0.029 Uiso 1 1 calc R U . . .
C15 C 0.9901(4) 0.2892(3) 0.31509(11) 0.0240(8) Uani 1 1 d . . . . .
H15 H 1.025295 0.267282 0.344165 0.029 Uiso 1 1 calc R U . . .
C16 C 1.0399(4) 0.2298(3) 0.27691(11) 0.0226(8) Uani 1 1 d . . . . .
H16 H 1.110333 0.168236 0.280217 0.027 Uiso 1 1 calc R U . . .
C17 C 0.9861(4) 0.2605(3) 0.23212(11) 0.0210(8) Uani 1 1 d . . . . .
C18 C 1.0407(4) 0.2017(3) 0.19244(12) 0.0254(8) Uani 1 1 d . . . . .
H18 H 1.108736 0.138491 0.195521 0.030 Uiso 1 1 calc R U . . .
C19 C 0.9947(5) 0.2368(3) 0.14949(11) 0.0252(8) Uani 1 1 d . . . . .
H19 H 1.033501 0.198507 0.123570 0.030 Uiso 1 1 calc R U . . .
C20 C 0.8898(4) 0.3297(3) 0.14415(11) 0.0219(8) Uani 1 1 d . . . . .
C21 C 0.7922(4) 0.5075(3) 0.03646(11) 0.0232(8) Uani 1 1 d . . . . .
C22 C 0.6853(5) 0.4343(3) 0.01512(12) 0.0263(9) Uani 1 1 d . . . . .
C23 C 0.6010(5) 0.4667(4) -0.02362(12) 0.0293(9) Uani 1 1 d . . . . .
C24 C 0.6217(5) 0.5775(4) -0.04257(12) 0.0312(9) Uani 1 1 d . . . . .
C25 C 0.7262(5) 0.6528(4) -0.02294(13) 0.0348(10) Uani 1 1 d . . . . .
C26 C 0.8076(5) 0.6182(4) 0.01554(12) 0.0304(9) Uani 1 1 d . . . . .
C27 C 1.1816(5) 0.5090(4) 0.10648(12) 0.0288(9) Uani 1 1 d . . . . .
H27A H 1.157830 0.468010 0.135017 0.035 Uiso 1 1 calc R U . . .
H27B H 1.190036 0.593336 0.112655 0.035 Uiso 1 1 calc R U . . .
C28 C 1.3280(5) 0.4615(4) 0.08510(14) 0.0343(9) Uani 1 1 d . . . . .
H28A H 1.401364 0.437872 0.108602 0.041 Uiso 1 1 calc R U . . .
H28B H 1.375490 0.519956 0.065092 0.041 Uiso 1 1 calc R U . . .
C29 C 1.2713(5) 0.3545(4) 0.05759(14) 0.0356(10) Uani 1 1 d . . . . .
H29A H 1.344280 0.332702 0.033717 0.043 Uiso 1 1 calc R U . . .
H29B H 1.253720 0.286735 0.077511 0.043 Uiso 1 1 calc R U . . .
C30 C 1.1228(5) 0.3990(4) 0.03709(12) 0.0338(9) Uani 1 1 d . . . . .
H30A H 1.141170 0.436839 0.007556 0.041 Uiso 1 1 calc R U . . .
H30B H 1.050654 0.334265 0.032750 0.041 Uiso 1 1 calc R U . . .
B1 B 0.8843(5) 0.4774(4) 0.08409(13) 0.0232(9) Uani 1 1 d . . . . .
O4A O 0.3636(10) 0.0534(8) 0.1189(3) 0.068(2) Uani 0.835(9) 1 d D U P A 2
C31A C 0.4333(8) 0.1231(9) 0.1553(2) 0.0617(19) Uani 0.835(9) 1 d D U P A 2
H31A H 0.424427 0.082566 0.184689 0.074 Uiso 0.835(9) 1 calc R U P A 2
H31B H 0.383383 0.199850 0.157762 0.074 Uiso 0.835(9) 1 calc R U P A 2
C32A C 0.5947(7) 0.1372(6) 0.14247(19) 0.0456(15) Uani 0.835(9) 1 d D U P A 2
H32A H 0.659691 0.145136 0.169508 0.055 Uiso 0.835(9) 1 calc R U P A 2
H32B H 0.609340 0.205582 0.122660 0.055 Uiso 0.835(9) 1 calc R U P A 2
C33A C 0.6283(9) 0.0211(8) 0.1166(3) 0.072(2) Uani 0.835(9) 1 d D U P A 2
H33A H 0.709092 0.031586 0.093842 0.086 Uiso 0.835(9) 1 calc R U P A 2
H33B H 0.657259 -0.041900 0.137652 0.086 Uiso 0.835(9) 1 calc R U P A 2
C34A C 0.4780(9) -0.0037(8) 0.0943(3) 0.0647(18) Uani 0.835(9) 1 d D U P A 2
H34A H 0.479106 0.024419 0.062713 0.078 Uiso 0.835(9) 1 calc R U P A 2
H34B H 0.458901 -0.088477 0.093994 0.078 Uiso 0.835(9) 1 calc R U P A 2
O4B O 0.366(5) 0.084(5) 0.1204(13) 0.065(5) Uani 0.165(9) 1 d D U P A 1
C31B C 0.471(4) 0.060(4) 0.1594(12) 0.065(5) Uani 0.165(9) 1 d D U P A 1
H31C H 0.436535 -0.012509 0.174445 0.079 Uiso 0.165(9) 1 calc R U P A 1
H31D H 0.461631 0.123560 0.181527 0.079 Uiso 0.165(9) 1 calc R U P A 1
C32B C 0.636(4) 0.045(4) 0.1477(11) 0.069(5) Uani 0.165(9) 1 d D U P A 1
H32C H 0.699880 0.097246 0.166354 0.083 Uiso 0.165(9) 1 calc R U P A 1
H32D H 0.669425 -0.035866 0.151951 0.083 Uiso 0.165(9) 1 calc R U P A 1
C33B C 0.642(4) 0.080(4) 0.0988(10) 0.062(5) Uani 0.165(9) 1 d D U P A 1
H33C H 0.709490 0.027595 0.081433 0.075 Uiso 0.165(9) 1 calc R U P A 1
H33D H 0.676387 0.160941 0.095159 0.075 Uiso 0.165(9) 1 calc R U P A 1
C34B C 0.481(4) 0.066(4) 0.0846(12) 0.065(5) Uani 0.165(9) 1 d D U P A 1
H34C H 0.460114 0.120605 0.059616 0.078 Uiso 0.165(9) 1 calc R U P A 1
H34D H 0.467328 -0.013990 0.072426 0.078 Uiso 0.165(9) 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
F1 C22 1.351(5) . ?
F2 C23 1.342(5) . ?
F3 C24 1.335(4) . ?
F4 C25 1.351(5) . ?
F5 C26 1.342(5) . ?
O1 C1 1.370(4) . ?
O1 B1 1.444(5) . ?
O2 C20 1.379(4) . ?
O2 B1 1.425(5) . ?
O3 C27 1.483(4) . ?
O3 C30 1.473(5) . ?
O3 B1 1.601(5) . ?
C1 C2 1.412(5) . ?
C1 C10 1.381(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.355(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.428(6) . ?
C4 C5 1.413(5) . ?
C4 C9 1.430(5) . ?
C5 H5 0.9300 . ?
C5 C6 1.366(6) . ?
C6 H6 0.9300 . ?
C6 C7 1.413(6) . ?
C7 H7 0.9300 . ?
C7 C8 1.363(6) . ?
C8 H8 0.9300 . ?
C8 C9 1.423(5) . ?
C9 C10 1.433(5) . ?
C10 C11 1.484(5) . ?
C11 C12 1.451(5) . ?
C11 C20 1.383(5) . ?
C12 C13 1.419(5) . ?
C12 C17 1.417(5) . ?
C13 H13 0.9300 . ?
C13 C14 1.372(5) . ?
C14 H14 0.9300 . ?
C14 C15 1.406(5) . ?
C15 H15 0.9300 . ?
C15 C16 1.364(5) . ?
C16 H16 0.9300 . ?
C16 C17 1.423(5) . ?
C17 C18 1.410(5) . ?
C18 H18 0.9300 . ?
C18 C19 1.367(5) . ?
C19 H19 0.9300 . ?
C19 C20 1.396(5) . ?
C21 C22 1.387(6) . ?
C21 C26 1.395(6) . ?
C21 B1 1.632(5) . ?
C22 C23 1.390(5) . ?
C23 C24 1.376(6) . ?
C24 C25 1.367(6) . ?
C25 C26 1.377(5) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.513(6) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C29 1.528(6) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C30 1.506(6) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
O4A C31A 1.449(10) . ?
O4A C34A 1.382(10) . ?
C31A H31A 0.9700 . ?
C31A H31B 0.9700 . ?
C31A C32A 1.459(8) . ?
C32A H32A 0.9700 . ?
C32A H32B 0.9700 . ?
C32A C33A 1.537(9) . ?
C33A H33A 0.9700 . ?
C33A H33B 0.9700 . ?
C33A C34A 1.482(10) . ?
C34A H34A 0.9700 . ?
C34A H34B 0.9700 . ?
O4B C31B 1.48(3) . ?
O4B C34B 1.45(3) . ?
C31B H31C 0.9700 . ?
C31B H31D 0.9700 . ?
C31B C32B 1.48(3) . ?
C32B H32C 0.9700 . ?
C32B H32D 0.9700 . ?
C32B C33B 1.47(3) . ?
C33B H33C 0.9700 . ?
C33B H33D 0.9700 . ?
C33B C34B 1.47(3) . ?
C34B H34C 0.9700 . ?
C34B H34D 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O1 B1 115.1(3) . . ?
C20 O2 B1 118.4(3) . . ?
C27 O3 B1 121.1(3) . . ?
C30 O3 C27 109.7(3) . . ?
C30 O3 B1 117.7(3) . . ?
O1 C1 C2 117.8(3) . . ?
O1 C1 C10 120.6(3) . . ?
C10 C1 C2 121.6(3) . . ?
C1 C2 H2 119.6 . . ?
C3 C2 C1 120.7(3) . . ?
C3 C2 H2 119.6 . . ?
C2 C3 H3 119.8 . . ?
C2 C3 C4 120.4(4) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 C9 118.7(3) . . ?
C5 C4 C3 121.6(4) . . ?
C5 C4 C9 119.6(3) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 C4 121.3(4) . . ?
C6 C5 H5 119.3 . . ?
C5 C6 H6 120.4 . . ?
C5 C6 C7 119.2(4) . . ?
C7 C6 H6 120.4 . . ?
C6 C7 H7 119.4 . . ?
C8 C7 C6 121.2(4) . . ?
C8 C7 H7 119.4 . . ?
C7 C8 H8 119.4 . . ?
C7 C8 C9 121.2(4) . . ?
C9 C8 H8 119.4 . . ?
C4 C9 C10 119.7(3) . . ?
C8 C9 C4 117.4(3) . . ?
C8 C9 C10 122.9(3) . . ?
C1 C10 C9 118.3(3) . . ?
C1 C10 C11 119.1(3) . . ?
C9 C10 C11 122.6(3) . . ?
C12 C11 C10 122.2(3) . . ?
C20 C11 C10 119.9(3) . . ?
C20 C11 C12 117.8(3) . . ?
C13 C12 C11 122.6(3) . . ?
C17 C12 C11 119.5(3) . . ?
C17 C12 C13 117.9(3) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 C12 121.5(3) . . ?
C14 C13 H13 119.3 . . ?
C13 C14 H14 119.9 . . ?
C13 C14 C15 120.3(3) . . ?
C15 C14 H14 119.9 . . ?
C14 C15 H15 120.1 . . ?
C16 C15 C14 119.9(3) . . ?
C16 C15 H15 120.1 . . ?
C15 C16 H16 119.4 . . ?
C15 C16 C17 121.1(3) . . ?
C17 C16 H16 119.4 . . ?
C12 C17 C16 119.3(3) . . ?
C18 C17 C12 119.4(3) . . ?
C18 C17 C16 121.3(3) . . ?
C17 C18 H18 119.7 . . ?
C19 C18 C17 120.6(3) . . ?
C19 C18 H18 119.7 . . ?
C18 C19 H19 119.7 . . ?
C18 C19 C20 120.6(3) . . ?
C20 C19 H19 119.7 . . ?
O2 C20 C11 120.8(3) . . ?
O2 C20 C19 117.3(3) . . ?
C11 C20 C19 121.9(3) . . ?
C22 C21 C26 113.8(3) . . ?
C22 C21 B1 125.6(3) . . ?
C26 C21 B1 120.5(3) . . ?
F1 C22 C21 121.4(3) . . ?
F1 C22 C23 114.8(3) . . ?
C21 C22 C23 123.8(4) . . ?
F2 C23 C22 120.7(4) . . ?
F2 C23 C24 119.8(3) . . ?
C24 C23 C22 119.5(4) . . ?
F3 C24 C23 119.8(4) . . ?
F3 C24 C25 121.2(4) . . ?
C25 C24 C23 119.0(3) . . ?
F4 C25 C24 120.1(3) . . ?
F4 C25 C26 119.7(4) . . ?
C24 C25 C26 120.1(4) . . ?
F5 C26 C21 119.0(3) . . ?
F5 C26 C25 117.1(4) . . ?
C25 C26 C21 123.8(4) . . ?
O3 C27 H27A 111.1 . . ?
O3 C27 H27B 111.1 . . ?
O3 C27 C28 103.5(3) . . ?
H27A C27 H27B 109.0 . . ?
C28 C27 H27A 111.1 . . ?
C28 C27 H27B 111.1 . . ?
C27 C28 H28A 111.2 . . ?
C27 C28 H28B 111.2 . . ?
C27 C28 C29 102.9(3) . . ?
H28A C28 H28B 109.1 . . ?
C29 C28 H28A 111.2 . . ?
C29 C28 H28B 111.2 . . ?
C28 C29 H29A 111.2 . . ?
C28 C29 H29B 111.2 . . ?
H29A C29 H29B 109.1 . . ?
C30 C29 C28 102.7(3) . . ?
C30 C29 H29A 111.2 . . ?
C30 C29 H29B 111.2 . . ?
O3 C30 C29 105.0(3) . . ?
O3 C30 H30A 110.7 . . ?
O3 C30 H30B 110.7 . . ?
C29 C30 H30A 110.7 . . ?
C29 C30 H30B 110.7 . . ?
H30A C30 H30B 108.8 . . ?
O1 B1 O3 101.0(3) . . ?
O1 B1 C21 113.5(3) . . ?
O2 B1 O1 115.7(3) . . ?
O2 B1 O3 109.4(3) . . ?
O2 B1 C21 110.9(3) . . ?
O3 B1 C21 105.1(3) . . ?
C34A O4A C31A 109.1(7) . . ?
O4A C31A H31A 110.5 . . ?
O4A C31A H31B 110.5 . . ?
O4A C31A C32A 105.9(6) . . ?
H31A C31A H31B 108.7 . . ?
C32A C31A H31A 110.5 . . ?
C32A C31A H31B 110.5 . . ?
C31A C32A H32A 111.3 . . ?
C31A C32A H32B 111.3 . . ?
C31A C32A C33A 102.4(6) . . ?
H32A C32A H32B 109.2 . . ?
C33A C32A H32A 111.3 . . ?
C33A C32A H32B 111.3 . . ?
C32A C33A H33A 111.4 . . ?
C32A C33A H33B 111.4 . . ?
H33A C33A H33B 109.3 . . ?
C34A C33A C32A 101.9(6) . . ?
C34A C33A H33A 111.4 . . ?
C34A C33A H33B 111.4 . . ?
O4A C34A C33A 108.7(6) . . ?
O4A C34A H34A 109.9 . . ?
O4A C34A H34B 109.9 . . ?
C33A C34A H34A 109.9 . . ?
C33A C34A H34B 109.9 . . ?
H34A C34A H34B 108.3 . . ?
C34B O4B C31B 96(3) . . ?
O4B C31B H31C 108.2 . . ?
O4B C31B H31D 108.2 . . ?
O4B C31B C32B 116(3) . . ?
H31C C31B H31D 107.4 . . ?
C32B C31B H31C 108.2 . . ?
C32B C31B H31D 108.2 . . ?
C31B C32B H32C 111.1 . . ?
C31B C32B H32D 111.1 . . ?
H32C C32B H32D 109.1 . . ?
C33B C32B C31B 103(3) . . ?
C33B C32B H32C 111.1 . . ?
C33B C32B H32D 111.1 . . ?
C32B C33B H33C 111.4 . . ?
C32B C33B H33D 111.4 . . ?
C32B C33B C34B 102(3) . . ?
H33C C33B H33D 109.2 . . ?
C34B C33B H33C 111.4 . . ?
C34B C33B H33D 111.4 . . ?
O4B C34B C33B 116(3) . . ?
O4B C34B H34C 108.3 . . ?
O4B C34B H34D 108.3 . . ?
C33B C34B H34C 108.3 . . ?
C33B C34B H34D 108.3 . . ?
H34C C34B H34D 107.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
F1 C22 C23 F2 1.4(5) . . . . ?
F1 C22 C23 C24 -179.9(3) . . . . ?
F2 C23 C24 F3 -2.1(6) . . . . ?
F2 C23 C24 C25 179.3(4) . . . . ?
F3 C24 C25 F4 -0.4(6) . . . . ?
F3 C24 C25 C26 -179.4(4) . . . . ?
F4 C25 C26 F5 0.4(6) . . . . ?
F4 C25 C26 C21 -178.2(4) . . . . ?
O1 C1 C2 C3 -177.6(3) . . . . ?
O1 C1 C10 C9 -176.5(3) . . . . ?
O1 C1 C10 C11 2.6(5) . . . . ?
O3 C27 C28 C29 -34.3(4) . . . . ?
C1 O1 B1 O2 -49.7(4) . . . . ?
C1 O1 B1 O3 -167.7(3) . . . . ?
C1 O1 B1 C21 80.3(4) . . . . ?
C1 C2 C3 C4 -3.8(5) . . . . ?
C1 C10 C11 C12 127.5(4) . . . . ?
C1 C10 C11 C20 -48.6(5) . . . . ?
C2 C1 C10 C9 6.9(5) . . . . ?
C2 C1 C10 C11 -174.0(3) . . . . ?
C2 C3 C4 C5 -176.0(3) . . . . ?
C2 C3 C4 C9 2.3(5) . . . . ?
C3 C4 C5 C6 175.8(4) . . . . ?
C3 C4 C9 C8 -175.1(3) . . . . ?
C3 C4 C9 C10 3.8(5) . . . . ?
C4 C5 C6 C7 0.0(6) . . . . ?
C4 C9 C10 C1 -8.2(5) . . . . ?
C4 C9 C10 C11 172.7(3) . . . . ?
C5 C4 C9 C8 3.2(5) . . . . ?
C5 C4 C9 C10 -178.0(3) . . . . ?
C5 C6 C7 C8 1.6(6) . . . . ?
C6 C7 C8 C9 -0.8(5) . . . . ?
C7 C8 C9 C4 -1.6(5) . . . . ?
C7 C8 C9 C10 179.6(3) . . . . ?
C8 C9 C10 C1 170.6(3) . . . . ?
C8 C9 C10 C11 -8.5(5) . . . . ?
C9 C4 C5 C6 -2.4(5) . . . . ?
C9 C10 C11 C12 -53.4(5) . . . . ?
C9 C10 C11 C20 130.4(4) . . . . ?
C10 C1 C2 C3 -0.9(5) . . . . ?
C10 C11 C12 C13 -3.3(5) . . . . ?
C10 C11 C12 C17 178.5(3) . . . . ?
C10 C11 C20 O2 -0.1(5) . . . . ?
C10 C11 C20 C19 -177.3(3) . . . . ?
C11 C12 C13 C14 -179.0(4) . . . . ?
C11 C12 C17 C16 179.6(3) . . . . ?
C11 C12 C17 C18 0.9(5) . . . . ?
C12 C11 C20 O2 -176.4(3) . . . . ?
C12 C11 C20 C19 6.4(5) . . . . ?
C12 C13 C14 C15 -0.6(6) . . . . ?
C12 C17 C18 C19 2.5(6) . . . . ?
C13 C12 C17 C16 1.4(5) . . . . ?
C13 C12 C17 C18 -177.3(3) . . . . ?
C13 C14 C15 C16 1.5(6) . . . . ?
C14 C15 C16 C17 -0.9(5) . . . . ?
C15 C16 C17 C12 -0.6(5) . . . . ?
C15 C16 C17 C18 178.1(4) . . . . ?
C16 C17 C18 C19 -176.2(4) . . . . ?
C17 C12 C13 C14 -0.9(5) . . . . ?
C17 C18 C19 C20 -1.5(6) . . . . ?
C18 C19 C20 O2 179.6(3) . . . . ?
C18 C19 C20 C11 -3.1(6) . . . . ?
C20 O2 B1 O1 -34.9(5) . . . . ?
C20 O2 B1 O3 78.4(3) . . . . ?
C20 O2 B1 C21 -166.1(3) . . . . ?
C20 C11 C12 C13 172.9(3) . . . . ?
C20 C11 C12 C17 -5.2(5) . . . . ?
C21 C22 C23 F2 -179.0(3) . . . . ?
C21 C22 C23 C24 -0.3(6) . . . . ?
C22 C21 C26 F5 -179.1(3) . . . . ?
C22 C21 C26 C25 -0.5(6) . . . . ?
C22 C21 B1 O1 -128.0(4) . . . . ?
C22 C21 B1 O2 4.3(5) . . . . ?
C22 C21 B1 O3 122.5(4) . . . . ?
C22 C23 C24 F3 179.2(3) . . . . ?
C22 C23 C24 C25 0.6(6) . . . . ?
C23 C24 C25 F4 178.2(4) . . . . ?
C23 C24 C25 C26 -0.8(6) . . . . ?
C24 C25 C26 F5 179.4(4) . . . . ?
C24 C25 C26 C21 0.8(6) . . . . ?
C26 C21 C22 F1 179.8(3) . . . . ?
C26 C21 C22 C23 0.2(5) . . . . ?
C26 C21 B1 O1 46.6(5) . . . . ?
C26 C21 B1 O2 178.9(3) . . . . ?
C26 C21 B1 O3 -62.9(4) . . . . ?
C27 O3 C30 C29 9.6(4) . . . . ?
C27 O3 B1 O1 38.0(4) . . . . ?
C27 O3 B1 O2 -84.5(4) . . . . ?
C27 O3 B1 C21 156.3(3) . . . . ?
C27 C28 C29 C30 40.3(4) . . . . ?
C28 C29 C30 O3 -30.7(4) . . . . ?
C30 O3 C27 C28 15.7(4) . . . . ?
C30 O3 B1 O1 177.6(3) . . . . ?
C30 O3 B1 O2 55.1(4) . . . . ?
C30 O3 B1 C21 -64.1(4) . . . . ?
B1 O1 C1 C2 -114.7(4) . . . . ?
B1 O1 C1 C10 68.5(4) . . . . ?
B1 O2 C20 C11 64.3(5) . . . . ?
B1 O2 C20 C19 -118.4(4) . . . . ?
B1 O3 C27 C28 158.2(3) . . . . ?
B1 O3 C30 C29 -134.3(3) . . . . ?
B1 C21 C22 F1 -5.3(5) . . . . ?
B1 C21 C22 C23 175.1(4) . . . . ?
B1 C21 C26 F5 5.7(5) . . . . ?
B1 C21 C26 C25 -175.7(4) . . . . ?
O4A C31A C32A C33A -31.9(9) . . . . ?
C31A O4A C34A C33A 4.0(11) . . . . ?
C31A C32A C33A C34A 33.2(8) . . . . ?
C32A C33A C34A O4A -23.3(10) . . . . ?
C34A O4A C31A C32A 18.4(10) . . . . ?
O4B C31B C32B C33B 8(6) . . . . ?
C31B O4B C34B C33B -23(5) . . . . ?
C31B C32B C33B C34B -20(5) . . . . ?
C32B C33B C34B O4B 30(5) . . . . ?
C34B O4B C31B C32B 8(5) . . . . ?

_olex2_date_sample_data_collection 2021-01-19
_olex2_date_sample_submission    2021-01-19
_olex2_exptl_crystal_mounting_method 'Hampton Research 20 micron nylon loop'
_olex2_submission_original_sample_id kre21_02
_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 1.889
_oxdiff_exptl_absorpt_empirical_full_min 0.439
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.80(19)
2 0.20(19)
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Tetrahydrofuran'
####################################################################### 
# 
# 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_R-9
_database_code_depnum_ccdc_archive 'CCDC 2058923'
loop_
_audit_author_name
_audit_author_address
'Daniel Unruh'
;Texas Tech University
United States of America
;
_audit_update_record             
;
2021-02-01 deposited with the CCDC.	2021-03-23 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_STRVA01_R-9                 
;
PROBLEM: Flack test results are ambiguous.
RESPONSE: The orientation of the structure was not determined from this 
          data.
;
_vrf_PLAT250_R-9                 
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.3 Note  
RESPONSE: Due to disorder about the interstitial benzene molecules.
;
_vrf_PLAT340_R-9                 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.00426 Ang.  
RESPONSE: Due to the weak diffraction quality of high angle reflections.
;
_vrf_PLAT911_R-9                 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          2 Report
RESPONSE: These reflections were omitted during the absorption correction.
;
# end Validation Reply Form

_audit_creation_date             2021-01-15
_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         'C81 H60 B2 N2 O6, 4(C6 H6)'
_chemical_formula_sum            'C105 H84 B2 N2 O6'
_chemical_formula_weight         1491.36
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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           1
_space_group_name_H-M_alt        'P 1'
_space_group_name_Hall           'P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'

_cell_length_a                   11.5215(17)
_cell_length_b                   14.608(2)
_cell_length_c                   14.677(2)
_cell_angle_alpha                62.145(2)
_cell_angle_beta                 87.982(2)
_cell_angle_gamma                66.868(2)
_cell_volume                     1974.7(5)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.96
_cell_measurement_theta_min      2.21
_shelx_estimated_absorpt_T_max   0.992
_shelx_estimated_absorpt_T_min   0.964
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.7196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0282 before and 0.0240 after correction.
The Ratio of minimum to maximum transmission is 0.9653.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             786
_exptl_crystal_size_max          0.485
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.105
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            47001
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.212
_diffrn_reflns_theta_min         1.596
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.993
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                14729
_reflns_number_total             17471
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.160
_refine_diff_density_min         -0.171
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.4(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1105
_refine_ls_number_reflns         17471
_refine_ls_number_restraints     255
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0394
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0399P)²+0.0462P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0862
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.6(8)
 0.4(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
C94A \\sim C95A \\sim C96A \\sim C97A \\sim C98A \\sim C99A \\sim C94B \\sim
C95B \\sim C96B \\sim C97B \\sim C98B \\sim C99B: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.04 within 2A
4. Rigid body (RIGU) restrains
 C94A, C95A, C96A, C97A, C98A, C99A, C94B, C95B, C96B, C97B, C98B, C99B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C98B)=Sof(H98B)=Sof(C97B)=Sof(H97B)=Sof(C96B)=Sof(H96B)=Sof(C95B)=
 Sof(H95B)=Sof(C94B)=Sof(H94B)=Sof(C99B)=Sof(H99B)=1-FVAR(1)
 Sof(C98A)=Sof(H98A)=Sof(C97A)=Sof(H97A)=Sof(C96A)=Sof(H96A)=Sof(C95A)=
 Sof(H95A)=Sof(C94A)=Sof(H94A)=Sof(C99A)=Sof(H99A)=FVAR(1)
 Sof(C106)=Sof(H106)=Sof(C107)=Sof(H107)=Sof(C108)=Sof(H108)=Sof(C109)=
 Sof(H109)=Sof(C110)=Sof(H110)=Sof(C111)=Sof(H111)=1-FVAR(2)
 Sof(C100)=Sof(H100)=Sof(C101)=Sof(H101)=Sof(C102)=Sof(H102)=Sof(C103)=
 Sof(H103)=Sof(C104)=Sof(H104)=Sof(C105)=Sof(H105)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C8(H8), C15(H15), C17(H17), C25(H25), C26(H26),
 C27(H27), C28(H28), C30(H30), C31(H31), C34(H34), C35(H35), C37(H37), C38(H38),
  C39(H39), C40(H40), C45(H45), C46(H46), C47(H47), C48(H48), C50(H50),
 C51(H51), C54(H54), C55(H55), C57(H57), C58(H58), C59(H59), C60(H60), C65(H65),
  C66(H66), C67(H67), C68(H68), C70(H70), C71(H71), C74(H74), C75(H75),
 C77(H77), C78(H78), C79(H79), C80(H80), C82(H82), C83(H83), C84(H84), C85(H85),
  C86(H86), C87(H87), C88(H88), C89(H89), C90(H90), C91(H91), C92(H92),
 C93(H93), C98A(H98A), C97A(H97A), C96A(H96A), C95A(H95A), C94A(H94A),
 C99A(H99A), C98B(H98B), C97B(H97B), C96B(H96B), C95B(H95B), C94B(H94B),
 C99B(H99B), C100(H100), C101(H101), C102(H102), C103(H103), C104(H104),
 C105(H105), C106(H106), C107(H107), C108(H108), C109(H109), C110(H110),
 C111(H111)
6.b Fitted hexagon refined as free rotating group:
 C98A(C97A,C96A,C95A,C94A,C99A), C98B(C97B,C96B,C95B,C94B,C99B), C100(C101,
 C102,C103,C104,C105), C106(C107,C108,C109,C110,C111)
6.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_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 0.69826(15) 0.34742(14) 0.54491(12) 0.0195(4) Uani 1 1 d . . . . .
O2 O 0.75978(16) 0.50128(14) 0.51276(13) 0.0197(4) Uani 1 1 d . . . . .
O3 O 0.74780(16) 0.45088(14) 0.38145(12) 0.0206(4) Uani 1 1 d . . . . .
O4 O 0.38682(15) 0.47187(14) 0.48397(13) 0.0205(4) Uani 1 1 d . . . . .
O5 O 0.39639(16) 0.64652(14) 0.43554(13) 0.0213(4) Uani 1 1 d . . . . .
O6 O 0.38750(16) 0.59520(14) 0.30710(13) 0.0220(4) Uani 1 1 d . . . . .
N1 N 1.03290(19) 0.32392(17) 0.48024(16) 0.0202(4) Uani 1 1 d . . . . .
N2 N 0.99911(19) 0.21642(17) 0.62797(15) 0.0192(4) Uani 1 1 d . . . . .
C1 C 0.9374(2) 0.3157(2) 0.53684(18) 0.0173(5) Uani 1 1 d . . . . .
C2 C 1.1496(2) 0.2317(2) 0.5355(2) 0.0263(6) Uani 1 1 d . . . . .
H2 H 1.229665 0.218979 0.512433 0.032 Uiso 1 1 calc R U . . .
C3 C 1.1282(2) 0.1642(2) 0.6274(2) 0.0265(6) Uani 1 1 d . . . . .
H3 H 1.189963 0.093735 0.682068 0.032 Uiso 1 1 calc R U . . .
C4 C 1.0327(2) 0.4194(2) 0.38308(19) 0.0204(5) Uani 1 1 d . . . . .
C5 C 1.0525(2) 0.5041(2) 0.3902(2) 0.0225(6) Uani 1 1 d . . . . .
C6 C 1.0659(2) 0.5892(2) 0.2987(2) 0.0264(6) Uani 1 1 d . . . . .
H6 H 1.077510 0.649066 0.300925 0.032 Uiso 1 1 calc R U . . .
C7 C 1.0628(2) 0.5886(2) 0.2045(2) 0.0291(6) Uani 1 1 d . . . . .
C8 C 1.0469(3) 0.5003(2) 0.2024(2) 0.0295(6) Uani 1 1 d . . . . .
H8 H 1.045491 0.499221 0.138283 0.035 Uiso 1 1 calc R U . . .
C9 C 1.0330(3) 0.4134(2) 0.2909(2) 0.0255(6) Uani 1 1 d . . . . .
C10 C 1.0633(3) 0.5032(2) 0.4924(2) 0.0270(6) Uani 1 1 d . . . . .
H10A H 1.077693 0.569214 0.481113 0.040 Uiso 1 1 calc R U . . .
H10B H 1.135455 0.432466 0.542807 0.040 Uiso 1 1 calc R U . . .
H10C H 0.983698 0.507263 0.519884 0.040 Uiso 1 1 calc R U . . .
C11 C 1.0800(3) 0.6812(3) 0.1070(2) 0.0405(8) Uani 1 1 d . . . . .
H11A H 1.137629 0.646458 0.070018 0.061 Uiso 1 1 calc R U . . .
H11B H 1.116931 0.720667 0.126987 0.061 Uiso 1 1 calc R U . . .
H11C H 0.996385 0.736236 0.060936 0.061 Uiso 1 1 calc R U . . .
C12 C 1.0215(3) 0.3168(3) 0.2859(2) 0.0355(7) Uani 1 1 d . . . . .
H12A H 0.930735 0.332594 0.275118 0.053 Uiso 1 1 calc R U . . .
H12B H 1.066770 0.245315 0.351747 0.053 Uiso 1 1 calc R U . . .
H12C H 1.059657 0.309362 0.227556 0.053 Uiso 1 1 calc R U . . .
C13 C 0.9552(2) 0.1671(2) 0.72608(19) 0.0202(5) Uani 1 1 d . . . . .
C14 C 0.9764(2) 0.1942(2) 0.80165(19) 0.0219(5) Uani 1 1 d . . . . .
C15 C 0.9475(2) 0.1376(2) 0.8995(2) 0.0250(6) Uani 1 1 d . . . . .
H15 H 0.961603 0.153671 0.952684 0.030 Uiso 1 1 calc R U . . .
C16 C 0.8982(3) 0.0576(2) 0.9216(2) 0.0274(6) Uani 1 1 d . . . . .
C17 C 0.8827(2) 0.0320(2) 0.8444(2) 0.0254(6) Uani 1 1 d . . . . .
H17 H 0.850231 -0.023145 0.859301 0.031 Uiso 1 1 calc R U . . .
C18 C 0.9127(2) 0.0840(2) 0.7459(2) 0.0221(5) Uani 1 1 d . . . . .
C19 C 1.0217(3) 0.2853(2) 0.7769(2) 0.0292(6) Uani 1 1 d . . . . .
H19A H 1.101860 0.267715 0.749751 0.044 Uiso 1 1 calc R U . . .
H19B H 1.036607 0.288070 0.840725 0.044 Uiso 1 1 calc R U . . .
H19C H 0.956273 0.359679 0.724029 0.044 Uiso 1 1 calc R U . . .
C20 C 0.8614(3) 0.0021(3) 1.0270(2) 0.0366(7) Uani 1 1 d . . . . .
H20A H 0.788614 0.060197 1.034798 0.055 Uiso 1 1 calc R U . . .
H20B H 0.934515 -0.032695 1.082739 0.055 Uiso 1 1 calc R U . . .
H20C H 0.837168 -0.057033 1.031907 0.055 Uiso 1 1 calc R U . . .
C21 C 0.9012(3) 0.0522(2) 0.6640(2) 0.0279(6) Uani 1 1 d . . . . .
H21A H 0.823434 0.111083 0.611536 0.042 Uiso 1 1 calc R U . . .
H21B H 0.896266 -0.021621 0.697154 0.042 Uiso 1 1 calc R U . . .
H21C H 0.976508 0.046591 0.629994 0.042 Uiso 1 1 calc R U . . .
C22 C 0.6491(2) 0.3283(2) 0.63457(18) 0.0175(5) Uani 1 1 d . . . . .
C23 C 0.5587(2) 0.2839(2) 0.65262(18) 0.0177(5) Uani 1 1 d . . . . .
C24 C 0.5112(2) 0.2561(2) 0.74844(19) 0.0190(5) Uani 1 1 d . . . . .
C25 C 0.4168(2) 0.2125(2) 0.7707(2) 0.0233(6) Uani 1 1 d . . . . .
H25 H 0.381420 0.203580 0.719426 0.028 Uiso 1 1 calc R U . . .
C26 C 0.3762(3) 0.1831(2) 0.8650(2) 0.0267(6) Uani 1 1 d . . . . .
H26 H 0.313481 0.153531 0.878542 0.032 Uiso 1 1 calc R U . . .
C27 C 0.4263(3) 0.1960(2) 0.9422(2) 0.0296(6) Uani 1 1 d . . . . .
H27 H 0.398361 0.174353 1.007707 0.036 Uiso 1 1 calc R U . . .
C28 C 0.5148(3) 0.2398(2) 0.9224(2) 0.0257(6) Uani 1 1 d . . . . .
H28 H 0.547457 0.249256 0.974347 0.031 Uiso 1 1 calc R U . . .
C29 C 0.5591(2) 0.2715(2) 0.82596(19) 0.0211(5) Uani 1 1 d . . . . .
C30 C 0.6472(2) 0.3212(2) 0.80227(19) 0.0205(5) Uani 1 1 d . . . . .
H30 H 0.677843 0.334074 0.852425 0.025 Uiso 1 1 calc R U . . .
C31 C 0.6894(2) 0.3510(2) 0.70888(19) 0.0194(5) Uani 1 1 d . . . . .
H31 H 0.745903 0.387125 0.693674 0.023 Uiso 1 1 calc R U . . .
C32 C 0.5062(2) 0.2728(2) 0.56925(18) 0.0176(5) Uani 1 1 d . . . . .
C33 C 0.4236(2) 0.3702(2) 0.48182(19) 0.0186(5) Uani 1 1 d . . . . .
C34 C 0.3743(2) 0.3681(2) 0.39678(19) 0.0207(5) Uani 1 1 d . . . . .
H34 H 0.317992 0.437228 0.337377 0.025 Uiso 1 1 calc R U . . .
C35 C 0.4084(2) 0.2655(2) 0.4010(2) 0.0227(6) Uani 1 1 d . . . . .
H35 H 0.376234 0.263837 0.343295 0.027 Uiso 1 1 calc R U . . .
C36 C 0.4905(2) 0.1617(2) 0.4890(2) 0.0218(5) Uani 1 1 d . . . . .
C37 C 0.5269(3) 0.0544(2) 0.4948(2) 0.0298(6) Uani 1 1 d . . . . .
H37 H 0.498009 0.051789 0.436568 0.036 Uiso 1 1 calc R U . . .
C38 C 0.6022(3) -0.0450(2) 0.5818(2) 0.0327(7) Uani 1 1 d . . . . .
H38 H 0.625888 -0.116062 0.583770 0.039 Uiso 1 1 calc R U . . .
C39 C 0.6451(3) -0.0426(2) 0.6689(2) 0.0286(6) Uani 1 1 d . . . . .
H39 H 0.695935 -0.112335 0.730223 0.034 Uiso 1 1 calc R U . . .
C40 C 0.6140(2) 0.0595(2) 0.6658(2) 0.0238(6) Uani 1 1 d . . . . .
H40 H 0.644269 0.059717 0.725054 0.029 Uiso 1 1 calc R U . . .
C41 C 0.5376(2) 0.1647(2) 0.57580(19) 0.0198(5) Uani 1 1 d . . . . .
C42 C 0.7018(2) 0.6162(2) 0.44081(19) 0.0197(5) Uani 1 1 d . . . . .
C43 C 0.5998(2) 0.6877(2) 0.46248(18) 0.0186(5) Uani 1 1 d . . . . .
C44 C 0.5452(2) 0.8084(2) 0.39180(19) 0.0194(5) Uani 1 1 d . . . . .
C45 C 0.4350(2) 0.8855(2) 0.4062(2) 0.0225(6) Uani 1 1 d . . . . .
H45 H 0.398315 0.856974 0.466471 0.027 Uiso 1 1 calc R U . . .
C46 C 0.3800(3) 1.0005(2) 0.3353(2) 0.0268(6) Uani 1 1 d . . . . .
H46 H 0.304221 1.050049 0.345318 0.032 Uiso 1 1 calc R U . . .
C47 C 0.4358(3) 1.0449(2) 0.2476(2) 0.0279(6) Uani 1 1 d . . . . .
H47 H 0.398634 1.124763 0.199355 0.034 Uiso 1 1 calc R U . . .
C48 C 0.5430(3) 0.9738(2) 0.2317(2) 0.0267(6) Uani 1 1 d . . . . .
H48 H 0.580942 1.004868 0.172977 0.032 Uiso 1 1 calc R U . . .
C49 C 0.5990(2) 0.8536(2) 0.30179(19) 0.0214(5) Uani 1 1 d . . . . .
C50 C 0.7020(2) 0.7769(2) 0.2819(2) 0.0229(6) Uani 1 1 d . . . . .
H50 H 0.738336 0.805850 0.221501 0.027 Uiso 1 1 calc R U . . .
C51 C 0.7504(2) 0.6617(2) 0.34811(19) 0.0209(5) Uani 1 1 d . . . . .
H51 H 0.817618 0.611357 0.331751 0.025 Uiso 1 1 calc R U . . .
C52 C 0.5363(2) 0.6420(2) 0.55210(19) 0.0193(5) Uani 1 1 d . . . . .
C53 C 0.4343(2) 0.6216(2) 0.53679(18) 0.0198(5) Uani 1 1 d . . . . .
C54 C 0.3627(2) 0.5869(2) 0.6152(2) 0.0224(5) Uani 1 1 d . . . . .
H54 H 0.292356 0.573768 0.601730 0.027 Uiso 1 1 calc R U . . .
C55 C 0.3958(3) 0.5724(2) 0.7111(2) 0.0250(6) Uani 1 1 d . . . . .
H55 H 0.347143 0.549901 0.764130 0.030 Uiso 1 1 calc R U . . .
C56 C 0.5012(3) 0.5904(2) 0.73293(19) 0.0237(6) Uani 1 1 d . . . . .
C57 C 0.5375(3) 0.5753(2) 0.8319(2) 0.0306(6) Uani 1 1 d . . . . .
H57 H 0.489455 0.552976 0.885530 0.037 Uiso 1 1 calc R U . . .
C58 C 0.6398(3) 0.5920(2) 0.8517(2) 0.0340(7) Uani 1 1 d . . . . .
H58 H 0.662136 0.582048 0.918444 0.041 Uiso 1 1 calc R U . . .
C59 C 0.7124(3) 0.6241(2) 0.7735(2) 0.0348(7) Uani 1 1 d . . . . .
H59 H 0.784376 0.634672 0.788108 0.042 Uiso 1 1 calc R U . . .
C60 C 0.6802(3) 0.6402(2) 0.6765(2) 0.0265(6) Uani 1 1 d . . . . .
H60 H 0.730146 0.661893 0.624354 0.032 Uiso 1 1 calc R U . . .
C61 C 0.5728(2) 0.6249(2) 0.65293(19) 0.0208(5) Uani 1 1 d . . . . .
C62 C 0.6966(2) 0.4098(2) 0.33552(18) 0.0190(5) Uani 1 1 d . . . . .
C63 C 0.6028(2) 0.4861(2) 0.24683(18) 0.0182(5) Uani 1 1 d . . . . .
C64 C 0.5497(2) 0.4450(2) 0.19554(19) 0.0201(5) Uani 1 1 d . . . . .
C65 C 0.4480(2) 0.5203(2) 0.1075(2) 0.0239(6) Uani 1 1 d . . . . .
H65 H 0.416961 0.600643 0.078787 0.029 Uiso 1 1 calc R U . . .
C66 C 0.3942(3) 0.4780(2) 0.0634(2) 0.0278(6) Uani 1 1 d . . . . .
H66 H 0.324894 0.529337 0.005588 0.033 Uiso 1 1 calc R U . . .
C67 C 0.4406(3) 0.3596(3) 0.1030(2) 0.0306(6) Uani 1 1 d . . . . .
H67 H 0.402684 0.331282 0.072020 0.037 Uiso 1 1 calc R U . . .
C68 C 0.5400(3) 0.2853(2) 0.1860(2) 0.0262(6) Uani 1 1 d . . . . .
H68 H 0.571982 0.205372 0.211434 0.031 Uiso 1 1 calc R U . . .
C69 C 0.5963(2) 0.3257(2) 0.2347(2) 0.0218(5) Uani 1 1 d . . . . .
C70 C 0.6949(2) 0.2502(2) 0.3244(2) 0.0230(6) Uani 1 1 d . . . . .
H70 H 0.727749 0.170020 0.350831 0.028 Uiso 1 1 calc R U . . .
C71 C 0.7434(2) 0.2900(2) 0.37359(19) 0.0218(5) Uani 1 1 d . . . . .
H71 H 0.809107 0.237524 0.433936 0.026 Uiso 1 1 calc R U . . .
C72 C 0.5485(2) 0.6122(2) 0.20571(18) 0.0193(5) Uani 1 1 d . . . . .
C73 C 0.4411(2) 0.6645(2) 0.23711(19) 0.0213(5) Uani 1 1 d . . . . .
C74 C 0.3811(3) 0.7837(2) 0.1968(2) 0.0261(6) Uani 1 1 d . . . . .
H74 H 0.307244 0.817191 0.220935 0.031 Uiso 1 1 calc R U . . .
C75 C 0.4307(3) 0.8506(2) 0.1226(2) 0.0291(6) Uani 1 1 d . . . . .
H75 H 0.390373 0.931136 0.094891 0.035 Uiso 1 1 calc R U . . .
C76 C 0.5407(3) 0.8019(2) 0.0864(2) 0.0256(6) Uani 1 1 d . . . . .
C77 C 0.5930(3) 0.8697(2) 0.0091(2) 0.0314(7) Uani 1 1 d . . . . .
H77 H 0.555009 0.950175 -0.018201 0.038 Uiso 1 1 calc R U . . .
C78 C 0.6974(3) 0.8209(3) -0.0266(2) 0.0365(7) Uani 1 1 d . . . . .
H78 H 0.730854 0.867767 -0.079024 0.044 Uiso 1 1 calc R U . . .
C79 C 0.7557(3) 0.7022(3) 0.0134(2) 0.0346(7) Uani 1 1 d . . . . .
H79 H 0.827913 0.669206 -0.012520 0.041 Uiso 1 1 calc R U . . .
C80 C 0.7093(3) 0.6336(2) 0.0895(2) 0.0273(6) Uani 1 1 d . . . . .
H80 H 0.750428 0.553114 0.116963 0.033 Uiso 1 1 calc R U . . .
C81 C 0.6003(2) 0.6815(2) 0.12781(19) 0.0221(5) Uani 1 1 d . . . . .
C82 C 0.1112(3) 0.8544(2) 0.4387(2) 0.0400(8) Uani 1 1 d . . . . .
H82 H 0.199988 0.837143 0.447296 0.048 Uiso 1 1 calc R U . . .
C83 C 0.0636(3) 0.8173(2) 0.3850(2) 0.0372(7) Uani 1 1 d . . . . .
H83 H 0.119868 0.773974 0.356409 0.045 Uiso 1 1 calc R U . . .
C84 C -0.0648(3) 0.8422(3) 0.3720(3) 0.0400(7) Uani 1 1 d . . . . .
H84 H -0.097115 0.816241 0.334658 0.048 Uiso 1 1 calc R U . . .
C85 C -0.1470(3) 0.9052(3) 0.4136(2) 0.0399(7) Uani 1 1 d . . . . .
H85 H -0.235833 0.922846 0.404379 0.048 Uiso 1 1 calc R U . . .
C86 C -0.1005(3) 0.9424(2) 0.4681(2) 0.0399(8) Uani 1 1 d . . . . .
H86 H -0.156792 0.985034 0.497166 0.048 Uiso 1 1 calc R U . . .
C87 C 0.0287(3) 0.9174(3) 0.4804(2) 0.0421(8) Uani 1 1 d . . . . .
H87 H 0.061066 0.943447 0.517656 0.051 Uiso 1 1 calc R U . . .
C88 C 1.0021(4) 0.1117(3) 0.1750(3) 0.0552(10) Uani 1 1 d . . . . .
H88 H 1.021996 0.035571 0.228650 0.066 Uiso 1 1 calc R U . . .
C89 C 0.8782(4) 0.1914(3) 0.1404(3) 0.0519(9) Uani 1 1 d . . . . .
H89 H 0.811952 0.170489 0.170277 0.062 Uiso 1 1 calc R U . . .
C90 C 0.8477(3) 0.3005(3) 0.0637(3) 0.0479(9) Uani 1 1 d . . . . .
H90 H 0.760560 0.355305 0.040012 0.057 Uiso 1 1 calc R U . . .
C91 C 0.9431(3) 0.3315(3) 0.0204(3) 0.0438(8) Uani 1 1 d . . . . .
H91 H 0.921952 0.408014 -0.032854 0.053 Uiso 1 1 calc R U . . .
C92 C 1.0692(3) 0.2518(3) 0.0543(3) 0.0452(8) Uani 1 1 d . . . . .
H92 H 1.135247 0.272835 0.024054 0.054 Uiso 1 1 calc R U . . .
C93 C 1.0992(3) 0.1411(3) 0.1324(3) 0.0529(10) Uani 1 1 d . . . . .
H93 H 1.186042 0.085584 0.156691 0.063 Uiso 1 1 calc R U . . .
C98A C 0.2226(4) 0.8709(4) 0.8897(3) 0.0425(13) Uani 0.645(7) 1 d G U P A 1
H98A H 0.178557 0.876739 0.944102 0.051 Uiso 0.645(7) 1 calc R U P A 1
C97A C 0.3236(4) 0.9028(3) 0.8680(3) 0.0405(13) Uani 0.645(7) 1 d G U P A 1
H97A H 0.348532 0.930366 0.907494 0.049 Uiso 0.645(7) 1 calc R U P A 1
C96A C 0.3880(3) 0.8943(4) 0.7884(4) 0.0444(15) Uani 0.645(7) 1 d G U P A 1
H96A H 0.456984 0.916101 0.773535 0.053 Uiso 0.645(7) 1 calc R U P A 1
C95A C 0.3514(5) 0.8540(4) 0.7306(3) 0.0498(15) Uani 0.645(7) 1 d G U P A 1
H95A H 0.395463 0.848208 0.676183 0.060 Uiso 0.645(7) 1 calc R U P A 1
C94A C 0.2505(5) 0.8221(4) 0.7523(4) 0.0472(14) Uani 0.645(7) 1 d G U P A 1
H94A H 0.225489 0.794580 0.712789 0.057 Uiso 0.645(7) 1 calc R U P A 1
C99A C 0.1860(3) 0.8306(4) 0.8319(4) 0.0454(15) Uani 0.645(7) 1 d G U P A 1
H99A H 0.117035 0.808845 0.846748 0.055 Uiso 0.645(7) 1 calc R U P A 1
C98B C 0.2052(7) 0.8234(9) 0.8565(6) 0.049(2) Uani 0.355(7) 1 d G U P A 2
H98B H 0.146003 0.803625 0.899618 0.059 Uiso 0.355(7) 1 calc R U P A 2
C97B C 0.2893(10) 0.8552(8) 0.8869(5) 0.058(2) Uani 0.355(7) 1 d G U P A 2
H97B H 0.287615 0.857244 0.950668 0.069 Uiso 0.355(7) 1 calc R U P A 2
C96B C 0.3760(9) 0.8841(8) 0.8238(8) 0.051(2) Uani 0.355(7) 1 d G U P A 2
H96B H 0.433490 0.905883 0.844538 0.061 Uiso 0.355(7) 1 calc R U P A 2
C95B C 0.3785(6) 0.8812(7) 0.7304(7) 0.041(2) Uani 0.355(7) 1 d G U P A 2
H95B H 0.437754 0.900904 0.687357 0.050 Uiso 0.355(7) 1 calc R U P A 2
C94B C 0.2944(7) 0.8493(6) 0.7001(5) 0.0322(19) Uani 0.355(7) 1 d G U P A 2
H94B H 0.296144 0.847287 0.636304 0.039 Uiso 0.355(7) 1 calc R U P A 2
C99B C 0.2078(7) 0.8204(8) 0.7632(7) 0.040(2) Uani 0.355(7) 1 d G U P A 2
H99B H 0.150268 0.798647 0.742434 0.047 Uiso 0.355(7) 1 calc R U P A 2
C100 C 0.1479(15) 0.4847(12) 0.8470(12) 0.042(4) Uani 0.46(4) 1 d G . P B 1
H100 H 0.208420 0.408334 0.892551 0.050 Uiso 0.46(4) 1 calc R U P B 1
C101 C 0.0921(15) 0.5592(19) 0.8860(9) 0.036(4) Uani 0.46(4) 1 d G . P B 1
H101 H 0.114446 0.533769 0.958194 0.043 Uiso 0.46(4) 1 calc R U P B 1
C102 C 0.0035(18) 0.6710(15) 0.8194(14) 0.029(3) Uani 0.46(4) 1 d G . P B 1
H102 H -0.034613 0.721916 0.846068 0.034 Uiso 0.46(4) 1 calc R U P B 1
C103 C -0.0292(14) 0.7082(9) 0.7138(12) 0.037(3) Uani 0.46(4) 1 d G . P B 1
H103 H -0.089701 0.784629 0.668299 0.044 Uiso 0.46(4) 1 calc R U P B 1
C104 C 0.0266(16) 0.6337(14) 0.6748(8) 0.043(4) Uani 0.46(4) 1 d G . P B 1
H104 H 0.004271 0.659196 0.602655 0.052 Uiso 0.46(4) 1 calc R U P B 1
C105 C 0.1152(19) 0.5220(12) 0.7414(14) 0.040(4) Uani 0.46(4) 1 d G . P B 1
H105 H 0.153331 0.471049 0.714779 0.048 Uiso 0.46(4) 1 calc R U P B 1
C106 C 0.1354(13) 0.4688(7) 0.8368(9) 0.036(3) Uani 0.54(4) 1 d G . P B 2
H106 H 0.184373 0.388384 0.868700 0.043 Uiso 0.54(4) 1 calc R U P B 2
C107 C 0.1105(14) 0.5220(14) 0.8975(8) 0.036(3) Uani 0.54(4) 1 d G . P B 2
H107 H 0.142445 0.477902 0.970845 0.043 Uiso 0.54(4) 1 calc R U P B 2
C108 C 0.0388(16) 0.6397(14) 0.8509(14) 0.033(3) Uani 0.54(4) 1 d G . P B 2
H108 H 0.021760 0.676082 0.892377 0.040 Uiso 0.54(4) 1 calc R U P B 2
C109 C -0.0080(13) 0.7043(7) 0.7436(14) 0.032(3) Uani 0.54(4) 1 d G . P B 2
H109 H -0.056997 0.784747 0.711764 0.038 Uiso 0.54(4) 1 calc R U P B 2
C110 C 0.0169(12) 0.6511(10) 0.6829(8) 0.030(3) Uani 0.54(4) 1 d G . P B 2
H110 H -0.015071 0.695231 0.609618 0.036 Uiso 0.54(4) 1 calc R U P B 2
C111 C 0.0886(15) 0.5334(10) 0.7296(9) 0.030(3) Uani 0.54(4) 1 d G . P B 2
H111 H 0.105614 0.497050 0.688084 0.036 Uiso 0.54(4) 1 calc R U P B 2
B1 B 0.7781(3) 0.4073(2) 0.4939(2) 0.0176(6) Uani 1 1 d . . . . .
B2 B 0.3932(3) 0.5693(2) 0.4094(2) 0.0192(6) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C22 1.363(3) . ?
O1 B1 1.464(3) . ?
O2 C42 1.375(3) . ?
O2 B1 1.459(3) . ?
O3 C62 1.360(3) . ?
O3 B1 1.461(3) . ?
O4 C33 1.392(3) . ?
O4 B2 1.360(3) . ?
O5 C53 1.395(3) . ?
O5 B2 1.363(3) . ?
O6 C73 1.392(3) . ?
O6 B2 1.364(3) . ?
N1 C1 1.364(3) . ?
N1 C2 1.383(3) . ?
N1 C4 1.455(3) . ?
N2 C1 1.357(3) . ?
N2 C3 1.381(3) . ?
N2 C13 1.454(3) . ?
C1 B1 1.709(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.333(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.393(4) . ?
C4 C9 1.395(4) . ?
C5 C6 1.397(4) . ?
C5 C10 1.503(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.387(4) . ?
C7 C8 1.387(4) . ?
C7 C11 1.515(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.389(4) . ?
C9 C12 1.503(4) . ?
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 C14 1.398(4) . ?
C13 C18 1.387(3) . ?
C14 C15 1.390(4) . ?
C14 C19 1.502(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.396(4) . ?
C16 C17 1.385(4) . ?
C16 C20 1.511(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.389(4) . ?
C18 C21 1.502(4) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.388(3) . ?
C22 C31 1.417(3) . ?
C23 C24 1.424(3) . ?
C23 C32 1.485(3) . ?
C24 C25 1.422(3) . ?
C24 C29 1.425(3) . ?
C25 H25 0.9500 . ?
C25 C26 1.370(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.409(4) . ?
C27 H27 0.9500 . ?
C27 C28 1.360(4) . ?
C28 H28 0.9500 . ?
C28 C29 1.414(3) . ?
C29 C30 1.413(3) . ?
C30 H30 0.9500 . ?
C30 C31 1.366(3) . ?
C31 H31 0.9500 . ?
C32 C33 1.376(3) . ?
C32 C41 1.430(3) . ?
C33 C34 1.407(3) . ?
C34 H34 0.9500 . ?
C34 C35 1.364(4) . ?
C35 H35 0.9500 . ?
C35 C36 1.411(4) . ?
C36 C37 1.414(4) . ?
C36 C41 1.429(3) . ?
C37 H37 0.9500 . ?
C37 C38 1.360(4) . ?
C38 H38 0.9500 . ?
C38 C39 1.407(4) . ?
C39 H39 0.9500 . ?
C39 C40 1.369(4) . ?
C40 H40 0.9500 . ?
C40 C41 1.416(4) . ?
C42 C43 1.376(3) . ?
C42 C51 1.414(3) . ?
C43 C44 1.431(3) . ?
C43 C52 1.485(3) . ?
C44 C45 1.416(3) . ?
C44 C49 1.419(3) . ?
C45 H45 0.9500 . ?
C45 C46 1.372(4) . ?
C46 H46 0.9500 . ?
C46 C47 1.407(4) . ?
C47 H47 0.9500 . ?
C47 C48 1.363(4) . ?
C48 H48 0.9500 . ?
C48 C49 1.423(3) . ?
C49 C50 1.410(4) . ?
C50 H50 0.9500 . ?
C50 C51 1.364(3) . ?
C51 H51 0.9500 . ?
C52 C53 1.370(3) . ?
C52 C61 1.430(3) . ?
C53 C54 1.407(3) . ?
C54 H54 0.9500 . ?
C54 C55 1.366(4) . ?
C55 H55 0.9500 . ?
C55 C56 1.415(4) . ?
C56 C57 1.416(4) . ?
C56 C61 1.421(4) . ?
C57 H57 0.9500 . ?
C57 C58 1.361(4) . ?
C58 H58 0.9500 . ?
C58 C59 1.404(4) . ?
C59 H59 0.9500 . ?
C59 C60 1.370(4) . ?
C60 H60 0.9500 . ?
C60 C61 1.421(4) . ?
C62 C63 1.379(3) . ?
C62 C71 1.424(3) . ?
C63 C64 1.430(3) . ?
C63 C72 1.493(3) . ?
C64 C65 1.421(4) . ?
C64 C69 1.416(3) . ?
C65 H65 0.9500 . ?
C65 C66 1.374(4) . ?
C66 H66 0.9500 . ?
C66 C67 1.403(4) . ?
C67 H67 0.9500 . ?
C67 C68 1.363(4) . ?
C68 H68 0.9500 . ?
C68 C69 1.418(4) . ?
C69 C70 1.415(4) . ?
C70 H70 0.9500 . ?
C70 C71 1.360(3) . ?
C71 H71 0.9500 . ?
C72 C73 1.369(4) . ?
C72 C81 1.426(3) . ?
C73 C74 1.407(4) . ?
C74 H74 0.9500 . ?
C74 C75 1.366(4) . ?
C75 H75 0.9500 . ?
C75 C76 1.412(4) . ?
C76 C77 1.414(4) . ?
C76 C81 1.420(4) . ?
C77 H77 0.9500 . ?
C77 C78 1.364(4) . ?
C78 H78 0.9500 . ?
C78 C79 1.401(4) . ?
C79 H79 0.9500 . ?
C79 C80 1.369(4) . ?
C80 H80 0.9500 . ?
C80 C81 1.417(4) . ?
C82 H82 0.9500 . ?
C82 C83 1.372(4) . ?
C82 C87 1.387(5) . ?
C83 H83 0.9500 . ?
C83 C84 1.375(4) . ?
C84 H84 0.9500 . ?
C84 C85 1.384(4) . ?
C85 H85 0.9500 . ?
C85 C86 1.373(4) . ?
C86 H86 0.9500 . ?
C86 C87 1.383(5) . ?
C87 H87 0.9500 . ?
C88 H88 0.9500 . ?
C88 C89 1.358(5) . ?
C88 C93 1.380(5) . ?
C89 H89 0.9500 . ?
C89 C90 1.357(5) . ?
C90 H90 0.9500 . ?
C90 C91 1.375(5) . ?
C91 H91 0.9500 . ?
C91 C92 1.377(5) . ?
C92 H92 0.9500 . ?
C92 C93 1.380(5) . ?
C93 H93 0.9500 . ?
C98A H98A 0.9500 . ?
C98A C97A 1.3900 . ?
C98A C99A 1.3900 . ?
C97A H97A 0.9500 . ?
C97A C96A 1.3900 . ?
C96A H96A 0.9500 . ?
C96A C95A 1.3900 . ?
C95A H95A 0.9500 . ?
C95A C94A 1.3900 . ?
C94A H94A 0.9500 . ?
C94A C99A 1.3900 . ?
C99A H99A 0.9500 . ?
C98B H98B 0.9500 . ?
C98B C97B 1.3900 . ?
C98B C99B 1.3900 . ?
C97B H97B 0.9500 . ?
C97B C96B 1.3900 . ?
C96B H96B 0.9500 . ?
C96B C95B 1.3900 . ?
C95B H95B 0.9500 . ?
C95B C94B 1.3900 . ?
C94B H94B 0.9500 . ?
C94B C99B 1.3900 . ?
C99B H99B 0.9500 . ?
C100 H100 0.9500 . ?
C100 C101 1.3900 . ?
C100 C105 1.3900 . ?
C101 H101 0.9500 . ?
C101 C102 1.3900 . ?
C102 H102 0.9500 . ?
C102 C103 1.3900 . ?
C103 H103 0.9500 . ?
C103 C104 1.3900 . ?
C104 H104 0.9500 . ?
C104 C105 1.3900 . ?
C105 H105 0.9500 . ?
C106 H106 0.9500 . ?
C106 C107 1.3900 . ?
C106 C111 1.3900 . ?
C107 H107 0.9500 . ?
C107 C108 1.3900 . ?
C108 H108 0.9500 . ?
C108 C109 1.3900 . ?
C109 H109 0.9500 . ?
C109 C110 1.3900 . ?
C110 H110 0.9500 . ?
C110 C111 1.3900 . ?
C111 H111 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
C22 O1 B1 132.66(19) . . ?
C42 O2 B1 126.53(19) . . ?
C62 O3 B1 126.30(18) . . ?
B2 O4 C33 126.77(19) . . ?
B2 O5 C53 124.91(19) . . ?
B2 O6 C73 122.8(2) . . ?
C1 N1 C2 111.3(2) . . ?
C1 N1 C4 130.0(2) . . ?
C2 N1 C4 117.9(2) . . ?
C1 N2 C3 111.6(2) . . ?
C1 N2 C13 130.6(2) . . ?
C3 N2 C13 117.2(2) . . ?
N1 C1 B1 126.0(2) . . ?
N2 C1 N1 103.3(2) . . ?
N2 C1 B1 130.6(2) . . ?
N1 C2 H2 126.6 . . ?
C3 C2 N1 106.9(2) . . ?
C3 C2 H2 126.6 . . ?
N2 C3 H3 126.6 . . ?
C2 C3 N2 106.9(2) . . ?
C2 C3 H3 126.6 . . ?
C5 C4 N1 117.4(2) . . ?
C5 C4 C9 122.8(2) . . ?
C9 C4 N1 119.1(2) . . ?
C4 C5 C6 117.4(2) . . ?
C4 C5 C10 121.9(2) . . ?
C6 C5 C10 120.7(2) . . ?
C5 C6 H6 119.1 . . ?
C7 C6 C5 121.7(3) . . ?
C7 C6 H6 119.1 . . ?
C6 C7 C11 120.4(3) . . ?
C8 C7 C6 118.6(2) . . ?
C8 C7 C11 121.0(3) . . ?
C7 C8 H8 118.9 . . ?
C7 C8 C9 122.3(3) . . ?
C9 C8 H8 118.9 . . ?
C4 C9 C12 122.5(2) . . ?
C8 C9 C4 117.2(2) . . ?
C8 C9 C12 120.3(2) . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
C5 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C11 H11A 109.5 . . ?
C7 C11 H11B 109.5 . . ?
C7 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 N2 117.1(2) . . ?
C18 C13 N2 119.0(2) . . ?
C18 C13 C14 123.3(2) . . ?
C13 C14 C19 121.6(2) . . ?
C15 C14 C13 117.2(2) . . ?
C15 C14 C19 121.1(2) . . ?
C14 C15 H15 119.2 . . ?
C14 C15 C16 121.7(2) . . ?
C16 C15 H15 119.2 . . ?
C15 C16 C20 120.2(3) . . ?
C17 C16 C15 118.4(2) . . ?
C17 C16 C20 121.4(3) . . ?
C16 C17 H17 118.8 . . ?
C16 C17 C18 122.5(2) . . ?
C18 C17 H17 118.8 . . ?
C13 C18 C17 116.9(2) . . ?
C13 C18 C21 120.8(2) . . ?
C17 C18 C21 122.3(2) . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
C14 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C16 C20 H20A 109.5 . . ?
C16 C20 H20B 109.5 . . ?
C16 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O1 C22 C23 118.1(2) . . ?
O1 C22 C31 121.8(2) . . ?
C23 C22 C31 120.1(2) . . ?
C22 C23 C24 119.7(2) . . ?
C22 C23 C32 119.7(2) . . ?
C24 C23 C32 120.5(2) . . ?
C23 C24 C29 119.7(2) . . ?
C25 C24 C23 122.3(2) . . ?
C25 C24 C29 117.9(2) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 C24 120.8(2) . . ?
C26 C25 H25 119.6 . . ?
C25 C26 H26 119.6 . . ?
C25 C26 C27 120.9(3) . . ?
C27 C26 H26 119.6 . . ?
C26 C27 H27 120.2 . . ?
C28 C27 C26 119.7(2) . . ?
C28 C27 H27 120.2 . . ?
C27 C28 H28 119.3 . . ?
C27 C28 C29 121.3(3) . . ?
C29 C28 H28 119.3 . . ?
C28 C29 C24 119.3(2) . . ?
C30 C29 C24 118.4(2) . . ?
C30 C29 C28 122.2(2) . . ?
C29 C30 H30 119.3 . . ?
C31 C30 C29 121.5(2) . . ?
C31 C30 H30 119.3 . . ?
C22 C31 H31 119.9 . . ?
C30 C31 C22 120.3(2) . . ?
C30 C31 H31 119.9 . . ?
C33 C32 C23 119.0(2) . . ?
C33 C32 C41 118.3(2) . . ?
C41 C32 C23 122.8(2) . . ?
O4 C33 C34 121.3(2) . . ?
C32 C33 O4 115.8(2) . . ?
C32 C33 C34 122.8(2) . . ?
C33 C34 H34 120.5 . . ?
C35 C34 C33 119.0(2) . . ?
C35 C34 H34 120.5 . . ?
C34 C35 H35 119.3 . . ?
C34 C35 C36 121.5(2) . . ?
C36 C35 H35 119.3 . . ?
C35 C36 C37 122.3(2) . . ?
C35 C36 C41 119.0(2) . . ?
C37 C36 C41 118.7(2) . . ?
C36 C37 H37 119.3 . . ?
C38 C37 C36 121.5(3) . . ?
C38 C37 H37 119.3 . . ?
C37 C38 H38 120.0 . . ?
C37 C38 C39 120.0(3) . . ?
C39 C38 H38 120.0 . . ?
C38 C39 H39 119.8 . . ?
C40 C39 C38 120.4(3) . . ?
C40 C39 H39 119.8 . . ?
C39 C40 H40 119.5 . . ?
C39 C40 C41 121.1(3) . . ?
C41 C40 H40 119.5 . . ?
C36 C41 C32 119.3(2) . . ?
C40 C41 C32 122.4(2) . . ?
C40 C41 C36 118.3(2) . . ?
O2 C42 C43 119.2(2) . . ?
O2 C42 C51 120.6(2) . . ?
C43 C42 C51 120.1(2) . . ?
C42 C43 C44 119.5(2) . . ?
C42 C43 C52 121.6(2) . . ?
C44 C43 C52 118.6(2) . . ?
C45 C44 C43 122.2(2) . . ?
C45 C44 C49 118.0(2) . . ?
C49 C44 C43 119.8(2) . . ?
C44 C45 H45 119.2 . . ?
C46 C45 C44 121.6(2) . . ?
C46 C45 H45 119.2 . . ?
C45 C46 H46 120.0 . . ?
C45 C46 C47 120.0(3) . . ?
C47 C46 H46 120.0 . . ?
C46 C47 H47 119.9 . . ?
C48 C47 C46 120.2(2) . . ?
C48 C47 H47 119.9 . . ?
C47 C48 H48 119.6 . . ?
C47 C48 C49 120.9(2) . . ?
C49 C48 H48 119.6 . . ?
C44 C49 C48 119.3(2) . . ?
C50 C49 C44 118.5(2) . . ?
C50 C49 C48 122.1(2) . . ?
C49 C50 H50 119.5 . . ?
C51 C50 C49 121.0(2) . . ?
C51 C50 H50 119.5 . . ?
C42 C51 H51 119.6 . . ?
C50 C51 C42 120.8(2) . . ?
C50 C51 H51 119.6 . . ?
C53 C52 C43 119.3(2) . . ?
C53 C52 C61 118.4(2) . . ?
C61 C52 C43 122.2(2) . . ?
O5 C53 C54 120.4(2) . . ?
C52 C53 O5 116.6(2) . . ?
C52 C53 C54 122.8(2) . . ?
C53 C54 H54 120.5 . . ?
C55 C54 C53 119.1(2) . . ?
C55 C54 H54 120.5 . . ?
C54 C55 H55 119.4 . . ?
C54 C55 C56 121.2(2) . . ?
C56 C55 H55 119.4 . . ?
C55 C56 C57 122.1(2) . . ?
C55 C56 C61 119.0(2) . . ?
C57 C56 C61 119.0(2) . . ?
C56 C57 H57 119.4 . . ?
C58 C57 C56 121.2(3) . . ?
C58 C57 H57 119.4 . . ?
C57 C58 H58 120.0 . . ?
C57 C58 C59 120.1(3) . . ?
C59 C58 H58 120.0 . . ?
C58 C59 H59 119.7 . . ?
C60 C59 C58 120.6(3) . . ?
C60 C59 H59 119.7 . . ?
C59 C60 H60 119.7 . . ?
C59 C60 C61 120.7(3) . . ?
C61 C60 H60 119.7 . . ?
C56 C61 C52 119.6(2) . . ?
C56 C61 C60 118.5(2) . . ?
C60 C61 C52 122.0(2) . . ?
O3 C62 C63 119.0(2) . . ?
O3 C62 C71 121.2(2) . . ?
C63 C62 C71 119.7(2) . . ?
C62 C63 C64 120.1(2) . . ?
C62 C63 C72 121.5(2) . . ?
C64 C63 C72 118.3(2) . . ?
C65 C64 C63 122.0(2) . . ?
C69 C64 C63 119.7(2) . . ?
C69 C64 C65 118.3(2) . . ?
C64 C65 H65 119.7 . . ?
C66 C65 C64 120.7(2) . . ?
C66 C65 H65 119.7 . . ?
C65 C66 H66 119.7 . . ?
C65 C66 C67 120.6(3) . . ?
C67 C66 H66 119.7 . . ?
C66 C67 H67 119.9 . . ?
C68 C67 C66 120.1(2) . . ?
C68 C67 H67 119.9 . . ?
C67 C68 H68 119.6 . . ?
C67 C68 C69 120.8(3) . . ?
C69 C68 H68 119.6 . . ?
C64 C69 C68 119.4(2) . . ?
C70 C69 C64 118.6(2) . . ?
C70 C69 C68 121.9(2) . . ?
C69 C70 H70 119.3 . . ?
C71 C70 C69 121.3(2) . . ?
C71 C70 H70 119.3 . . ?
C62 C71 H71 119.7 . . ?
C70 C71 C62 120.7(2) . . ?
C70 C71 H71 119.7 . . ?
C73 C72 C63 119.9(2) . . ?
C73 C72 C81 118.6(2) . . ?
C81 C72 C63 121.4(2) . . ?
O6 C73 C74 120.3(2) . . ?
C72 C73 O6 116.9(2) . . ?
C72 C73 C74 122.6(2) . . ?
C73 C74 H74 120.5 . . ?
C75 C74 C73 119.1(2) . . ?
C75 C74 H74 120.5 . . ?
C74 C75 H75 119.5 . . ?
C74 C75 C76 121.1(2) . . ?
C76 C75 H75 119.5 . . ?
C75 C76 C77 122.0(3) . . ?
C75 C76 C81 119.2(2) . . ?
C77 C76 C81 118.8(3) . . ?
C76 C77 H77 119.6 . . ?
C78 C77 C76 120.8(3) . . ?
C78 C77 H77 119.6 . . ?
C77 C78 H78 119.8 . . ?
C77 C78 C79 120.5(3) . . ?
C79 C78 H78 119.8 . . ?
C78 C79 H79 119.8 . . ?
C80 C79 C78 120.4(3) . . ?
C80 C79 H79 119.8 . . ?
C79 C80 H80 119.7 . . ?
C79 C80 C81 120.6(3) . . ?
C81 C80 H80 119.7 . . ?
C76 C81 C72 119.4(2) . . ?
C80 C81 C72 121.8(2) . . ?
C80 C81 C76 118.8(2) . . ?
C83 C82 H82 120.3 . . ?
C83 C82 C87 119.5(3) . . ?
C87 C82 H82 120.3 . . ?
C82 C83 H83 119.7 . . ?
C82 C83 C84 120.6(3) . . ?
C84 C83 H83 119.7 . . ?
C83 C84 H84 120.1 . . ?
C83 C84 C85 119.8(3) . . ?
C85 C84 H84 120.1 . . ?
C84 C85 H85 119.9 . . ?
C86 C85 C84 120.2(3) . . ?
C86 C85 H85 119.9 . . ?
C85 C86 H86 120.2 . . ?
C85 C86 C87 119.7(3) . . ?
C87 C86 H86 120.2 . . ?
C82 C87 H87 119.9 . . ?
C86 C87 C82 120.3(3) . . ?
C86 C87 H87 119.9 . . ?
C89 C88 H88 120.0 . . ?
C89 C88 C93 120.1(3) . . ?
C93 C88 H88 120.0 . . ?
C88 C89 H89 119.5 . . ?
C90 C89 C88 120.9(3) . . ?
C90 C89 H89 119.5 . . ?
C89 C90 H90 120.1 . . ?
C89 C90 C91 119.9(3) . . ?
C91 C90 H90 120.1 . . ?
C90 C91 H91 120.0 . . ?
C90 C91 C92 120.0(3) . . ?
C92 C91 H91 120.0 . . ?
C91 C92 H92 120.2 . . ?
C91 C92 C93 119.6(3) . . ?
C93 C92 H92 120.2 . . ?
C88 C93 C92 119.5(3) . . ?
C88 C93 H93 120.3 . . ?
C92 C93 H93 120.3 . . ?
C97A C98A H98A 120.0 . . ?
C97A C98A C99A 120.0 . . ?
C99A C98A H98A 120.0 . . ?
C98A C97A H97A 120.0 . . ?
C96A C97A C98A 120.0 . . ?
C96A C97A H97A 120.0 . . ?
C97A C96A H96A 120.0 . . ?
C95A C96A C97A 120.0 . . ?
C95A C96A H96A 120.0 . . ?
C96A C95A H95A 120.0 . . ?
C96A C95A C94A 120.0 . . ?
C94A C95A H95A 120.0 . . ?
C95A C94A H94A 120.0 . . ?
C99A C94A C95A 120.0 . . ?
C99A C94A H94A 120.0 . . ?
C98A C99A H99A 120.0 . . ?
C94A C99A C98A 120.0 . . ?
C94A C99A H99A 120.0 . . ?
C97B C98B H98B 120.0 . . ?
C97B C98B C99B 120.0 . . ?
C99B C98B H98B 120.0 . . ?
C98B C97B H97B 120.0 . . ?
C96B C97B C98B 120.0 . . ?
C96B C97B H97B 120.0 . . ?
C97B C96B H96B 120.0 . . ?
C95B C96B C97B 120.0 . . ?
C95B C96B H96B 120.0 . . ?
C96B C95B H95B 120.0 . . ?
C96B C95B C94B 120.0 . . ?
C94B C95B H95B 120.0 . . ?
C95B C94B H94B 120.0 . . ?
C99B C94B C95B 120.0 . . ?
C99B C94B H94B 120.0 . . ?
C98B C99B H99B 120.0 . . ?
C94B C99B C98B 120.0 . . ?
C94B C99B H99B 120.0 . . ?
C101 C100 H100 120.0 . . ?
C101 C100 C105 120.0 . . ?
C105 C100 H100 120.0 . . ?
C100 C101 H101 120.0 . . ?
C102 C101 C100 120.0 . . ?
C102 C101 H101 120.0 . . ?
C101 C102 H102 120.0 . . ?
C103 C102 C101 120.0 . . ?
C103 C102 H102 120.0 . . ?
C102 C103 H103 120.0 . . ?
C102 C103 C104 120.0 . . ?
C104 C103 H103 120.0 . . ?
C103 C104 H104 120.0 . . ?
C105 C104 C103 120.0 . . ?
C105 C104 H104 120.0 . . ?
C100 C105 H105 120.0 . . ?
C104 C105 C100 120.0 . . ?
C104 C105 H105 120.0 . . ?
C107 C106 H106 120.0 . . ?
C107 C106 C111 120.0 . . ?
C111 C106 H106 120.0 . . ?
C106 C107 H107 120.0 . . ?
C106 C107 C108 120.0 . . ?
C108 C107 H107 120.0 . . ?
C107 C108 H108 120.0 . . ?
C109 C108 C107 120.0 . . ?
C109 C108 H108 120.0 . . ?
C108 C109 H109 120.0 . . ?
C110 C109 C108 120.0 . . ?
C110 C109 H109 120.0 . . ?
C109 C110 H110 120.0 . . ?
C109 C110 C111 120.0 . . ?
C111 C110 H110 120.0 . . ?
C106 C111 H111 120.0 . . ?
C110 C111 C106 120.0 . . ?
C110 C111 H111 120.0 . . ?
O1 B1 C1 110.85(19) . . ?
O2 B1 O1 114.1(2) . . ?
O2 B1 O3 109.7(2) . . ?
O2 B1 C1 106.41(19) . . ?
O3 B1 O1 107.42(19) . . ?
O3 B1 C1 108.32(19) . . ?
O4 B2 O5 119.8(2) . . ?
O4 B2 O6 121.1(2) . . ?
O5 B2 O6 119.0(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C22 C23 C24 176.1(2) . . . . ?
O1 C22 C23 C32 -7.8(3) . . . . ?
O1 C22 C31 C30 -174.0(2) . . . . ?
O2 C42 C43 C44 175.3(2) . . . . ?
O2 C42 C43 C52 -10.8(3) . . . . ?
O2 C42 C51 C50 -173.0(2) . . . . ?
O3 C62 C63 C64 178.4(2) . . . . ?
O3 C62 C63 C72 -5.4(3) . . . . ?
O3 C62 C71 C70 -177.3(2) . . . . ?
O4 C33 C34 C35 -176.7(2) . . . . ?
O5 C53 C54 C55 -174.5(2) . . . . ?
O6 C73 C74 C75 -175.3(2) . . . . ?
N1 C1 B1 O1 149.8(2) . . . . ?
N1 C1 B1 O2 -85.7(3) . . . . ?
N1 C1 B1 O3 32.2(3) . . . . ?
N1 C2 C3 N2 -0.7(3) . . . . ?
N1 C4 C5 C6 173.3(2) . . . . ?
N1 C4 C5 C10 -4.8(3) . . . . ?
N1 C4 C9 C8 -173.1(2) . . . . ?
N1 C4 C9 C12 5.7(4) . . . . ?
N2 C1 B1 O1 -25.1(3) . . . . ?
N2 C1 B1 O2 99.4(3) . . . . ?
N2 C1 B1 O3 -142.7(2) . . . . ?
N2 C13 C14 C15 -173.1(2) . . . . ?
N2 C13 C14 C19 10.2(3) . . . . ?
N2 C13 C18 C17 174.4(2) . . . . ?
N2 C13 C18 C21 -5.3(3) . . . . ?
C1 N1 C2 C3 0.3(3) . . . . ?
C1 N1 C4 C5 82.0(3) . . . . ?
C1 N1 C4 C9 -107.8(3) . . . . ?
C1 N2 C3 C2 0.9(3) . . . . ?
C1 N2 C13 C14 -91.2(3) . . . . ?
C1 N2 C13 C18 98.1(3) . . . . ?
C2 N1 C1 N2 0.2(3) . . . . ?
C2 N1 C1 B1 -175.9(2) . . . . ?
C2 N1 C4 C5 -86.7(3) . . . . ?
C2 N1 C4 C9 83.5(3) . . . . ?
C3 N2 C1 N1 -0.7(3) . . . . ?
C3 N2 C1 B1 175.1(2) . . . . ?
C3 N2 C13 C14 79.6(3) . . . . ?
C3 N2 C13 C18 -91.0(3) . . . . ?
C4 N1 C1 N2 -169.1(2) . . . . ?
C4 N1 C1 B1 14.9(4) . . . . ?
C4 N1 C2 C3 171.1(2) . . . . ?
C4 C5 C6 C7 -1.5(4) . . . . ?
C5 C4 C9 C8 -3.6(4) . . . . ?
C5 C4 C9 C12 175.2(2) . . . . ?
C5 C6 C7 C8 -0.5(4) . . . . ?
C5 C6 C7 C11 -179.0(2) . . . . ?
C6 C7 C8 C9 0.5(4) . . . . ?
C7 C8 C9 C4 1.4(4) . . . . ?
C7 C8 C9 C12 -177.4(3) . . . . ?
C9 C4 C5 C6 3.6(4) . . . . ?
C9 C4 C5 C10 -174.6(2) . . . . ?
C10 C5 C6 C7 176.7(2) . . . . ?
C11 C7 C8 C9 179.0(3) . . . . ?
C13 N2 C1 N1 170.6(2) . . . . ?
C13 N2 C1 B1 -13.6(4) . . . . ?
C13 N2 C3 C2 -171.6(2) . . . . ?
C13 C14 C15 C16 -0.5(4) . . . . ?
C14 C13 C18 C17 4.3(4) . . . . ?
C14 C13 C18 C21 -175.3(2) . . . . ?
C14 C15 C16 C17 2.4(4) . . . . ?
C14 C15 C16 C20 -176.8(2) . . . . ?
C15 C16 C17 C18 -0.8(4) . . . . ?
C16 C17 C18 C13 -2.4(4) . . . . ?
C16 C17 C18 C21 177.2(2) . . . . ?
C18 C13 C14 C15 -2.9(4) . . . . ?
C18 C13 C14 C19 -179.6(2) . . . . ?
C19 C14 C15 C16 176.2(2) . . . . ?
C20 C16 C17 C18 178.3(2) . . . . ?
C22 O1 B1 O2 -29.7(3) . . . . ?
C22 O1 B1 O3 -151.5(2) . . . . ?
C22 O1 B1 C1 90.4(3) . . . . ?
C22 C23 C24 C25 178.7(2) . . . . ?
C22 C23 C24 C29 -1.4(3) . . . . ?
C22 C23 C32 C33 -71.2(3) . . . . ?
C22 C23 C32 C41 108.9(3) . . . . ?
C23 C22 C31 C30 5.1(3) . . . . ?
C23 C24 C25 C26 177.9(2) . . . . ?
C23 C24 C29 C28 -177.8(2) . . . . ?
C23 C24 C29 C30 3.9(3) . . . . ?
C23 C32 C33 O4 -5.8(3) . . . . ?
C23 C32 C33 C34 176.8(2) . . . . ?
C23 C32 C41 C36 -175.5(2) . . . . ?
C23 C32 C41 C40 4.7(4) . . . . ?
C24 C23 C32 C33 104.9(3) . . . . ?
C24 C23 C32 C41 -75.1(3) . . . . ?
C24 C25 C26 C27 0.5(4) . . . . ?
C24 C29 C30 C31 -1.9(3) . . . . ?
C25 C24 C29 C28 2.1(3) . . . . ?
C25 C24 C29 C30 -176.3(2) . . . . ?
C25 C26 C27 C28 0.9(4) . . . . ?
C26 C27 C28 C29 -0.8(4) . . . . ?
C27 C28 C29 C24 -0.8(4) . . . . ?
C27 C28 C29 C30 177.5(2) . . . . ?
C28 C29 C30 C31 179.8(2) . . . . ?
C29 C24 C25 C26 -1.9(4) . . . . ?
C29 C30 C31 C22 -2.6(4) . . . . ?
C31 C22 C23 C24 -3.1(3) . . . . ?
C31 C22 C23 C32 173.1(2) . . . . ?
C32 C23 C24 C25 2.7(3) . . . . ?
C32 C23 C24 C29 -177.5(2) . . . . ?
C32 C33 C34 C35 0.5(3) . . . . ?
C33 O4 B2 O5 -157.6(2) . . . . ?
C33 O4 B2 O6 27.0(4) . . . . ?
C33 C32 C41 C36 4.6(3) . . . . ?
C33 C32 C41 C40 -175.3(2) . . . . ?
C33 C34 C35 C36 0.9(4) . . . . ?
C34 C35 C36 C37 179.9(2) . . . . ?
C34 C35 C36 C41 0.5(4) . . . . ?
C35 C36 C37 C38 -177.6(2) . . . . ?
C35 C36 C41 C32 -3.3(3) . . . . ?
C35 C36 C41 C40 176.6(2) . . . . ?
C36 C37 C38 C39 0.4(4) . . . . ?
C37 C36 C41 C32 177.3(2) . . . . ?
C37 C36 C41 C40 -2.9(3) . . . . ?
C37 C38 C39 C40 -1.6(4) . . . . ?
C38 C39 C40 C41 0.5(4) . . . . ?
C39 C40 C41 C32 -178.4(2) . . . . ?
C39 C40 C41 C36 1.7(4) . . . . ?
C41 C32 C33 O4 174.13(19) . . . . ?
C41 C32 C33 C34 -3.3(3) . . . . ?
C41 C36 C37 C38 1.8(4) . . . . ?
C42 O2 B1 O1 -109.7(3) . . . . ?
C42 O2 B1 O3 10.8(3) . . . . ?
C42 O2 B1 C1 127.8(2) . . . . ?
C42 C43 C44 C45 175.8(2) . . . . ?
C42 C43 C44 C49 -1.9(3) . . . . ?
C42 C43 C52 C53 -90.6(3) . . . . ?
C42 C43 C52 C61 93.3(3) . . . . ?
C43 C42 C51 C50 3.6(4) . . . . ?
C43 C44 C45 C46 -176.9(2) . . . . ?
C43 C44 C49 C48 179.5(2) . . . . ?
C43 C44 C49 C50 3.0(3) . . . . ?
C43 C52 C53 O5 -0.4(3) . . . . ?
C43 C52 C53 C54 -174.9(2) . . . . ?
C43 C52 C61 C56 174.5(2) . . . . ?
C43 C52 C61 C60 -6.1(4) . . . . ?
C44 C43 C52 C53 83.4(3) . . . . ?
C44 C43 C52 C61 -92.7(3) . . . . ?
C44 C45 C46 C47 -2.4(4) . . . . ?
C44 C49 C50 C51 -0.8(3) . . . . ?
C45 C44 C49 C48 1.7(3) . . . . ?
C45 C44 C49 C50 -174.8(2) . . . . ?
C45 C46 C47 C48 1.3(4) . . . . ?
C46 C47 C48 C49 1.2(4) . . . . ?
C47 C48 C49 C44 -2.7(4) . . . . ?
C47 C48 C49 C50 173.7(2) . . . . ?
C48 C49 C50 C51 -177.2(2) . . . . ?
C49 C44 C45 C46 0.8(4) . . . . ?
C49 C50 C51 C42 -2.5(4) . . . . ?
C51 C42 C43 C44 -1.4(3) . . . . ?
C51 C42 C43 C52 172.6(2) . . . . ?
C52 C43 C44 C45 1.7(3) . . . . ?
C52 C43 C44 C49 -176.0(2) . . . . ?
C52 C53 C54 C55 -0.2(4) . . . . ?
C53 O5 B2 O4 21.6(4) . . . . ?
C53 O5 B2 O6 -162.9(2) . . . . ?
C53 C52 C61 C56 -1.6(3) . . . . ?
C53 C52 C61 C60 177.8(2) . . . . ?
C53 C54 C55 C56 -0.7(4) . . . . ?
C54 C55 C56 C57 -179.6(2) . . . . ?
C54 C55 C56 C61 0.4(4) . . . . ?
C55 C56 C57 C58 179.5(3) . . . . ?
C55 C56 C61 C52 0.7(3) . . . . ?
C55 C56 C61 C60 -178.6(2) . . . . ?
C56 C57 C58 C59 -0.5(4) . . . . ?
C57 C56 C61 C52 -179.2(2) . . . . ?
C57 C56 C61 C60 1.4(3) . . . . ?
C57 C58 C59 C60 0.8(4) . . . . ?
C58 C59 C60 C61 0.0(4) . . . . ?
C59 C60 C61 C52 179.5(2) . . . . ?
C59 C60 C61 C56 -1.1(4) . . . . ?
C61 C52 C53 O5 175.9(2) . . . . ?
C61 C52 C53 C54 1.4(3) . . . . ?
C61 C56 C57 C58 -0.6(4) . . . . ?
C62 O3 B1 O1 -23.1(3) . . . . ?
C62 O3 B1 O2 -147.6(2) . . . . ?
C62 O3 B1 C1 96.7(2) . . . . ?
C62 C63 C64 C65 176.4(2) . . . . ?
C62 C63 C64 C69 -1.6(3) . . . . ?
C62 C63 C72 C73 -91.9(3) . . . . ?
C62 C63 C72 C81 93.0(3) . . . . ?
C63 C62 C71 C70 -1.2(4) . . . . ?
C63 C64 C65 C66 -176.3(2) . . . . ?
C63 C64 C69 C68 177.6(2) . . . . ?
C63 C64 C69 C70 0.1(3) . . . . ?
C63 C72 C73 O6 -0.2(3) . . . . ?
C63 C72 C73 C74 -176.3(2) . . . . ?
C63 C72 C81 C76 176.2(2) . . . . ?
C63 C72 C81 C80 -3.1(4) . . . . ?
C64 C63 C72 C73 84.4(3) . . . . ?
C64 C63 C72 C81 -90.7(3) . . . . ?
C64 C65 C66 C67 -1.5(4) . . . . ?
C64 C69 C70 C71 0.9(4) . . . . ?
C65 C64 C69 C68 -0.5(3) . . . . ?
C65 C64 C69 C70 -178.0(2) . . . . ?
C65 C66 C67 C68 0.0(4) . . . . ?
C66 C67 C68 C69 1.2(4) . . . . ?
C67 C68 C69 C64 -1.0(4) . . . . ?
C67 C68 C69 C70 176.5(2) . . . . ?
C68 C69 C70 C71 -176.5(2) . . . . ?
C69 C64 C65 C66 1.7(4) . . . . ?
C69 C70 C71 C62 -0.4(4) . . . . ?
C71 C62 C63 C64 2.2(3) . . . . ?
C71 C62 C63 C72 178.4(2) . . . . ?
C72 C63 C64 C65 0.1(3) . . . . ?
C72 C63 C64 C69 -178.0(2) . . . . ?
C72 C73 C74 C75 0.7(4) . . . . ?
C73 O6 B2 O4 -154.4(2) . . . . ?
C73 O6 B2 O5 30.2(3) . . . . ?
C73 C72 C81 C76 1.0(3) . . . . ?
C73 C72 C81 C80 -178.3(2) . . . . ?
C73 C74 C75 C76 -0.3(4) . . . . ?
C74 C75 C76 C77 179.6(2) . . . . ?
C74 C75 C76 C81 0.2(4) . . . . ?
C75 C76 C77 C78 -178.2(3) . . . . ?
C75 C76 C81 C72 -0.6(4) . . . . ?
C75 C76 C81 C80 178.8(2) . . . . ?
C76 C77 C78 C79 -0.6(4) . . . . ?
C77 C76 C81 C72 -180.0(2) . . . . ?
C77 C76 C81 C80 -0.6(4) . . . . ?
C77 C78 C79 C80 -0.6(4) . . . . ?
C78 C79 C80 C81 1.1(4) . . . . ?
C79 C80 C81 C72 178.8(2) . . . . ?
C79 C80 C81 C76 -0.5(4) . . . . ?
C81 C72 C73 O6 175.1(2) . . . . ?
C81 C72 C73 C74 -1.1(4) . . . . ?
C81 C76 C77 C78 1.2(4) . . . . ?
C82 C83 C84 C85 0.0(5) . . . . ?
C83 C82 C87 C86 0.1(4) . . . . ?
C83 C84 C85 C86 -0.3(5) . . . . ?
C84 C85 C86 C87 0.6(5) . . . . ?
C85 C86 C87 C82 -0.5(4) . . . . ?
C87 C82 C83 C84 0.2(5) . . . . ?
C88 C89 C90 C91 -0.3(5) . . . . ?
C89 C88 C93 C92 -0.2(5) . . . . ?
C89 C90 C91 C92 0.5(5) . . . . ?
C90 C91 C92 C93 -0.6(5) . . . . ?
C91 C92 C93 C88 0.5(5) . . . . ?
C93 C88 C89 C90 0.2(5) . . . . ?
C98A C97A C96A C95A 0.0 . . . . ?
C97A C98A C99A C94A 0.0 . . . . ?
C97A C96A C95A C94A 0.0 . . . . ?
C96A C95A C94A C99A 0.0 . . . . ?
C95A C94A C99A C98A 0.0 . . . . ?
C99A C98A C97A C96A 0.0 . . . . ?
C98B C97B C96B C95B 0.0 . . . . ?
C97B C98B C99B C94B 0.0 . . . . ?
C97B C96B C95B C94B 0.0 . . . . ?
C96B C95B C94B C99B 0.0 . . . . ?
C95B C94B C99B C98B 0.0 . . . . ?
C99B C98B C97B C96B 0.0 . . . . ?
C100 C101 C102 C103 0.0 . . . . ?
C101 C100 C105 C104 0.0 . . . . ?
C101 C102 C103 C104 0.0 . . . . ?
C102 C103 C104 C105 0.0 . . . . ?
C103 C104 C105 C100 0.0 . . . . ?
C105 C100 C101 C102 0.0 . . . . ?
C106 C107 C108 C109 0.0 . . . . ?
C107 C106 C111 C110 0.0 . . . . ?
C107 C108 C109 C110 0.0 . . . . ?
C108 C109 C110 C111 0.0 . . . . ?
C109 C110 C111 C106 0.0 . . . . ?
C111 C106 C107 C108 0.0 . . . . ?
B1 O1 C22 C23 169.5(2) . . . . ?
B1 O1 C22 C31 -11.4(4) . . . . ?
B1 O2 C42 C43 124.2(2) . . . . ?
B1 O2 C42 C51 -59.2(3) . . . . ?
B1 O3 C62 C63 138.6(2) . . . . ?
B1 O3 C62 C71 -45.2(3) . . . . ?
B2 O4 C33 C32 128.2(2) . . . . ?
B2 O4 C33 C34 -54.4(3) . . . . ?
B2 O5 C53 C52 120.8(3) . . . . ?
B2 O5 C53 C54 -64.6(3) . . . . ?
B2 O6 C73 C72 109.1(3) . . . . ?
B2 O6 C73 C74 -74.6(3) . . . . ?

_olex2_exptl_crystal_mounting_method 'MiTeGen 200 micron MicroLoop'
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.6(8)
2 0.4(8)
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Benzene'
####################################################################### 
# 
# 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_R-3
_database_code_depnum_ccdc_archive 'CCDC 2058922'
loop_
_audit_author_name
_audit_author_address
'Daniel Unruh'
;Texas Tech University
United States of America
;
_audit_update_record             
;
2021-02-01 deposited with the CCDC.	2021-03-23 downloaded from the CCDC.
;
_audit_creation_date             2021-01-15
_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         'C32 H27 B F5 O3 P'
_chemical_formula_sum            'C32 H27 B F5 O3 P'
_chemical_formula_weight         596.31
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   10.0487(10)
_cell_length_b                   12.5685(13)
_cell_length_c                   22.072(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2787.6(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9860
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.151
_cell_measurement_theta_min      2.227
_shelx_estimated_absorpt_T_max   0.937
_shelx_estimated_absorpt_T_min   0.925
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0418 before and 0.0279 after correction.
The Ratio of minimum to maximum transmission is 0.9238.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.4
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            28202
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.179
_diffrn_reflns_theta_min         1.845
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.776
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                5990
_reflns_number_total             6187
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details 
;
 Flack x determined using 2562 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         6187
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0257
_refine_ls_restrained_S_all      1.026
_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)+(0.0327P)²+0.8902P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0653
_refine_special_details          Twin
_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 Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C29(H29A,H29B), C31(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C15(H15), C16(H16), C19(H19),
 C20(H20), C22(H22), C23(H23), C24(H24), C25(H25)
2.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.70839(4) 0.44014(4) 0.37138(2) 0.01201(10) Uani 1 1 d . . . . .
F1 F 0.25829(12) 0.59661(9) 0.32497(5) 0.0231(3) Uani 1 1 d . . . . .
F2 F 0.18527(14) 0.79366(10) 0.35223(6) 0.0293(3) Uani 1 1 d . . . . .
F3 F 0.27064(14) 0.88755(9) 0.45656(6) 0.0303(3) Uani 1 1 d . . . . .
F4 F 0.42593(15) 0.77567(10) 0.53510(6) 0.0356(3) Uani 1 1 d . . . . .
F5 F 0.49746(13) 0.57719(9) 0.50966(5) 0.0258(3) Uani 1 1 d . . . . .
O1 O 0.58812(12) 0.45941(10) 0.41299(6) 0.0132(3) Uani 1 1 d . . . . .
O2 O 0.42138(12) 0.41510(10) 0.34103(6) 0.0129(2) Uani 1 1 d . . . . .
O3 O 0.37957(12) 0.38665(10) 0.44890(6) 0.0123(3) Uani 1 1 d . . . . .
C1 C 0.38361(17) 0.57621(14) 0.41557(8) 0.0133(3) Uani 1 1 d . . . . .
C2 C 0.30380(19) 0.63658(14) 0.37800(8) 0.0151(3) Uani 1 1 d . . . . .
C3 C 0.2641(2) 0.73990(15) 0.39086(9) 0.0186(4) Uani 1 1 d . . . . .
C4 C 0.3061(2) 0.78764(15) 0.44353(9) 0.0212(4) Uani 1 1 d . . . . .
C5 C 0.3852(2) 0.73055(16) 0.48303(9) 0.0212(4) Uani 1 1 d . . . . .
C6 C 0.42107(19) 0.62760(15) 0.46871(9) 0.0170(4) Uani 1 1 d . . . . .
C7 C 0.32075(17) 0.34686(14) 0.32681(8) 0.0126(3) Uani 1 1 d . . . . .
C8 C 0.30281(18) 0.25013(14) 0.35608(7) 0.0124(3) Uani 1 1 d . . . . .
C9 C 0.18821(18) 0.18757(14) 0.34070(8) 0.0126(3) Uani 1 1 d . . . . .
C10 C 0.15220(18) 0.09445(14) 0.37354(8) 0.0145(3) Uani 1 1 d . . . . .
H10 H 0.206732 0.071196 0.406109 0.017 Uiso 1 1 calc R U . . .
C11 C 0.04010(19) 0.03777(15) 0.35895(9) 0.0184(4) Uani 1 1 d . . . . .
H11 H 0.017293 -0.023690 0.381759 0.022 Uiso 1 1 calc R U . . .
C12 C -0.04140(18) 0.06995(16) 0.31045(9) 0.0199(4) Uani 1 1 d . . . . .
H12 H -0.118615 0.029954 0.300535 0.024 Uiso 1 1 calc R U . . .
C13 C -0.00979(19) 0.15866(15) 0.27752(9) 0.0171(4) Uani 1 1 d . . . . .
H13 H -0.064553 0.179047 0.244416 0.021 Uiso 1 1 calc R U . . .
C14 C 0.10355(18) 0.22047(15) 0.29219(8) 0.0139(3) Uani 1 1 d . . . . .
C15 C 0.13414(19) 0.31512(15) 0.26045(8) 0.0154(4) Uani 1 1 d . . . . .
H15 H 0.080951 0.335848 0.226888 0.018 Uiso 1 1 calc R U . . .
C16 C 0.23894(18) 0.37680(14) 0.27748(8) 0.0143(4) Uani 1 1 d . . . . .
H16 H 0.257394 0.440645 0.256030 0.017 Uiso 1 1 calc R U . . .
C17 C 0.39976(17) 0.21552(14) 0.40335(8) 0.0120(3) Uani 1 1 d . . . . .
C18 C 0.43153(17) 0.28602(14) 0.44909(8) 0.0119(3) Uani 1 1 d . . . . .
C19 C 0.52034(19) 0.25904(15) 0.49629(8) 0.0151(4) Uani 1 1 d . . . . .
H19 H 0.536132 0.307845 0.528361 0.018 Uiso 1 1 calc R U . . .
C20 C 0.58345(19) 0.16288(15) 0.49581(9) 0.0167(4) Uani 1 1 d . . . . .
H20 H 0.642714 0.144919 0.527747 0.020 Uiso 1 1 calc R U . . .
C21 C 0.56122(18) 0.08942(15) 0.44795(9) 0.0156(4) Uani 1 1 d . . . . .
C22 C 0.6321(2) -0.00784(17) 0.44515(10) 0.0232(4) Uani 1 1 d . . . . .
H22 H 0.692525 -0.025490 0.476689 0.028 Uiso 1 1 calc R U . . .
C23 C 0.6152(2) -0.07684(17) 0.39784(10) 0.0263(4) Uani 1 1 d . . . . .
H23 H 0.663351 -0.141839 0.396716 0.032 Uiso 1 1 calc R U . . .
C24 C 0.5258(2) -0.05113(16) 0.35068(9) 0.0225(4) Uani 1 1 d . . . . .
H24 H 0.514776 -0.098659 0.317593 0.027 Uiso 1 1 calc R U . . .
C25 C 0.45449(19) 0.04236(15) 0.35236(9) 0.0171(4) Uani 1 1 d . . . . .
H25 H 0.394617 0.058365 0.320324 0.021 Uiso 1 1 calc R U . . .
C26 C 0.46876(18) 0.11544(14) 0.40112(8) 0.0133(3) Uani 1 1 d . . . . .
C27 C 0.73342(19) 0.30294(15) 0.35155(9) 0.0192(4) Uani 1 1 d . . . . .
H27A H 0.830216 0.291014 0.346668 0.023 Uiso 1 1 calc R U . . .
H27B H 0.703552 0.258682 0.386074 0.023 Uiso 1 1 calc R U . . .
C28 C 0.6639(2) 0.26257(17) 0.29452(10) 0.0243(4) Uani 1 1 d . . . . .
H28A H 0.698878 0.300351 0.259087 0.036 Uiso 1 1 calc R U . . .
H28B H 0.568015 0.275331 0.297874 0.036 Uiso 1 1 calc R U . . .
H28C H 0.680324 0.186123 0.289986 0.036 Uiso 1 1 calc R U . . .
C29 C 0.84768(18) 0.48256(16) 0.41556(9) 0.0168(4) Uani 1 1 d . . . . .
H29A H 0.826571 0.552826 0.433416 0.020 Uiso 1 1 calc R U . . .
H29B H 0.859703 0.431841 0.449439 0.020 Uiso 1 1 calc R U . . .
C30 C 0.97941(19) 0.49165(19) 0.38135(10) 0.0257(5) Uani 1 1 d . . . . .
H30A H 1.004181 0.421805 0.365158 0.039 Uiso 1 1 calc R U . . .
H30B H 1.048940 0.516628 0.409047 0.039 Uiso 1 1 calc R U . . .
H30C H 0.969572 0.542347 0.347917 0.039 Uiso 1 1 calc R U . . .
C31 C 0.6959(2) 0.51908(16) 0.30385(9) 0.0182(4) Uani 1 1 d . . . . .
H31A H 0.778890 0.511538 0.280050 0.022 Uiso 1 1 calc R U . . .
H31B H 0.621437 0.492281 0.278776 0.022 Uiso 1 1 calc R U . . .
C32 C 0.6728(2) 0.63681(17) 0.31805(11) 0.0272(5) Uani 1 1 d . . . . .
H32A H 0.657538 0.675822 0.280242 0.041 Uiso 1 1 calc R U . . .
H32B H 0.751304 0.665882 0.338574 0.041 Uiso 1 1 calc R U . . .
H32C H 0.594916 0.644114 0.344415 0.041 Uiso 1 1 calc R U . . .
B1 B 0.43804(19) 0.45455(16) 0.40322(9) 0.0119(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 O1 1.5372(13) . ?
P1 C27 1.7967(19) . ?
P1 C29 1.7873(19) . ?
P1 C31 1.7949(19) . ?
F1 C2 1.353(2) . ?
F2 C3 1.346(2) . ?
F3 C4 1.337(2) . ?
F4 C5 1.345(2) . ?
F5 C6 1.345(2) . ?
O1 B1 1.525(2) . ?
O2 C7 1.363(2) . ?
O2 B1 1.469(2) . ?
O3 C18 1.368(2) . ?
O3 B1 1.446(2) . ?
C1 C2 1.381(3) . ?
C1 C6 1.391(3) . ?
C1 B1 1.647(3) . ?
C2 C3 1.388(3) . ?
C3 C4 1.375(3) . ?
C4 C5 1.381(3) . ?
C5 C6 1.380(3) . ?
C7 C8 1.388(2) . ?
C7 C16 1.415(2) . ?
C8 C9 1.435(2) . ?
C8 C17 1.492(2) . ?
C9 C10 1.423(3) . ?
C9 C14 1.429(2) . ?
C10 H10 0.9500 . ?
C10 C11 1.371(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.407(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.368(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.416(3) . ?
C14 C15 1.414(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.361(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.381(2) . ?
C17 C26 1.437(2) . ?
C18 C19 1.413(2) . ?
C19 H19 0.9500 . ?
C19 C20 1.365(3) . ?
C20 H20 0.9500 . ?
C20 C21 1.421(3) . ?
C21 C22 1.416(3) . ?
C21 C26 1.428(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.368(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.412(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.377(3) . ?
C25 H25 0.9500 . ?
C25 C26 1.422(3) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.526(3) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.528(3) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.530(3) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 P1 C27 114.00(8) . . ?
O1 P1 C29 104.04(8) . . ?
O1 P1 C31 110.74(8) . . ?
C29 P1 C27 108.04(9) . . ?
C29 P1 C31 110.05(9) . . ?
C31 P1 C27 109.76(10) . . ?
B1 O1 P1 133.39(12) . . ?
C7 O2 B1 120.82(14) . . ?
C18 O3 B1 113.13(13) . . ?
C2 C1 C6 114.11(17) . . ?
C2 C1 B1 127.14(16) . . ?
C6 C1 B1 118.75(16) . . ?
F1 C2 C1 120.79(16) . . ?
F1 C2 C3 115.29(16) . . ?
C1 C2 C3 123.93(18) . . ?
F2 C3 C2 120.61(17) . . ?
F2 C3 C4 119.82(17) . . ?
C4 C3 C2 119.56(18) . . ?
F3 C4 C3 120.69(18) . . ?
F3 C4 C5 120.38(18) . . ?
C3 C4 C5 118.93(18) . . ?
F4 C5 C4 119.70(17) . . ?
F4 C5 C6 120.76(18) . . ?
C6 C5 C4 119.54(18) . . ?
F5 C6 C1 120.17(16) . . ?
F5 C6 C5 115.91(17) . . ?
C5 C6 C1 123.92(18) . . ?
O2 C7 C8 122.71(16) . . ?
O2 C7 C16 116.16(16) . . ?
C8 C7 C16 121.02(16) . . ?
C7 C8 C9 118.28(16) . . ?
C7 C8 C17 119.72(16) . . ?
C9 C8 C17 121.98(16) . . ?
C10 C9 C8 122.27(16) . . ?
C10 C9 C14 117.92(16) . . ?
C14 C9 C8 119.77(16) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 C9 121.10(17) . . ?
C11 C10 H10 119.5 . . ?
C10 C11 H11 119.8 . . ?
C10 C11 C12 120.49(18) . . ?
C12 C11 H11 119.8 . . ?
C11 C12 H12 119.9 . . ?
C13 C12 C11 120.20(17) . . ?
C13 C12 H12 119.9 . . ?
C12 C13 H13 119.6 . . ?
C12 C13 C14 120.82(17) . . ?
C14 C13 H13 119.6 . . ?
C13 C14 C9 119.44(17) . . ?
C15 C14 C9 119.02(16) . . ?
C15 C14 C13 121.53(17) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 C14 120.71(17) . . ?
C16 C15 H15 119.6 . . ?
C7 C16 H16 119.6 . . ?
C15 C16 C7 120.70(17) . . ?
C15 C16 H16 119.6 . . ?
C18 C17 C8 118.37(16) . . ?
C18 C17 C26 118.36(16) . . ?
C26 C17 C8 123.11(16) . . ?
O3 C18 C17 120.17(15) . . ?
O3 C18 C19 117.72(16) . . ?
C17 C18 C19 122.09(16) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 C18 120.01(17) . . ?
C20 C19 H19 120.0 . . ?
C19 C20 H20 119.7 . . ?
C19 C20 C21 120.54(17) . . ?
C21 C20 H20 119.7 . . ?
C20 C21 C26 119.46(17) . . ?
C22 C21 C20 120.96(18) . . ?
C22 C21 C26 119.56(18) . . ?
C21 C22 H22 119.4 . . ?
C23 C22 C21 121.19(19) . . ?
C23 C22 H22 119.4 . . ?
C22 C23 H23 120.1 . . ?
C22 C23 C24 119.78(19) . . ?
C24 C23 H23 120.1 . . ?
C23 C24 H24 119.8 . . ?
C25 C24 C23 120.43(19) . . ?
C25 C24 H24 119.8 . . ?
C24 C25 H25 119.4 . . ?
C24 C25 C26 121.27(18) . . ?
C26 C25 H25 119.4 . . ?
C21 C26 C17 119.32(16) . . ?
C25 C26 C17 122.85(16) . . ?
C25 C26 C21 117.75(16) . . ?
P1 C27 H27A 108.0 . . ?
P1 C27 H27B 108.0 . . ?
H27A C27 H27B 107.3 . . ?
C28 C27 P1 117.12(14) . . ?
C28 C27 H27A 108.0 . . ?
C28 C27 H27B 108.0 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
P1 C29 H29A 108.4 . . ?
P1 C29 H29B 108.4 . . ?
H29A C29 H29B 107.5 . . ?
C30 C29 P1 115.53(14) . . ?
C30 C29 H29A 108.4 . . ?
C30 C29 H29B 108.4 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
P1 C31 H31A 109.2 . . ?
P1 C31 H31B 109.2 . . ?
H31A C31 H31B 107.9 . . ?
C32 C31 P1 112.03(14) . . ?
C32 C31 H31A 109.2 . . ?
C32 C31 H31B 109.2 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O1 B1 C1 105.55(14) . . ?
O2 B1 O1 104.97(14) . . ?
O2 B1 C1 115.48(15) . . ?
O3 B1 O1 109.09(15) . . ?
O3 B1 O2 113.95(15) . . ?
O3 B1 C1 107.32(14) . . ?

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
P1 O1 B1 O2 5.1(2) . . . . ?
P1 O1 B1 O3 127.55(15) . . . . ?
P1 O1 B1 C1 -117.41(15) . . . . ?
F1 C2 C3 F2 0.3(3) . . . . ?
F1 C2 C3 C4 -179.56(18) . . . . ?
F2 C3 C4 F3 -0.8(3) . . . . ?
F2 C3 C4 C5 178.99(19) . . . . ?
F3 C4 C5 F4 0.5(3) . . . . ?
F3 C4 C5 C6 -179.80(19) . . . . ?
F4 C5 C6 F5 0.1(3) . . . . ?
F4 C5 C6 C1 -179.45(19) . . . . ?
O1 P1 C27 C28 90.00(16) . . . . ?
O1 P1 C29 C30 -169.21(15) . . . . ?
O1 P1 C31 C32 52.58(17) . . . . ?
O2 C7 C8 C9 175.59(15) . . . . ?
O2 C7 C8 C17 -2.7(2) . . . . ?
O2 C7 C16 C15 -178.69(16) . . . . ?
O3 C18 C19 C20 -174.56(16) . . . . ?
C1 C2 C3 F2 -179.49(17) . . . . ?
C1 C2 C3 C4 0.6(3) . . . . ?
C2 C1 C6 F5 179.15(16) . . . . ?
C2 C1 C6 C5 -1.3(3) . . . . ?
C2 C1 B1 O1 128.26(18) . . . . ?
C2 C1 B1 O2 12.8(3) . . . . ?
C2 C1 B1 O3 -115.48(19) . . . . ?
C2 C3 C4 F3 179.11(18) . . . . ?
C2 C3 C4 C5 -1.1(3) . . . . ?
C3 C4 C5 F4 -179.27(19) . . . . ?
C3 C4 C5 C6 0.5(3) . . . . ?
C4 C5 C6 F5 -179.59(19) . . . . ?
C4 C5 C6 C1 0.8(3) . . . . ?
C6 C1 C2 F1 -179.24(16) . . . . ?
C6 C1 C2 C3 0.5(3) . . . . ?
C6 C1 B1 O1 -50.7(2) . . . . ?
C6 C1 B1 O2 -166.19(16) . . . . ?
C6 C1 B1 O3 65.5(2) . . . . ?
C7 O2 B1 O1 142.64(15) . . . . ?
C7 O2 B1 O3 23.4(2) . . . . ?
C7 O2 B1 C1 -101.58(18) . . . . ?
C7 C8 C9 C10 -171.74(16) . . . . ?
C7 C8 C9 C14 6.1(2) . . . . ?
C7 C8 C17 C18 50.4(2) . . . . ?
C7 C8 C17 C26 -124.99(19) . . . . ?
C8 C7 C16 C15 5.0(3) . . . . ?
C8 C9 C10 C11 178.17(17) . . . . ?
C8 C9 C14 C13 -179.62(16) . . . . ?
C8 C9 C14 C15 -0.5(2) . . . . ?
C8 C17 C18 O3 -3.1(2) . . . . ?
C8 C17 C18 C19 178.75(16) . . . . ?
C8 C17 C26 C21 179.17(16) . . . . ?
C8 C17 C26 C25 2.5(3) . . . . ?
C9 C8 C17 C18 -127.89(18) . . . . ?
C9 C8 C17 C26 56.7(2) . . . . ?
C9 C10 C11 C12 0.7(3) . . . . ?
C9 C14 C15 C16 -3.0(3) . . . . ?
C10 C9 C14 C13 -1.7(2) . . . . ?
C10 C9 C14 C15 177.44(16) . . . . ?
C10 C11 C12 C13 -0.3(3) . . . . ?
C11 C12 C13 C14 -1.1(3) . . . . ?
C12 C13 C14 C9 2.1(3) . . . . ?
C12 C13 C14 C15 -176.98(18) . . . . ?
C13 C14 C15 C16 176.08(17) . . . . ?
C14 C9 C10 C11 0.3(3) . . . . ?
C14 C15 C16 C7 0.9(3) . . . . ?
C16 C7 C8 C9 -8.4(2) . . . . ?
C16 C7 C8 C17 173.27(16) . . . . ?
C17 C8 C9 C10 6.6(3) . . . . ?
C17 C8 C9 C14 -175.60(15) . . . . ?
C17 C18 C19 C20 3.7(3) . . . . ?
C18 O3 B1 O1 -57.31(19) . . . . ?
C18 O3 B1 O2 59.62(19) . . . . ?
C18 O3 B1 C1 -171.20(14) . . . . ?
C18 C17 C26 C21 3.8(2) . . . . ?
C18 C17 C26 C25 -172.84(17) . . . . ?
C18 C19 C20 C21 0.3(3) . . . . ?
C19 C20 C21 C22 176.22(18) . . . . ?
C19 C20 C21 C26 -2.0(3) . . . . ?
C20 C21 C22 C23 -177.3(2) . . . . ?
C20 C21 C26 C17 -0.1(3) . . . . ?
C20 C21 C26 C25 176.75(17) . . . . ?
C21 C22 C23 C24 0.1(3) . . . . ?
C22 C21 C26 C17 -178.33(17) . . . . ?
C22 C21 C26 C25 -1.5(3) . . . . ?
C22 C23 C24 C25 -0.7(3) . . . . ?
C23 C24 C25 C26 0.2(3) . . . . ?
C24 C25 C26 C17 177.65(18) . . . . ?
C24 C25 C26 C21 1.0(3) . . . . ?
C26 C17 C18 O3 172.51(15) . . . . ?
C26 C17 C18 C19 -5.7(3) . . . . ?
C26 C21 C22 C23 1.0(3) . . . . ?
C27 P1 O1 B1 -71.21(18) . . . . ?
C27 P1 C29 C30 69.30(18) . . . . ?
C27 P1 C31 C32 179.33(15) . . . . ?
C29 P1 O1 B1 171.35(16) . . . . ?
C29 P1 C27 C28 -154.89(15) . . . . ?
C29 P1 C31 C32 -61.90(17) . . . . ?
C31 P1 O1 B1 53.15(18) . . . . ?
C31 P1 C27 C28 -34.88(18) . . . . ?
C31 P1 C29 C30 -50.53(18) . . . . ?
B1 O2 C7 C8 -56.3(2) . . . . ?
B1 O2 C7 C16 127.52(17) . . . . ?
B1 O3 C18 C17 -72.8(2) . . . . ?
B1 O3 C18 C19 105.41(18) . . . . ?
B1 C1 C2 F1 1.7(3) . . . . ?
B1 C1 C2 C3 -178.51(17) . . . . ?
B1 C1 C6 F5 -1.7(3) . . . . ?
B1 C1 C6 C5 177.86(18) . . . . ?

_olex2_exptl_crystal_mounting_method 'MiTeGen 200 micron MicroLoop'
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Benzene'
####################################################################### 
# 
# 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_RR-2
_database_code_depnum_ccdc_archive 'CCDC 2058921'
loop_
_audit_author_name
_audit_author_address
'Daniel Unruh'
;Texas Tech University
United States of America
;
_audit_update_record             
;
2021-02-01 deposited with the CCDC.	2021-03-23 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT340_RR-2                
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01197 Ang.  
RESPONSE: Due to the small crystals and the weakly diffracting nature of 
          the crystals. Multiple crystals were analyzed after multiple 
          crystallization attempts, but this data represents the highest
          quality data set to be collected.
;
_vrf_PLAT089_RR-2                
;
PROBLEM: Poor Data / Parameter Ratio (Zmax < 18) ........       6.63 Note  
RESPONSE: Due to the weak diffraction quality of the crystal.
;
_vrf_PLAT911_RR-2                
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         30 Report
RESPONSE: These reflections were omitted during the absorption correction.
;
# end Validation Reply Form

_audit_creation_date             2021-01-15
_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         'C52 H24 B2 F10 O4'
_chemical_formula_sum            'C52 H24 B2 F10 O4'
_chemical_formula_weight         924.33
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   15.525(3)
_cell_length_b                   11.785(2)
_cell_length_c                   23.532(5)
_cell_angle_alpha                90
_cell_angle_beta                 108.241(4)
_cell_angle_gamma                90
_cell_volume                     4089.1(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.254
_cell_measurement_theta_min      2.217
_shelx_estimated_absorpt_T_max   0.991
_shelx_estimated_absorpt_T_min   0.971
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0783 before and 0.0520 after correction.
The Ratio of minimum to maximum transmission is 0.7003.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.075
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0900
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            15324
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.446
_diffrn_reflns_theta_min         1.381
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.876
_reflns_Friedel_fraction_full    0.975
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                11534
_reflns_number_total             15324
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    ?
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 
;
 Flack x determined using 3861 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.1(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1190
_refine_ls_number_reflns         15324
_refine_ls_number_restraints     55
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0598
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0538P)²+0.6137P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1221
_refine_special_details          'Refined as a 2-component twin.,Twin'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.5964(14)
 0.4036(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Rigid body (RIGU) restrains
 C59, C67, C68, C69, C66, C65, C64
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C53, C54, C58, B3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C11(H11), C12(H12), C13(H13), C14(H14), C19(H19), C20(H20),
 C21(H21), C22(H22), C24(H24), C25(H25), C28(H28), C29(H29), C31(H31), C32(H32),
  C33(H33), C34(H34), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44),
 C45(H45), C60(H60), C61(H61), C63(H63), C64(H64), C65(H65), C66(H66), C71(H71),
  C72(H72), C73(H73), C74(H74), C76(H76), C77(H77), C80(H80), C81(H81),
 C83(H83), C84(H84), C85(H85), C86(H86), C91(H91), C92(H92), C93(H93), C94(H94),
  C96(H96), C97(H97)
4.b Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C53(C54,C55,C56,C57,C58), C99(C100,C101,C102,C103,C104)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
F1 F 0.8666(4) 0.4882(4) 0.8187(2) 0.0417(14) Uani 1 1 d . . . . .
F2 F 0.8868(4) 0.6604(5) 0.7488(2) 0.0518(17) Uani 1 1 d . . . . .
F3 F 0.8676(4) 0.8789(5) 0.7808(2) 0.0544(17) Uani 1 1 d . . . . .
F4 F 0.8280(5) 0.9231(5) 0.8843(3) 0.0563(17) Uani 1 1 d . . . . .
F5 F 0.8068(4) 0.7498(4) 0.9533(2) 0.0406(14) Uani 1 1 d . . . . .
F6 F 0.6269(4) -0.0178(4) 0.9442(2) 0.0428(14) Uani 1 1 d . . . . .
F7 F 0.5186(5) -0.1648(5) 0.8654(3) 0.0595(18) Uani 1 1 d . . . . .
F8 F 0.3836(4) -0.0871(5) 0.7701(3) 0.0583(18) Uani 1 1 d . . . . .
F9 F 0.3604(4) 0.1390(5) 0.7501(2) 0.0476(16) Uani 1 1 d . . . . .
F10 F 0.4660(4) 0.2873(4) 0.8292(2) 0.0381(14) Uani 1 1 d . . . . .
F11 F 0.3309(3) 0.2085(4) 0.5416(2) 0.0340(13) Uani 1 1 d . . . . .
F12 F 0.4135(4) 0.0407(5) 0.6183(2) 0.0452(15) Uani 1 1 d . . . . .
F13 F 0.5572(4) 0.0902(4) 0.7152(2) 0.0440(15) Uani 1 1 d . . . . .
F14 F 0.6184(4) 0.3064(5) 0.73598(19) 0.0405(14) Uani 1 1 d . . . . .
F15 F 0.5389(3) 0.4737(4) 0.6591(2) 0.0334(12) Uani 1 1 d . . . . .
F16 F 0.1971(3) 0.9850(4) 0.5410(2) 0.0330(13) Uani 1 1 d . . . . .
F17 F 0.1839(4) 1.1621(4) 0.6111(2) 0.0421(14) Uani 1 1 d . . . . .
F18 F 0.1484(4) 1.1243(4) 0.7157(2) 0.0403(14) Uani 1 1 d . . . . .
F19 F 0.1311(4) 0.9093(5) 0.75129(19) 0.0399(14) Uani 1 1 d . . . . .
F20 F 0.1471(4) 0.7310(4) 0.6823(2) 0.0386(13) Uani 1 1 d . . . . .
O1 O 0.9012(4) 0.4685(5) 0.9685(3) 0.0280(14) Uani 1 1 d . . . . .
O2 O 0.7434(4) 0.4734(5) 0.9306(2) 0.0286(14) Uani 1 1 d . . . . .
O3 O 0.7013(4) 0.2444(5) 0.9419(2) 0.0246(14) Uani 1 1 d . . . . .
O4 O 0.5742(4) 0.2852(4) 0.9710(2) 0.0227(14) Uani 1 1 d . . . . .
O5 O 0.3003(4) 0.4846(4) 0.5578(2) 0.0200(13) Uani 1 1 d . . . . .
O6 O 0.4213(4) 0.4950(4) 0.5192(2) 0.0205(13) Uani 1 1 d . . . . .
O7 O 0.1004(4) 0.7043(5) 0.5321(2) 0.0258(14) Uani 1 1 d . . . . .
O8 O 0.2583(4) 0.7112(4) 0.5617(2) 0.0218(14) Uani 1 1 d . . . . .
C1 C 0.8376(4) 0.6149(4) 0.8878(2) 0.027(2) Uani 1 1 d G . . . .
C2 C 0.8576(4) 0.5931(4) 0.8352(3) 0.028(2) Uani 1 1 d G . . . .
C3 C 0.8671(4) 0.6824(5) 0.7991(2) 0.031(2) Uani 1 1 d G . . . .
C4 C 0.8566(4) 0.7936(4) 0.8155(2) 0.039(3) Uani 1 1 d G . . . .
C5 C 0.8366(5) 0.8154(3) 0.8681(3) 0.036(2) Uani 1 1 d G . . . .
C6 C 0.8271(4) 0.7261(5) 0.9042(2) 0.031(2) Uani 1 1 d G . . . .
C7 C 0.8995(5) 0.3865(7) 1.0122(4) 0.023(2) Uani 1 1 d . . . . .
C8 C 0.9258(6) 0.4266(8) 1.0713(4) 0.031(2) Uani 1 1 d . . . . .
H8 H 0.942843 0.503586 1.080187 0.038 Uiso 1 1 calc R U . . .
C9 C 0.9262(6) 0.3521(8) 1.1156(4) 0.034(2) Uani 1 1 d . . . . .
H9 H 0.939148 0.379276 1.155419 0.041 Uiso 1 1 calc R U . . .
C10 C 0.9078(6) 0.2351(8) 1.1039(4) 0.032(2) Uani 1 1 d . . . . .
C11 C 0.9120(6) 0.1561(9) 1.1496(4) 0.040(3) Uani 1 1 d . . . . .
H11 H 0.925107 0.182370 1.189617 0.048 Uiso 1 1 calc R U . . .
C12 C 0.8979(6) 0.0430(10) 1.1381(5) 0.050(3) Uani 1 1 d . . . . .
H12 H 0.903287 -0.009382 1.169740 0.059 Uiso 1 1 calc R U . . .
C13 C 0.8750(6) 0.0052(9) 1.0783(5) 0.041(3) Uani 1 1 d . . . . .
H13 H 0.863536 -0.073078 1.069627 0.049 Uiso 1 1 calc R U . . .
C14 C 0.8692(6) 0.0792(8) 1.0330(4) 0.036(2) Uani 1 1 d . . . . .
H14 H 0.854558 0.051667 0.993162 0.043 Uiso 1 1 calc R U . . .
C15 C 0.8846(6) 0.1970(7) 1.0442(4) 0.023(2) Uani 1 1 d . . . . .
C16 C 0.8801(6) 0.2770(7) 0.9969(3) 0.021(2) Uani 1 1 d . . . . .
C17 C 0.8466(6) 0.2371(7) 0.9334(4) 0.0216(19) Uani 1 1 d . . . . .
C18 C 0.9084(6) 0.2177(7) 0.8988(4) 0.026(2) Uani 1 1 d . . . . .
C19 C 1.0025(6) 0.2371(7) 0.9236(4) 0.030(2) Uani 1 1 d . . . . .
H19 H 1.027295 0.264175 0.963462 0.036 Uiso 1 1 calc R U . . .
C20 C 1.0577(7) 0.2158(8) 0.8888(4) 0.036(2) Uani 1 1 d . . . . .
H20 H 1.121438 0.225423 0.905658 0.043 Uiso 1 1 calc R U . . .
C21 C 1.0219(7) 0.1807(7) 0.8296(4) 0.036(2) Uani 1 1 d . . . . .
H21 H 1.061311 0.170505 0.806179 0.043 Uiso 1 1 calc R U . . .
C22 C 0.9315(7) 0.1606(8) 0.8045(4) 0.032(2) Uani 1 1 d . . . . .
H22 H 0.908404 0.134392 0.764408 0.038 Uiso 1 1 calc R U . . .
C23 C 0.8721(6) 0.1792(7) 0.8387(4) 0.025(2) Uani 1 1 d . . . . .
C24 C 0.7785(6) 0.1620(8) 0.8148(4) 0.032(2) Uani 1 1 d . . . . .
H24 H 0.754310 0.135302 0.774876 0.039 Uiso 1 1 calc R U . . .
C25 C 0.7207(6) 0.1824(7) 0.8473(4) 0.028(2) Uani 1 1 d . . . . .
H25 H 0.657129 0.173042 0.829661 0.033 Uiso 1 1 calc R U . . .
C26 C 0.7575(6) 0.2177(7) 0.9076(4) 0.026(2) Uani 1 1 d . . . . .
C27 C 0.6557(6) 0.5022(7) 0.8958(4) 0.025(2) Uani 1 1 d . . . . .
C28 C 0.6332(6) 0.5220(7) 0.8334(4) 0.027(2) Uani 1 1 d . . . . .
H28 H 0.678412 0.517861 0.813990 0.033 Uiso 1 1 calc R U . . .
C29 C 0.5467(6) 0.5468(7) 0.8021(4) 0.028(2) Uani 1 1 d . . . . .
H29 H 0.531741 0.559301 0.760278 0.034 Uiso 1 1 calc R U . . .
C30 C 0.4772(6) 0.5552(7) 0.8290(4) 0.025(2) Uani 1 1 d . . . . .
C31 C 0.3866(7) 0.5800(7) 0.7972(4) 0.031(2) Uani 1 1 d . . . . .
H31 H 0.371032 0.596325 0.755721 0.037 Uiso 1 1 calc R U . . .
C32 C 0.3204(6) 0.5816(8) 0.8234(4) 0.032(2) Uani 1 1 d . . . . .
H32 H 0.259846 0.600441 0.800732 0.038 Uiso 1 1 calc R U . . .
C33 C 0.3427(6) 0.5546(7) 0.8855(4) 0.032(2) Uani 1 1 d . . . . .
H33 H 0.296543 0.552359 0.904102 0.038 Uiso 1 1 calc R U . . .
C34 C 0.4303(6) 0.5320(6) 0.9179(4) 0.0213(19) Uani 1 1 d . . . . .
H34 H 0.444469 0.516198 0.959447 0.026 Uiso 1 1 calc R U . . .
C35 C 0.4997(6) 0.5314(6) 0.8921(4) 0.0189(19) Uani 1 1 d . . . . .
C36 C 0.5916(6) 0.5045(6) 0.9247(4) 0.0192(19) Uani 1 1 d . . . . .
C37 C 0.6204(6) 0.4794(7) 0.9895(4) 0.0223(19) Uani 1 1 d . . . . .
C38 C 0.6544(5) 0.5693(7) 1.0323(3) 0.0205(19) Uani 1 1 d . . . . .
C39 C 0.6526(6) 0.6846(8) 1.0150(4) 0.027(2) Uani 1 1 d . . . . .
H39 H 0.630730 0.703973 0.973757 0.032 Uiso 1 1 calc R U . . .
C40 C 0.6818(6) 0.7680(8) 1.0567(4) 0.030(2) Uani 1 1 d . . . . .
H40 H 0.677042 0.845250 1.044489 0.036 Uiso 1 1 calc R U . . .
C41 C 0.7188(6) 0.7407(8) 1.1177(4) 0.031(2) Uani 1 1 d . . . . .
H41 H 0.739759 0.799419 1.146332 0.038 Uiso 1 1 calc R U . . .
C42 C 0.7249(6) 0.6305(9) 1.1359(4) 0.034(2) Uani 1 1 d . . . . .
H42 H 0.751509 0.613506 1.177175 0.041 Uiso 1 1 calc R U . . .
C43 C 0.6922(5) 0.5401(7) 1.0944(4) 0.0224(19) Uani 1 1 d . . . . .
C44 C 0.6938(6) 0.4268(8) 1.1127(4) 0.031(2) Uani 1 1 d . . . . .
H44 H 0.721481 0.407753 1.153606 0.037 Uiso 1 1 calc R U . . .
C45 C 0.6558(6) 0.3430(7) 1.0721(3) 0.028(2) Uani 1 1 d . . . . .
H45 H 0.654272 0.267015 1.085167 0.034 Uiso 1 1 calc R U . . .
C46 C 0.6186(6) 0.3705(7) 1.0103(3) 0.021(2) Uani 1 1 d . . . . .
C47 C 0.5497(6) 0.1409(7) 0.8906(3) 0.0225(19) Uani 1 1 d . . . . .
C48 C 0.5596(6) 0.0234(8) 0.8960(4) 0.033(2) Uani 1 1 d . . . . .
C49 C 0.5061(7) -0.0529(7) 0.8563(5) 0.036(2) Uani 1 1 d . . . . .
C50 C 0.4394(7) -0.0145(8) 0.8088(4) 0.034(2) Uani 1 1 d . . . . .
C51 C 0.4271(6) 0.1014(8) 0.7991(4) 0.035(2) Uani 1 1 d . . . . .
C52 C 0.4802(6) 0.1739(8) 0.8390(4) 0.029(2) Uani 1 1 d . . . . .
C53 C 0.4342(4) 0.3441(4) 0.5981(2) 0.0215(16) Uani 1 1 d G . . . .
C54 C 0.4018(3) 0.2335(4) 0.5879(2) 0.0252(18) Uani 1 1 d G . . . .
C55 C 0.4435(4) 0.1476(3) 0.6273(2) 0.026(2) Uani 1 1 d G . . . .
C56 C 0.5175(4) 0.1722(4) 0.6771(2) 0.030(2) Uani 1 1 d G . . . .
C57 C 0.5499(3) 0.2828(5) 0.68732(19) 0.029(2) Uani 1 1 d G . . . .
C58 C 0.5082(4) 0.3687(4) 0.6478(2) 0.0278(19) Uani 1 1 d G . . . .
C59 C 0.3811(5) 0.5833(7) 0.4796(3) 0.0185(16) Uani 1 1 d . . . . .
C60 C 0.3468(6) 0.5520(8) 0.4192(4) 0.030(2) Uani 1 1 d . . . . .
H60 H 0.350641 0.475697 0.407301 0.036 Uiso 1 1 calc R U . . .
C61 C 0.3072(6) 0.6342(8) 0.3775(4) 0.028(2) Uani 1 1 d . . . . .
H61 H 0.281683 0.613299 0.336628 0.034 Uiso 1 1 calc R U . . .
C62 C 0.3040(6) 0.7476(7) 0.3941(3) 0.024(2) Uani 1 1 d . . . . .
C63 C 0.2655(6) 0.8355(8) 0.3512(4) 0.031(2) Uani 1 1 d . . . . .
H63 H 0.239149 0.816541 0.310206 0.037 Uiso 1 1 calc R U . . .
C64 C 0.2665(6) 0.9446(8) 0.3687(4) 0.034(2) Uani 1 1 d . . . . .
H64 H 0.242604 1.002030 0.339723 0.041 Uiso 1 1 calc R U . . .
C65 C 0.3021(6) 0.9738(9) 0.4289(4) 0.035(2) Uani 1 1 d . . . . .
H65 H 0.302004 1.051197 0.440231 0.042 Uiso 1 1 calc R U . . .
C66 C 0.3372(6) 0.8939(7) 0.4720(4) 0.0262(18) Uani 1 1 d . . . . .
H66 H 0.359253 0.915631 0.512926 0.031 Uiso 1 1 calc R U . . .
C67 C 0.3406(5) 0.7779(7) 0.4557(4) 0.0200(16) Uani 1 1 d . . . . .
C68 C 0.3783(5) 0.6932(7) 0.4994(3) 0.0171(15) Uani 1 1 d . . . . .
C69 C 0.4102(5) 0.7212(7) 0.5646(3) 0.0166(17) Uani 1 1 d . . . . .
C70 C 0.5027(5) 0.7400(6) 0.5962(3) 0.0159(17) Uani 1 1 d . . . . .
C71 C 0.5715(5) 0.7355(7) 0.5677(3) 0.0197(19) Uani 1 1 d . . . . .
H71 H 0.555048 0.718023 0.526274 0.024 Uiso 1 1 calc R U . . .
C72 C 0.6601(6) 0.7558(7) 0.5987(4) 0.026(2) Uani 1 1 d . . . . .
H72 H 0.704372 0.754966 0.578475 0.031 Uiso 1 1 calc R U . . .
C73 C 0.6863(6) 0.7781(7) 0.6606(4) 0.031(2) Uani 1 1 d . . . . .
H73 H 0.748472 0.789800 0.682287 0.037 Uiso 1 1 calc R U . . .
C74 C 0.6232(6) 0.7829(8) 0.6893(4) 0.028(2) Uani 1 1 d . . . . .
H74 H 0.641635 0.799331 0.730855 0.034 Uiso 1 1 calc R U . . .
C75 C 0.5299(6) 0.7637(7) 0.6584(3) 0.021(2) Uani 1 1 d . . . . .
C76 C 0.4628(6) 0.7695(7) 0.6873(4) 0.029(2) Uani 1 1 d . . . . .
H76 H 0.480441 0.785163 0.728967 0.035 Uiso 1 1 calc R U . . .
C77 C 0.3739(6) 0.7530(7) 0.6569(4) 0.026(2) Uani 1 1 d . . . . .
H77 H 0.329766 0.755620 0.677174 0.032 Uiso 1 1 calc R U . . .
C78 C 0.3476(6) 0.7319(7) 0.5946(4) 0.0204(19) Uani 1 1 d . . . . .
C79 C 0.2491(6) 0.4614(7) 0.5957(3) 0.0221(19) Uani 1 1 d . . . . .
C80 C 0.2906(6) 0.4301(7) 0.6553(4) 0.027(2) Uani 1 1 d . . . . .
H80 H 0.354741 0.423962 0.671182 0.032 Uiso 1 1 calc R U . . .
C81 C 0.2364(6) 0.4083(7) 0.6907(3) 0.025(2) Uani 1 1 d . . . . .
H81 H 0.263869 0.385743 0.731104 0.030 Uiso 1 1 calc R U . . .
C82 C 0.1408(6) 0.4186(7) 0.6682(4) 0.023(2) Uani 1 1 d . . . . .
C83 C 0.0849(6) 0.3971(7) 0.7044(4) 0.025(2) Uani 1 1 d . . . . .
H83 H 0.111462 0.373743 0.744805 0.030 Uiso 1 1 calc R U . . .
C84 C -0.0075(6) 0.4098(8) 0.6814(4) 0.035(2) Uani 1 1 d . . . . .
H84 H -0.044743 0.394492 0.705708 0.042 Uiso 1 1 calc R U . . .
C85 C -0.0470(6) 0.4456(7) 0.6218(4) 0.033(2) Uani 1 1 d . . . . .
H85 H -0.110906 0.454811 0.606248 0.040 Uiso 1 1 calc R U . . .
C86 C 0.0056(6) 0.4672(7) 0.5862(4) 0.0228(19) Uani 1 1 d . . . . .
H86 H -0.022693 0.490666 0.546027 0.027 Uiso 1 1 calc R U . . .
C87 C 0.1025(6) 0.4553(7) 0.6078(4) 0.0222(19) Uani 1 1 d . . . . .
C88 C 0.1573(6) 0.4758(7) 0.5710(3) 0.0186(19) Uani 1 1 d . . . . .
C89 C 0.1183(6) 0.5105(7) 0.5070(4) 0.022(2) Uani 1 1 d . . . . .
C90 C 0.1094(6) 0.4256(7) 0.4610(3) 0.0222(19) Uani 1 1 d . . . . .
C91 C 0.1269(6) 0.3094(7) 0.4759(4) 0.023(2) Uani 1 1 d . . . . .
H91 H 0.146409 0.286474 0.516668 0.027 Uiso 1 1 calc R U . . .
C92 C 0.1156(6) 0.2303(9) 0.4314(4) 0.032(2) Uani 1 1 d . . . . .
H92 H 0.126995 0.152524 0.441711 0.038 Uiso 1 1 calc R U . . .
C93 C 0.0874(6) 0.2624(10) 0.3708(4) 0.043(3) Uani 1 1 d . . . . .
H93 H 0.079300 0.206568 0.340423 0.051 Uiso 1 1 calc R U . . .
C94 C 0.0719(6) 0.3730(9) 0.3559(4) 0.035(2) Uani 1 1 d . . . . .
H94 H 0.054138 0.394008 0.314908 0.042 Uiso 1 1 calc R U . . .
C95 C 0.0815(6) 0.4590(8) 0.4002(4) 0.028(2) Uani 1 1 d . . . . .
C96 C 0.0610(6) 0.5755(9) 0.3858(4) 0.037(3) Uani 1 1 d . . . . .
H96 H 0.041835 0.598724 0.345126 0.045 Uiso 1 1 calc R U . . .
C97 C 0.0683(6) 0.6539(8) 0.4294(4) 0.030(2) Uani 1 1 d . . . . .
H97 H 0.053928 0.731172 0.419280 0.036 Uiso 1 1 calc R U . . .
C98 C 0.0976(5) 0.6194(7) 0.4900(4) 0.023(2) Uani 1 1 d . . . . .
C99 C 0.1719(4) 0.8548(3) 0.6096(2) 0.0198(19) Uani 1 1 d G . . . .
C100 C 0.1815(4) 0.9652(4) 0.59175(19) 0.025(2) Uani 1 1 d G . . . .
C101 C 0.1744(4) 1.0560(3) 0.6277(2) 0.031(2) Uani 1 1 d G . . . .
C102 C 0.1577(4) 1.0364(4) 0.6816(2) 0.029(2) Uani 1 1 d G . . . .
C103 C 0.1481(4) 0.9260(5) 0.69945(18) 0.027(2) Uani 1 1 d G . . . .
C104 C 0.1551(4) 0.8352(3) 0.6635(2) 0.024(2) Uani 1 1 d G . . . .
B1 B 0.8255(7) 0.5151(8) 0.9298(4) 0.024(2) Uani 1 1 d . . . . .
B2 B 0.6112(7) 0.2259(9) 0.9346(4) 0.023(2) Uani 1 1 d . . . . .
B3 B 0.3822(7) 0.4457(8) 0.5569(4) 0.023(2) Uani 1 1 d . . . . .
B4 B 0.1790(7) 0.7508(9) 0.5670(4) 0.024(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
F1 C2 1.316(6) . ?
F2 C3 1.337(6) . ?
F3 C4 1.340(6) . ?
F4 C5 1.344(7) . ?
F5 C6 1.320(6) . ?
F6 C48 1.369(10) . ?
F7 C49 1.340(10) . ?
F8 C50 1.350(10) . ?
F9 C51 1.360(11) . ?
F10 C52 1.363(10) . ?
F11 C54 1.317(6) . ?
F12 C55 1.337(7) . ?
F13 C56 1.331(6) . ?
F14 C57 1.326(6) . ?
F15 C58 1.323(6) . ?
F16 C100 1.311(6) . ?
F17 C101 1.332(7) . ?
F18 C102 1.346(6) . ?
F19 C103 1.341(6) . ?
F20 C104 1.325(6) . ?
O1 C7 1.419(10) . ?
O1 B1 1.357(11) . ?
O2 C27 1.394(10) . ?
O2 B1 1.371(12) . ?
O3 C26 1.397(10) . ?
O3 B2 1.373(11) . ?
O4 C46 1.394(10) . ?
O4 B2 1.363(11) . ?
O5 C79 1.395(10) . ?
O5 B3 1.359(11) . ?
O6 C59 1.406(9) . ?
O6 B3 1.352(11) . ?
O7 C98 1.399(10) . ?
O7 B4 1.356(12) . ?
O8 C78 1.381(9) . ?
O8 B4 1.359(12) . ?
C1 C2 1.3900 . ?
C1 C6 1.3900 . ?
C1 B1 1.585(10) . ?
C2 C3 1.3900 . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
C5 C6 1.3900 . ?
C7 C8 1.403(12) . ?
C7 C16 1.349(11) . ?
C8 H8 0.9500 . ?
C8 C9 1.361(12) . ?
C9 H9 0.9500 . ?
C9 C10 1.418(13) . ?
C10 C11 1.408(13) . ?
C10 C15 1.410(12) . ?
C11 H11 0.9500 . ?
C11 C12 1.365(15) . ?
C12 H12 0.9500 . ?
C12 C13 1.411(15) . ?
C13 H13 0.9500 . ?
C13 C14 1.358(13) . ?
C14 H14 0.9500 . ?
C14 C15 1.419(12) . ?
C15 C16 1.444(11) . ?
C16 C17 1.495(11) . ?
C17 C18 1.458(12) . ?
C17 C26 1.344(12) . ?
C18 C19 1.412(12) . ?
C18 C23 1.424(12) . ?
C19 H19 0.9500 . ?
C19 C20 1.382(12) . ?
C20 H20 0.9500 . ?
C20 C21 1.393(13) . ?
C21 H21 0.9500 . ?
C21 C22 1.362(13) . ?
C22 H22 0.9500 . ?
C22 C23 1.417(12) . ?
C23 C24 1.399(12) . ?
C24 H24 0.9500 . ?
C24 C25 1.369(12) . ?
C25 H25 0.9500 . ?
C25 C26 1.416(11) . ?
C27 C28 1.420(11) . ?
C27 C36 1.370(11) . ?
C28 H28 0.9500 . ?
C28 C29 1.345(11) . ?
C29 H29 0.9500 . ?
C29 C30 1.414(11) . ?
C30 C31 1.402(12) . ?
C30 C35 1.443(11) . ?
C31 H31 0.9500 . ?
C31 C32 1.353(13) . ?
C32 H32 0.9500 . ?
C32 C33 1.429(12) . ?
C33 H33 0.9500 . ?
C33 C34 1.361(11) . ?
C34 H34 0.9500 . ?
C34 C35 1.394(11) . ?
C35 C36 1.428(11) . ?
C36 C37 1.478(11) . ?
C37 C38 1.443(11) . ?
C37 C46 1.376(11) . ?
C38 C39 1.416(12) . ?
C38 C43 1.436(11) . ?
C39 H39 0.9500 . ?
C39 C40 1.363(12) . ?
C40 H40 0.9500 . ?
C40 C41 1.406(12) . ?
C41 H41 0.9500 . ?
C41 C42 1.361(13) . ?
C42 H42 0.9500 . ?
C42 C43 1.427(12) . ?
C43 C44 1.401(12) . ?
C44 H44 0.9500 . ?
C44 C45 1.372(12) . ?
C45 H45 0.9500 . ?
C45 C46 1.424(11) . ?
C47 C48 1.394(12) . ?
C47 C52 1.403(12) . ?
C47 B2 1.540(13) . ?
C48 C49 1.375(13) . ?
C49 C50 1.341(14) . ?
C50 C51 1.388(13) . ?
C51 C52 1.344(12) . ?
C53 C54 1.3900 . ?
C53 C58 1.3900 . ?
C53 B3 1.592(11) . ?
C54 C55 1.3900 . ?
C55 C56 1.3900 . ?
C56 C57 1.3900 . ?
C57 C58 1.3900 . ?
C59 C60 1.401(11) . ?
C59 C68 1.382(11) . ?
C60 H60 0.9500 . ?
C60 C61 1.379(12) . ?
C61 H61 0.9500 . ?
C61 C62 1.398(12) . ?
C62 C63 1.439(11) . ?
C62 C67 1.426(11) . ?
C63 H63 0.9500 . ?
C63 C64 1.348(13) . ?
C64 H64 0.9500 . ?
C64 C65 1.393(13) . ?
C65 H65 0.9500 . ?
C65 C66 1.367(12) . ?
C66 H66 0.9500 . ?
C66 C67 1.426(12) . ?
C67 C68 1.422(11) . ?
C68 C69 1.494(11) . ?
C69 C70 1.414(11) . ?
C69 C78 1.374(11) . ?
C70 C71 1.429(10) . ?
C70 C75 1.417(10) . ?
C71 H71 0.9500 . ?
C71 C72 1.361(11) . ?
C72 H72 0.9500 . ?
C72 C73 1.410(12) . ?
C73 H73 0.9500 . ?
C73 C74 1.354(12) . ?
C74 H74 0.9500 . ?
C74 C75 1.421(11) . ?
C75 C76 1.413(12) . ?
C76 H76 0.9500 . ?
C76 C77 1.355(12) . ?
C77 H77 0.9500 . ?
C77 C78 1.416(11) . ?
C79 C80 1.398(11) . ?
C79 C88 1.370(12) . ?
C80 H80 0.9500 . ?
C80 C81 1.380(12) . ?
C81 H81 0.9500 . ?
C81 C82 1.416(12) . ?
C82 C83 1.418(12) . ?
C82 C87 1.426(11) . ?
C83 H83 0.9500 . ?
C83 C84 1.374(12) . ?
C84 H84 0.9500 . ?
C84 C85 1.408(12) . ?
C85 H85 0.9500 . ?
C85 C86 1.365(12) . ?
C86 H86 0.9500 . ?
C86 C87 1.437(11) . ?
C87 C88 1.411(11) . ?
C88 C89 1.493(11) . ?
C89 C90 1.449(11) . ?
C89 C98 1.353(11) . ?
C90 C91 1.418(12) . ?
C90 C95 1.415(11) . ?
C91 H91 0.9500 . ?
C91 C92 1.372(12) . ?
C92 H92 0.9500 . ?
C92 C93 1.407(13) . ?
C93 H93 0.9500 . ?
C93 C94 1.351(14) . ?
C94 H94 0.9500 . ?
C94 C95 1.427(12) . ?
C95 C96 1.426(14) . ?
C96 H96 0.9500 . ?
C96 C97 1.358(13) . ?
C97 H97 0.9500 . ?
C97 C98 1.414(11) . ?
C99 C100 1.3900 . ?
C99 C104 1.3900 . ?
C99 B4 1.609(11) . ?
C100 C101 1.3900 . ?
C101 C102 1.3900 . ?
C102 C103 1.3900 . ?
C103 C104 1.3900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
B1 O1 C7 123.5(7) . . ?
B1 O2 C27 130.2(7) . . ?
B2 O3 C26 133.5(7) . . ?
B2 O4 C46 124.7(7) . . ?
B3 O5 C79 131.9(7) . . ?
B3 O6 C59 123.8(7) . . ?
B4 O7 C98 122.7(7) . . ?
B4 O8 C78 131.9(7) . . ?
C2 C1 C6 120.0 . . ?
C2 C1 B1 121.4(5) . . ?
C6 C1 B1 118.6(5) . . ?
F1 C2 C1 120.7(4) . . ?
F1 C2 C3 119.3(4) . . ?
C3 C2 C1 120.0 . . ?
F2 C3 C2 119.5(5) . . ?
F2 C3 C4 120.5(5) . . ?
C2 C3 C4 120.0 . . ?
F3 C4 C3 119.3(5) . . ?
F3 C4 C5 120.7(5) . . ?
C5 C4 C3 120.0 . . ?
F4 C5 C4 119.9(5) . . ?
F4 C5 C6 120.1(5) . . ?
C4 C5 C6 120.0 . . ?
F5 C6 C1 121.6(4) . . ?
F5 C6 C5 118.4(4) . . ?
C5 C6 C1 120.0 . . ?
C8 C7 O1 115.1(7) . . ?
C16 C7 O1 120.7(7) . . ?
C16 C7 C8 124.0(8) . . ?
C7 C8 H8 120.9 . . ?
C9 C8 C7 118.2(9) . . ?
C9 C8 H8 120.9 . . ?
C8 C9 H9 119.1 . . ?
C8 C9 C10 121.7(9) . . ?
C10 C9 H9 119.1 . . ?
C11 C10 C9 122.4(9) . . ?
C11 C10 C15 119.2(9) . . ?
C15 C10 C9 118.4(8) . . ?
C10 C11 H11 119.1 . . ?
C12 C11 C10 121.8(10) . . ?
C12 C11 H11 119.1 . . ?
C11 C12 H12 120.6 . . ?
C11 C12 C13 118.7(9) . . ?
C13 C12 H12 120.6 . . ?
C12 C13 H13 119.5 . . ?
C14 C13 C12 121.0(10) . . ?
C14 C13 H13 119.5 . . ?
C13 C14 H14 119.5 . . ?
C13 C14 C15 121.1(9) . . ?
C15 C14 H14 119.5 . . ?
C10 C15 C14 118.2(8) . . ?
C10 C15 C16 119.8(8) . . ?
C14 C15 C16 122.1(8) . . ?
C7 C16 C15 117.7(7) . . ?
C7 C16 C17 123.2(8) . . ?
C15 C16 C17 118.8(8) . . ?
C18 C17 C16 121.5(8) . . ?
C26 C17 C16 119.5(8) . . ?
C26 C17 C18 119.0(8) . . ?
C19 C18 C17 121.4(8) . . ?
C19 C18 C23 119.9(8) . . ?
C23 C18 C17 118.7(8) . . ?
C18 C19 H19 120.7 . . ?
C20 C19 C18 118.7(8) . . ?
C20 C19 H19 120.7 . . ?
C19 C20 H20 119.3 . . ?
C19 C20 C21 121.3(9) . . ?
C21 C20 H20 119.3 . . ?
C20 C21 H21 119.3 . . ?
C22 C21 C20 121.3(9) . . ?
C22 C21 H21 119.3 . . ?
C21 C22 H22 120.3 . . ?
C21 C22 C23 119.5(8) . . ?
C23 C22 H22 120.3 . . ?
C22 C23 C18 119.2(8) . . ?
C24 C23 C18 118.9(8) . . ?
C24 C23 C22 121.9(8) . . ?
C23 C24 H24 119.0 . . ?
C25 C24 C23 122.0(8) . . ?
C25 C24 H24 119.0 . . ?
C24 C25 H25 120.6 . . ?
C24 C25 C26 118.8(8) . . ?
C26 C25 H25 120.6 . . ?
O3 C26 C25 121.1(8) . . ?
C17 C26 O3 116.1(7) . . ?
C17 C26 C25 122.6(8) . . ?
O2 C27 C28 121.7(7) . . ?
C36 C27 O2 116.2(7) . . ?
C36 C27 C28 122.0(8) . . ?
C27 C28 H28 120.6 . . ?
C29 C28 C27 118.7(8) . . ?
C29 C28 H28 120.6 . . ?
C28 C29 H29 118.6 . . ?
C28 C29 C30 122.8(8) . . ?
C30 C29 H29 118.6 . . ?
C29 C30 C35 118.3(8) . . ?
C31 C30 C29 123.7(8) . . ?
C31 C30 C35 117.9(8) . . ?
C30 C31 H31 118.7 . . ?
C32 C31 C30 122.7(8) . . ?
C32 C31 H31 118.7 . . ?
C31 C32 H32 120.5 . . ?
C31 C32 C33 119.1(9) . . ?
C33 C32 H32 120.5 . . ?
C32 C33 H33 120.1 . . ?
C34 C33 C32 119.9(9) . . ?
C34 C33 H33 120.1 . . ?
C33 C34 H34 119.0 . . ?
C33 C34 C35 122.0(8) . . ?
C35 C34 H34 119.0 . . ?
C34 C35 C30 118.5(8) . . ?
C34 C35 C36 123.0(7) . . ?
C36 C35 C30 118.4(7) . . ?
C27 C36 C35 119.7(7) . . ?
C27 C36 C37 118.4(8) . . ?
C35 C36 C37 121.9(7) . . ?
C38 C37 C36 119.9(7) . . ?
C46 C37 C36 121.3(7) . . ?
C46 C37 C38 118.7(7) . . ?
C39 C38 C37 122.3(7) . . ?
C39 C38 C43 119.2(7) . . ?
C43 C38 C37 118.6(7) . . ?
C38 C39 H39 119.6 . . ?
C40 C39 C38 120.9(8) . . ?
C40 C39 H39 119.6 . . ?
C39 C40 H40 119.8 . . ?
C39 C40 C41 120.4(9) . . ?
C41 C40 H40 119.8 . . ?
C40 C41 H41 119.8 . . ?
C42 C41 C40 120.4(8) . . ?
C42 C41 H41 119.8 . . ?
C41 C42 H42 119.3 . . ?
C41 C42 C43 121.5(8) . . ?
C43 C42 H42 119.3 . . ?
C42 C43 C38 117.5(8) . . ?
C44 C43 C38 120.2(8) . . ?
C44 C43 C42 122.3(8) . . ?
C43 C44 H44 119.7 . . ?
C45 C44 C43 120.6(8) . . ?
C45 C44 H44 119.7 . . ?
C44 C45 H45 120.1 . . ?
C44 C45 C46 119.7(8) . . ?
C46 C45 H45 120.1 . . ?
O4 C46 C45 118.1(7) . . ?
C37 C46 O4 119.9(7) . . ?
C37 C46 C45 121.9(7) . . ?
C48 C47 C52 112.9(8) . . ?
C48 C47 B2 123.8(8) . . ?
C52 C47 B2 123.3(8) . . ?
F6 C48 C47 117.6(8) . . ?
F6 C48 C49 118.3(8) . . ?
C49 C48 C47 124.2(9) . . ?
F7 C49 C48 120.6(10) . . ?
F7 C49 C50 120.1(9) . . ?
C50 C49 C48 119.3(9) . . ?
F8 C50 C51 119.1(9) . . ?
C49 C50 F8 120.9(9) . . ?
C49 C50 C51 120.0(9) . . ?
F9 C51 C50 119.3(8) . . ?
C52 C51 F9 121.5(9) . . ?
C52 C51 C50 119.2(9) . . ?
F10 C52 C47 117.3(7) . . ?
C51 C52 F10 118.3(8) . . ?
C51 C52 C47 124.4(9) . . ?
C54 C53 C58 120.0 . . ?
C54 C53 B3 120.8(5) . . ?
C58 C53 B3 118.9(5) . . ?
F11 C54 C53 121.1(4) . . ?
F11 C54 C55 118.9(4) . . ?
C55 C54 C53 120.0 . . ?
F12 C55 C54 120.9(4) . . ?
F12 C55 C56 119.1(5) . . ?
C54 C55 C56 120.0 . . ?
F13 C56 C55 120.1(5) . . ?
F13 C56 C57 119.9(5) . . ?
C55 C56 C57 120.0 . . ?
F14 C57 C56 119.7(5) . . ?
F14 C57 C58 120.3(5) . . ?
C58 C57 C56 120.0 . . ?
F15 C58 C53 121.0(4) . . ?
F15 C58 C57 119.0(4) . . ?
C57 C58 C53 120.0 . . ?
C60 C59 O6 115.3(7) . . ?
C68 C59 O6 121.7(7) . . ?
C68 C59 C60 123.1(8) . . ?
C59 C60 H60 120.6 . . ?
C61 C60 C59 118.8(8) . . ?
C61 C60 H60 120.6 . . ?
C60 C61 H61 119.4 . . ?
C60 C61 C62 121.2(8) . . ?
C62 C61 H61 119.4 . . ?
C61 C62 C63 122.4(8) . . ?
C61 C62 C67 119.1(7) . . ?
C67 C62 C63 118.5(8) . . ?
C62 C63 H63 119.6 . . ?
C64 C63 C62 120.7(8) . . ?
C64 C63 H63 119.6 . . ?
C63 C64 H64 119.7 . . ?
C63 C64 C65 120.6(9) . . ?
C65 C64 H64 119.7 . . ?
C64 C65 H65 119.2 . . ?
C66 C65 C64 121.6(9) . . ?
C66 C65 H65 119.2 . . ?
C65 C66 H66 120.0 . . ?
C65 C66 C67 120.0(9) . . ?
C67 C66 H66 120.0 . . ?
C66 C67 C62 118.5(8) . . ?
C68 C67 C62 120.2(7) . . ?
C68 C67 C66 121.3(7) . . ?
C59 C68 C67 117.6(7) . . ?
C59 C68 C69 121.2(7) . . ?
C67 C68 C69 121.1(7) . . ?
C70 C69 C68 122.1(7) . . ?
C78 C69 C68 119.2(7) . . ?
C78 C69 C70 118.7(7) . . ?
C69 C70 C71 122.2(7) . . ?
C69 C70 C75 120.0(7) . . ?
C75 C70 C71 117.9(7) . . ?
C70 C71 H71 119.3 . . ?
C72 C71 C70 121.4(7) . . ?
C72 C71 H71 119.3 . . ?
C71 C72 H72 119.9 . . ?
C71 C72 C73 120.2(8) . . ?
C73 C72 H72 119.9 . . ?
C72 C73 H73 119.9 . . ?
C74 C73 C72 120.2(8) . . ?
C74 C73 H73 119.9 . . ?
C73 C74 H74 119.3 . . ?
C73 C74 C75 121.3(8) . . ?
C75 C74 H74 119.3 . . ?
C70 C75 C74 119.0(8) . . ?
C76 C75 C70 118.8(8) . . ?
C76 C75 C74 122.2(7) . . ?
C75 C76 H76 119.3 . . ?
C77 C76 C75 121.4(7) . . ?
C77 C76 H76 119.3 . . ?
C76 C77 H77 120.4 . . ?
C76 C77 C78 119.2(8) . . ?
C78 C77 H77 120.4 . . ?
O8 C78 C77 121.6(8) . . ?
C69 C78 O8 116.3(7) . . ?
C69 C78 C77 121.9(8) . . ?
O5 C79 C80 121.1(8) . . ?
C88 C79 O5 115.4(7) . . ?
C88 C79 C80 123.4(8) . . ?
C79 C80 H80 120.7 . . ?
C81 C80 C79 118.5(8) . . ?
C81 C80 H80 120.7 . . ?
C80 C81 H81 119.2 . . ?
C80 C81 C82 121.6(7) . . ?
C82 C81 H81 119.2 . . ?
C81 C82 C83 121.7(7) . . ?
C81 C82 C87 117.4(8) . . ?
C83 C82 C87 120.8(8) . . ?
C82 C83 H83 119.9 . . ?
C84 C83 C82 120.2(8) . . ?
C84 C83 H83 119.9 . . ?
C83 C84 H84 119.9 . . ?
C83 C84 C85 120.1(8) . . ?
C85 C84 H84 119.9 . . ?
C84 C85 H85 119.7 . . ?
C86 C85 C84 120.6(9) . . ?
C86 C85 H85 119.7 . . ?
C85 C86 H86 119.1 . . ?
C85 C86 C87 121.8(8) . . ?
C87 C86 H86 119.1 . . ?
C82 C87 C86 116.5(8) . . ?
C88 C87 C82 121.3(8) . . ?
C88 C87 C86 122.2(7) . . ?
C79 C88 C87 117.7(7) . . ?
C79 C88 C89 120.1(7) . . ?
C87 C88 C89 122.2(8) . . ?
C90 C89 C88 118.6(7) . . ?
C98 C89 C88 122.8(7) . . ?
C98 C89 C90 118.4(8) . . ?
C91 C90 C89 121.0(7) . . ?
C95 C90 C89 119.4(8) . . ?
C95 C90 C91 119.6(8) . . ?
C90 C91 H91 120.1 . . ?
C92 C91 C90 119.9(8) . . ?
C92 C91 H91 120.1 . . ?
C91 C92 H92 119.5 . . ?
C91 C92 C93 121.1(9) . . ?
C93 C92 H92 119.5 . . ?
C92 C93 H93 120.1 . . ?
C94 C93 C92 119.7(9) . . ?
C94 C93 H93 120.1 . . ?
C93 C94 H94 119.1 . . ?
C93 C94 C95 121.8(9) . . ?
C95 C94 H94 119.1 . . ?
C90 C95 C94 118.0(9) . . ?
C90 C95 C96 118.8(8) . . ?
C96 C95 C94 123.2(8) . . ?
C95 C96 H96 119.4 . . ?
C97 C96 C95 121.1(8) . . ?
C97 C96 H96 119.4 . . ?
C96 C97 H97 120.3 . . ?
C96 C97 C98 119.3(9) . . ?
C98 C97 H97 120.3 . . ?
O7 C98 C97 115.9(7) . . ?
C89 C98 O7 121.2(7) . . ?
C89 C98 C97 122.9(8) . . ?
C100 C99 C104 120.0 . . ?
C100 C99 B4 119.4(5) . . ?
C104 C99 B4 120.6(5) . . ?
F16 C100 C99 120.7(4) . . ?
F16 C100 C101 119.3(4) . . ?
C101 C100 C99 120.0 . . ?
F17 C101 C100 120.5(4) . . ?
F17 C101 C102 119.5(4) . . ?
C102 C101 C100 120.0 . . ?
F18 C102 C101 120.1(4) . . ?
F18 C102 C103 119.9(4) . . ?
C101 C102 C103 120.0 . . ?
F19 C103 C102 118.9(4) . . ?
F19 C103 C104 121.1(4) . . ?
C102 C103 C104 120.0 . . ?
F20 C104 C99 121.6(4) . . ?
F20 C104 C103 118.4(4) . . ?
C103 C104 C99 120.0 . . ?
O1 B1 O2 117.4(8) . . ?
O1 B1 C1 118.1(8) . . ?
O2 B1 C1 124.6(8) . . ?
O3 B2 C47 125.5(8) . . ?
O4 B2 O3 117.0(8) . . ?
O4 B2 C47 117.5(8) . . ?
O5 B3 C53 122.8(8) . . ?
O6 B3 O5 118.7(8) . . ?
O6 B3 C53 118.5(8) . . ?
O7 B4 O8 118.4(8) . . ?
O7 B4 C99 117.5(8) . . ?
O8 B4 C99 124.0(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
F1 C2 C3 F2 -1.2(6) . . . . ?
F1 C2 C3 C4 179.1(6) . . . . ?
F2 C3 C4 F3 -1.0(6) . . . . ?
F2 C3 C4 C5 -179.7(6) . . . . ?
F3 C4 C5 F4 0.1(6) . . . . ?
F3 C4 C5 C6 -178.8(6) . . . . ?
F4 C5 C6 F5 2.0(6) . . . . ?
F4 C5 C6 C1 -178.9(7) . . . . ?
F6 C48 C49 F7 1.5(13) . . . . ?
F6 C48 C49 C50 179.7(8) . . . . ?
F7 C49 C50 F8 0.6(14) . . . . ?
F7 C49 C50 C51 -179.4(8) . . . . ?
F8 C50 C51 F9 -1.5(13) . . . . ?
F8 C50 C51 C52 177.3(8) . . . . ?
F9 C51 C52 F10 -0.2(13) . . . . ?
F9 C51 C52 C47 179.6(8) . . . . ?
F11 C54 C55 F12 1.1(6) . . . . ?
F11 C54 C55 C56 -178.9(5) . . . . ?
F12 C55 C56 F13 -0.5(6) . . . . ?
F12 C55 C56 C57 180.0(6) . . . . ?
F13 C56 C57 F14 -2.0(6) . . . . ?
F13 C56 C57 C58 -179.5(6) . . . . ?
F14 C57 C58 F15 1.1(6) . . . . ?
F14 C57 C58 C53 -177.6(6) . . . . ?
F16 C100 C101 F17 -0.4(6) . . . . ?
F16 C100 C101 C102 179.9(5) . . . . ?
F17 C101 C102 F18 2.0(6) . . . . ?
F17 C101 C102 C103 -179.8(6) . . . . ?
F18 C102 C103 F19 -1.1(6) . . . . ?
F18 C102 C103 C104 178.2(6) . . . . ?
F19 C103 C104 F20 -1.8(6) . . . . ?
F19 C103 C104 C99 179.3(5) . . . . ?
O1 C7 C8 C9 -179.6(8) . . . . ?
O1 C7 C16 C15 176.5(7) . . . . ?
O1 C7 C16 C17 -9.1(13) . . . . ?
O2 C27 C28 C29 178.4(8) . . . . ?
O2 C27 C36 C35 -179.0(7) . . . . ?
O2 C27 C36 C37 1.4(11) . . . . ?
O5 C79 C80 C81 179.9(7) . . . . ?
O5 C79 C88 C87 -178.9(7) . . . . ?
O5 C79 C88 C89 1.9(11) . . . . ?
O6 C59 C60 C61 -179.3(8) . . . . ?
O6 C59 C68 C67 176.7(7) . . . . ?
O6 C59 C68 C69 -5.7(12) . . . . ?
C1 C2 C3 F2 179.7(6) . . . . ?
C1 C2 C3 C4 0.0 . . . . ?
C2 C1 C6 F5 179.0(6) . . . . ?
C2 C1 C6 C5 0.0 . . . . ?
C2 C1 B1 O1 81.4(8) . . . . ?
C2 C1 B1 O2 -99.6(9) . . . . ?
C2 C3 C4 F3 178.8(6) . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
C3 C4 C5 F4 178.9(7) . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C4 C5 C6 F5 -179.1(6) . . . . ?
C4 C5 C6 C1 0.0 . . . . ?
C6 C1 C2 F1 -179.1(6) . . . . ?
C6 C1 C2 C3 0.0 . . . . ?
C6 C1 B1 O1 -99.1(8) . . . . ?
C6 C1 B1 O2 79.9(9) . . . . ?
C7 O1 B1 O2 -5.2(12) . . . . ?
C7 O1 B1 C1 173.8(7) . . . . ?
C7 C8 C9 C10 5.0(14) . . . . ?
C7 C16 C17 C18 80.5(11) . . . . ?
C7 C16 C17 C26 -99.9(11) . . . . ?
C8 C7 C16 C15 1.6(13) . . . . ?
C8 C7 C16 C17 176.0(8) . . . . ?
C8 C9 C10 C11 177.1(9) . . . . ?
C8 C9 C10 C15 -2.9(14) . . . . ?
C9 C10 C11 C12 -177.2(9) . . . . ?
C9 C10 C15 C14 178.0(8) . . . . ?
C9 C10 C15 C16 0.0(13) . . . . ?
C10 C11 C12 C13 -2.4(15) . . . . ?
C10 C15 C16 C7 0.6(12) . . . . ?
C10 C15 C16 C17 -174.1(8) . . . . ?
C11 C10 C15 C14 -2.0(13) . . . . ?
C11 C10 C15 C16 -180.0(8) . . . . ?
C11 C12 C13 C14 1.5(15) . . . . ?
C12 C13 C14 C15 -0.9(14) . . . . ?
C13 C14 C15 C10 1.1(13) . . . . ?
C13 C14 C15 C16 179.1(8) . . . . ?
C14 C15 C16 C7 -177.3(8) . . . . ?
C14 C15 C16 C17 8.0(12) . . . . ?
C15 C10 C11 C12 2.7(14) . . . . ?
C15 C16 C17 C18 -105.1(9) . . . . ?
C15 C16 C17 C26 74.4(11) . . . . ?
C16 C7 C8 C9 -4.4(14) . . . . ?
C16 C17 C18 C19 -0.7(13) . . . . ?
C16 C17 C18 C23 179.7(7) . . . . ?
C16 C17 C26 O3 4.1(11) . . . . ?
C16 C17 C26 C25 178.5(8) . . . . ?
C17 C18 C19 C20 179.2(8) . . . . ?
C17 C18 C23 C22 179.7(8) . . . . ?
C17 C18 C23 C24 0.4(12) . . . . ?
C18 C17 C26 O3 -176.3(7) . . . . ?
C18 C17 C26 C25 -2.0(13) . . . . ?
C18 C19 C20 C21 2.7(13) . . . . ?
C18 C23 C24 C25 0.9(13) . . . . ?
C19 C18 C23 C22 0.1(13) . . . . ?
C19 C18 C23 C24 -179.2(8) . . . . ?
C19 C20 C21 C22 -3.2(14) . . . . ?
C20 C21 C22 C23 2.0(13) . . . . ?
C21 C22 C23 C18 -0.5(13) . . . . ?
C21 C22 C23 C24 178.8(9) . . . . ?
C22 C23 C24 C25 -178.4(9) . . . . ?
C23 C18 C19 C20 -1.2(13) . . . . ?
C23 C24 C25 C26 -2.5(13) . . . . ?
C24 C25 C26 O3 177.2(8) . . . . ?
C24 C25 C26 C17 3.2(13) . . . . ?
C26 O3 B2 O4 -166.2(7) . . . . ?
C26 O3 B2 C47 16.2(15) . . . . ?
C26 C17 C18 C19 179.7(8) . . . . ?
C26 C17 C18 C23 0.2(12) . . . . ?
C27 O2 B1 O1 -178.5(7) . . . . ?
C27 O2 B1 C1 2.6(13) . . . . ?
C27 C28 C29 C30 0.6(13) . . . . ?
C27 C36 C37 C38 87.0(10) . . . . ?
C27 C36 C37 C46 -90.7(10) . . . . ?
C28 C27 C36 C35 -2.2(12) . . . . ?
C28 C27 C36 C37 178.1(7) . . . . ?
C28 C29 C30 C31 -179.5(8) . . . . ?
C28 C29 C30 C35 -2.6(13) . . . . ?
C29 C30 C31 C32 176.4(9) . . . . ?
C29 C30 C35 C34 -175.7(8) . . . . ?
C29 C30 C35 C36 2.1(11) . . . . ?
C30 C31 C32 C33 -1.4(14) . . . . ?
C30 C35 C36 C27 0.2(11) . . . . ?
C30 C35 C36 C37 179.8(7) . . . . ?
C31 C30 C35 C34 1.3(12) . . . . ?
C31 C30 C35 C36 179.2(7) . . . . ?
C31 C32 C33 C34 2.5(13) . . . . ?
C32 C33 C34 C35 -1.7(13) . . . . ?
C33 C34 C35 C30 -0.2(12) . . . . ?
C33 C34 C35 C36 -178.0(8) . . . . ?
C34 C35 C36 C27 178.0(8) . . . . ?
C34 C35 C36 C37 -2.4(12) . . . . ?
C35 C30 C31 C32 -0.5(13) . . . . ?
C35 C36 C37 C38 -92.7(10) . . . . ?
C35 C36 C37 C46 89.6(10) . . . . ?
C36 C27 C28 C29 1.9(13) . . . . ?
C36 C37 C38 C39 6.8(12) . . . . ?
C36 C37 C38 C43 -172.4(8) . . . . ?
C36 C37 C46 O4 -11.6(13) . . . . ?
C36 C37 C46 C45 172.6(8) . . . . ?
C37 C38 C39 C40 177.3(8) . . . . ?
C37 C38 C43 C42 -179.7(7) . . . . ?
C37 C38 C43 C44 -1.5(12) . . . . ?
C38 C37 C46 O4 170.7(7) . . . . ?
C38 C37 C46 C45 -5.1(13) . . . . ?
C38 C39 C40 C41 3.4(14) . . . . ?
C38 C43 C44 C45 -2.9(13) . . . . ?
C39 C38 C43 C42 1.1(12) . . . . ?
C39 C38 C43 C44 179.3(8) . . . . ?
C39 C40 C41 C42 -0.9(14) . . . . ?
C40 C41 C42 C43 -1.5(14) . . . . ?
C41 C42 C43 C38 1.4(13) . . . . ?
C41 C42 C43 C44 -176.8(8) . . . . ?
C42 C43 C44 C45 175.2(9) . . . . ?
C43 C38 C39 C40 -3.5(13) . . . . ?
C43 C44 C45 C46 3.3(14) . . . . ?
C44 C45 C46 O4 -175.1(8) . . . . ?
C44 C45 C46 C37 0.7(14) . . . . ?
C46 O4 B2 O3 6.8(12) . . . . ?
C46 O4 B2 C47 -175.4(7) . . . . ?
C46 C37 C38 C39 -175.4(8) . . . . ?
C46 C37 C38 C43 5.3(12) . . . . ?
C47 C48 C49 F7 -178.5(8) . . . . ?
C47 C48 C49 C50 -0.2(15) . . . . ?
C48 C47 C52 F10 -179.1(7) . . . . ?
C48 C47 C52 C51 1.1(13) . . . . ?
C48 C47 B2 O3 67.8(12) . . . . ?
C48 C47 B2 O4 -109.8(10) . . . . ?
C48 C49 C50 F8 -177.6(8) . . . . ?
C48 C49 C50 C51 2.4(14) . . . . ?
C49 C50 C51 F9 178.6(8) . . . . ?
C49 C50 C51 C52 -2.7(14) . . . . ?
C50 C51 C52 F10 -178.9(8) . . . . ?
C50 C51 C52 C47 0.9(14) . . . . ?
C52 C47 C48 F6 178.6(7) . . . . ?
C52 C47 C48 C49 -1.4(13) . . . . ?
C52 C47 B2 O3 -109.1(11) . . . . ?
C52 C47 B2 O4 73.3(11) . . . . ?
C53 C54 C55 F12 -180.0(6) . . . . ?
C53 C54 C55 C56 0.0 . . . . ?
C54 C53 C58 F15 -178.6(6) . . . . ?
C54 C53 C58 C57 0.0 . . . . ?
C54 C53 B3 O5 69.9(9) . . . . ?
C54 C53 B3 O6 -109.8(7) . . . . ?
C54 C55 C56 F13 179.5(6) . . . . ?
C54 C55 C56 C57 0.0 . . . . ?
C55 C56 C57 F14 177.6(6) . . . . ?
C55 C56 C57 C58 0.0 . . . . ?
C56 C57 C58 F15 178.6(6) . . . . ?
C56 C57 C58 C53 0.0 . . . . ?
C58 C53 C54 F11 178.8(5) . . . . ?
C58 C53 C54 C55 0.0 . . . . ?
C58 C53 B3 O5 -104.6(8) . . . . ?
C58 C53 B3 O6 75.7(8) . . . . ?
C59 O6 B3 O5 -1.4(12) . . . . ?
C59 O6 B3 C53 178.3(6) . . . . ?
C59 C60 C61 C62 2.4(14) . . . . ?
C59 C68 C69 C70 83.2(11) . . . . ?
C59 C68 C69 C78 -98.4(10) . . . . ?
C60 C59 C68 C67 -1.6(13) . . . . ?
C60 C59 C68 C69 175.9(8) . . . . ?
C60 C61 C62 C63 178.2(8) . . . . ?
C60 C61 C62 C67 -1.5(14) . . . . ?
C61 C62 C63 C64 -177.7(9) . . . . ?
C61 C62 C67 C66 179.8(8) . . . . ?
C61 C62 C67 C68 -1.0(13) . . . . ?
C62 C63 C64 C65 -2.1(15) . . . . ?
C62 C67 C68 C59 2.5(12) . . . . ?
C62 C67 C68 C69 -175.1(8) . . . . ?
C63 C62 C67 C66 0.1(12) . . . . ?
C63 C62 C67 C68 179.3(8) . . . . ?
C63 C64 C65 C66 0.1(15) . . . . ?
C64 C65 C66 C67 2.1(14) . . . . ?
C65 C66 C67 C62 -2.1(13) . . . . ?
C65 C66 C67 C68 178.8(8) . . . . ?
C66 C67 C68 C59 -178.4(8) . . . . ?
C66 C67 C68 C69 4.1(12) . . . . ?
C67 C62 C63 C64 2.0(13) . . . . ?
C67 C68 C69 C70 -99.3(10) . . . . ?
C67 C68 C69 C78 79.1(10) . . . . ?
C68 C59 C60 C61 -0.8(14) . . . . ?
C68 C69 C70 C71 1.2(12) . . . . ?
C68 C69 C70 C75 -178.6(7) . . . . ?
C68 C69 C78 O8 2.4(11) . . . . ?
C68 C69 C78 C77 176.9(8) . . . . ?
C69 C70 C71 C72 178.8(8) . . . . ?
C69 C70 C75 C74 -179.7(8) . . . . ?
C69 C70 C75 C76 -0.7(12) . . . . ?
C70 C69 C78 O8 -179.2(7) . . . . ?
C70 C69 C78 C77 -4.7(12) . . . . ?
C70 C71 C72 C73 2.2(13) . . . . ?
C70 C75 C76 C77 -0.2(13) . . . . ?
C71 C70 C75 C74 0.5(12) . . . . ?
C71 C70 C75 C76 179.5(7) . . . . ?
C71 C72 C73 C74 -2.0(13) . . . . ?
C72 C73 C74 C75 1.1(14) . . . . ?
C73 C74 C75 C70 -0.4(13) . . . . ?
C73 C74 C75 C76 -179.3(9) . . . . ?
C74 C75 C76 C77 178.8(9) . . . . ?
C75 C70 C71 C72 -1.4(12) . . . . ?
C75 C76 C77 C78 -1.3(13) . . . . ?
C76 C77 C78 O8 178.0(8) . . . . ?
C76 C77 C78 C69 3.8(13) . . . . ?
C78 O8 B4 O7 -172.1(7) . . . . ?
C78 O8 B4 C99 11.6(14) . . . . ?
C78 C69 C70 C71 -177.1(8) . . . . ?
C78 C69 C70 C75 3.1(12) . . . . ?
C79 O5 B3 O6 -171.3(7) . . . . ?
C79 O5 B3 C53 9.0(13) . . . . ?
C79 C80 C81 C82 -1.0(13) . . . . ?
C79 C88 C89 C90 77.5(11) . . . . ?
C79 C88 C89 C98 -97.2(10) . . . . ?
C80 C79 C88 C87 -1.5(12) . . . . ?
C80 C79 C88 C89 179.4(8) . . . . ?
C80 C81 C82 C83 -179.5(8) . . . . ?
C80 C81 C82 C87 -1.5(12) . . . . ?
C81 C82 C83 C84 178.9(8) . . . . ?
C81 C82 C87 C86 -178.9(7) . . . . ?
C81 C82 C87 C88 2.7(12) . . . . ?
C82 C83 C84 C85 -0.7(14) . . . . ?
C82 C87 C88 C79 -1.2(12) . . . . ?
C82 C87 C88 C89 177.9(7) . . . . ?
C83 C82 C87 C86 -0.9(12) . . . . ?
C83 C82 C87 C88 -179.3(8) . . . . ?
C83 C84 C85 C86 0.5(14) . . . . ?
C84 C85 C86 C87 -0.5(13) . . . . ?
C85 C86 C87 C82 0.7(12) . . . . ?
C85 C86 C87 C88 179.1(8) . . . . ?
C86 C87 C88 C79 -179.6(8) . . . . ?
C86 C87 C88 C89 -0.5(12) . . . . ?
C87 C82 C83 C84 0.9(13) . . . . ?
C87 C88 C89 C90 -101.6(9) . . . . ?
C87 C88 C89 C98 83.7(11) . . . . ?
C88 C79 C80 C81 2.6(13) . . . . ?
C88 C89 C90 C91 7.4(12) . . . . ?
C88 C89 C90 C95 -173.5(8) . . . . ?
C88 C89 C98 O7 -8.6(13) . . . . ?
C88 C89 C98 C97 174.2(8) . . . . ?
C89 C90 C91 C92 178.3(8) . . . . ?
C89 C90 C95 C94 -179.0(8) . . . . ?
C89 C90 C95 C96 -1.4(13) . . . . ?
C90 C89 C98 O7 176.7(7) . . . . ?
C90 C89 C98 C97 -0.5(13) . . . . ?
C90 C91 C92 C93 0.5(13) . . . . ?
C90 C95 C96 C97 0.4(14) . . . . ?
C91 C90 C95 C94 0.1(12) . . . . ?
C91 C90 C95 C96 177.7(8) . . . . ?
C91 C92 C93 C94 0.6(14) . . . . ?
C92 C93 C94 C95 -1.3(15) . . . . ?
C93 C94 C95 C90 1.0(14) . . . . ?
C93 C94 C95 C96 -176.5(9) . . . . ?
C94 C95 C96 C97 177.8(8) . . . . ?
C95 C90 C91 C92 -0.8(13) . . . . ?
C95 C96 C97 C98 0.6(14) . . . . ?
C96 C97 C98 O7 -177.8(8) . . . . ?
C96 C97 C98 C89 -0.5(14) . . . . ?
C98 O7 B4 O8 -1.4(12) . . . . ?
C98 O7 B4 C99 175.1(6) . . . . ?
C98 C89 C90 C91 -177.7(8) . . . . ?
C98 C89 C90 C95 1.4(12) . . . . ?
C99 C100 C101 F17 179.8(6) . . . . ?
C99 C100 C101 C102 0.0 . . . . ?
C100 C99 C104 F20 -178.8(6) . . . . ?
C100 C99 C104 C103 0.0 . . . . ?
C100 C99 B4 O7 -99.7(8) . . . . ?
C100 C99 B4 O8 76.6(9) . . . . ?
C100 C101 C102 F18 -178.2(6) . . . . ?
C100 C101 C102 C103 0.0 . . . . ?
C101 C102 C103 F19 -179.3(5) . . . . ?
C101 C102 C103 C104 0.0 . . . . ?
C102 C103 C104 F20 178.9(6) . . . . ?
C102 C103 C104 C99 0.0 . . . . ?
C104 C99 C100 F16 -179.9(5) . . . . ?
C104 C99 C100 C101 0.0 . . . . ?
C104 C99 B4 O7 79.5(8) . . . . ?
C104 C99 B4 O8 -104.2(8) . . . . ?
B1 O1 C7 C8 -106.6(9) . . . . ?
B1 O1 C7 C16 78.1(11) . . . . ?
B1 O2 C27 C28 41.7(12) . . . . ?
B1 O2 C27 C36 -141.6(8) . . . . ?
B1 C1 C2 F1 0.4(7) . . . . ?
B1 C1 C2 C3 179.5(6) . . . . ?
B1 C1 C6 F5 -0.5(7) . . . . ?
B1 C1 C6 C5 -179.5(6) . . . . ?
B2 O3 C26 C17 -171.5(9) . . . . ?
B2 O3 C26 C25 14.1(14) . . . . ?
B2 O4 C46 C37 82.9(10) . . . . ?
B2 O4 C46 C45 -101.2(10) . . . . ?
B2 C47 C48 F6 1.4(12) . . . . ?
B2 C47 C48 C49 -178.6(9) . . . . ?
B2 C47 C52 F10 -1.9(12) . . . . ?
B2 C47 C52 C51 178.3(9) . . . . ?
B3 O5 C79 C80 28.8(13) . . . . ?
B3 O5 C79 C88 -153.7(8) . . . . ?
B3 O6 C59 C60 -106.1(9) . . . . ?
B3 O6 C59 C68 75.4(11) . . . . ?
B3 C53 C54 F11 4.4(7) . . . . ?
B3 C53 C54 C55 -174.4(6) . . . . ?
B3 C53 C58 F15 -4.1(7) . . . . ?
B3 C53 C58 C57 174.5(6) . . . . ?
B4 O7 C98 C89 77.0(11) . . . . ?
B4 O7 C98 C97 -105.6(9) . . . . ?
B4 O8 C78 C69 -152.2(9) . . . . ?
B4 O8 C78 C77 33.3(13) . . . . ?
B4 C99 C100 F16 -0.6(7) . . . . ?
B4 C99 C100 C101 179.2(6) . . . . ?
B4 C99 C104 F20 1.9(7) . . . . ?
B4 C99 C104 C103 -179.2(6) . . . . ?

_olex2_exptl_crystal_mounting_method 'MiTeGen 200 micron MicroLoop'
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.5964(14)
2 0.4036(14)
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Benzene'
####################################################################### 
# 
# 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_R-8
_database_code_depnum_ccdc_archive 'CCDC 2068872'
loop_
_audit_author_name
_audit_author_address
'Daniel Unruh'
;Texas Tech University
United States of America
;
_audit_update_record             
;
2021-03-08 deposited with the CCDC.	2021-03-23 downloaded from the CCDC.
;

_audit_creation_date             2021-02-24
_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
loop_
_audit_author_email
Shipra.Garg@ttu.edu
daniel.unruh@ttu.edu
Clemens.krempner@ttu.edu
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C40 H24 B O4), 2(C5 H6 N), 6(C4 H8 O)'
_chemical_formula_sum            'C114 H108 B2 N2 O14'
_chemical_formula_weight         1751.64
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C120  H120  B6  N6  O12  '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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           1
_space_group_name_H-M_alt        'P 1'
_space_group_name_Hall           'P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'

_cell_length_a                   11.16170(10)
_cell_length_b                   14.9858(2)
_cell_length_c                   15.9416(2)
_cell_angle_alpha                65.7730(10)
_cell_angle_beta                 82.0400(10)
_cell_angle_gamma                68.4450(10)
_cell_volume                     2261.36(5)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    49385
_cell_measurement_temperature    99.9(4)
_cell_measurement_theta_max      76.9140
_cell_measurement_theta_min      3.0350
_shelx_estimated_absorpt_T_max   0.954
_shelx_estimated_absorpt_T_min   0.890
_exptl_absorpt_coefficient_mu    0.664
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.611
_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    1.286
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             928
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 9 7 0.0331
-1 -9 -7 0.0345
3 -7 -2 0.0581
-5 0 -6 0.0871
6 4 -4 0.0649
3 -4 5 0.0538
-2 -5 6 0.0578
-7 0 0 0.0960
-1 4 -6 0.0850
5 -3 -5 0.0602
2 -3 -9 0.0655
-6 -8 -3 0.0807
5 9 1 0.0620
0 8 -1 0.0755
0 -1 9 0.0488
7 2 -3 0.0680
7 6 1 0.0652

_exptl_crystal_recrystallization_method 
'Slow evaporation from a mixture of THF and pyridine'
_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.071
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.5634 8.8031 6.9525 -0.8449 -0.4602 -0.2727
-0.9228 -8.7943 -7.3252 0.8591 0.4679 0.2073
3.0448 -6.5929 -1.5494 0.4873 0.2665 0.8316
-5.3400 0.0578 -5.5921 0.2186 0.1174 -0.9687
5.7967 3.5609 -4.1563 -0.4668 0.8588 0.2110
2.9315 -3.5897 5.2000 0.1722 -0.3119 0.9344
-1.8845 -4.7128 6.1669 0.4210 -0.7713 0.4773
-6.8151 -0.3107 -0.3636 0.2553 -0.4732 -0.8432
-0.6780 4.3979 -6.0353 -0.3100 0.5660 -0.7639
4.7532 -3.4379 -5.4031 0.1884 0.7908 0.5824
2.3620 -2.6690 -9.2014 0.2324 0.9724 0.0192
-6.0060 -7.9658 -2.6109 0.9150 -0.3235 -0.2412
4.5277 8.9216 1.4845 -0.9399 0.3316 -0.0807
-0.3348 7.5898 -1.4781 -0.6382 0.2238 -0.7367
-0.0809 -0.6245 9.1409 -0.0201 -0.8483 0.5291
6.5304 1.6083 -3.1458 -0.3294 0.7915 0.5149
6.8963 5.9844 1.4505 -0.7618 0.4651 0.4509

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            66406
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.061
_diffrn_reflns_theta_max         67.061
_diffrn_reflns_theta_min         3.040
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -72.00  25.00   0.50    0.45    --  -47.95  81.00 145.00  194
  2  ω    -21.00  72.00   0.50    0.45    --   47.95 -81.00  23.00  186
  3  ω   -111.00 -13.00   0.50    1.80    --  -86.25  81.00 145.00  196
  4  ω   -159.00 -79.00   0.50    1.80    --  -86.25 -81.00  23.00  160
  5  ω    101.00 178.00   0.50    1.80    --  107.74  81.00 145.00  154
  6  ω     35.00 132.00   0.50    1.80    --  107.74 -81.00  23.00  194
  7  ω    -49.00 -17.00   0.50    0.45    --    2.00 132.00   0.75   64
  8  ω    -21.00  14.00   0.50    0.45    --   14.00 102.00 -72.06   70
  9  ω    -13.00  14.00   0.50    0.45    --   22.00 102.00-174.80   54
 10  ω      9.00  43.00   0.50    0.45    --   34.00  82.00  63.02   68
 11  ω      8.00  39.00   0.50    0.45    --   38.00  92.00  88.78   62
 12  ω     14.00  43.00   0.50    0.45    --   42.00  88.00 -22.02   58
 13  ω     17.00  43.00   0.50    0.45    --   46.00  90.00-179.86   52
 14  ω     17.00  43.00   0.50    0.45    --   46.00  90.00 -93.68   52
 15  ω    -41.00  25.00   0.50    0.45    --  -47.95  38.00-120.00  132
 16  ω     35.00 122.00   0.50    0.45    --   47.95  19.00  60.00  174
 17  ω     35.00 122.00   0.50    0.45    --   47.95  19.00-180.00  174
 18  ω     34.00  96.00   0.50    0.45    --   47.95-125.00  30.00  124
 19  ω   -122.00 -27.00   0.50    0.45    --  -50.00 -77.00-164.97  190
 20  ω   -126.00 -31.00   0.50    0.45    --  -54.00 -77.00 -34.19  190
 21  ω     31.00 126.00   0.50    0.45    --   54.00  77.00 -26.24  190
 22  ω     32.00 126.00   0.50    0.45    --   54.00  76.00 148.53  188
 23  ω   -131.00 -35.00   0.50    0.45    --  -58.00 -76.00 146.43  192
 24  ω   -131.00 -37.00   0.50    0.45    --  -58.00 -73.00-176.10  188
 25  ω   -131.00 -35.00   0.50    0.45    --  -58.00 -76.00-107.19  192
 26  ω     35.00 131.00   0.50    0.45    --   58.00  77.00  25.31  192
 27  ω     36.00 131.00   0.50    0.45    --   58.00  76.00  64.11  190
 28  ω    -67.00 -41.00   0.50    0.45    --  -62.00 -73.00 168.60   52
 29  ω    -73.00 -47.00   0.50    0.45    --  -66.00 -67.00  -0.37   52
 30  ω    -83.00 -46.00   0.50    0.45    --  -66.00 -70.00 -32.01   74
 31  ω     43.00  80.00   0.50    0.45    --   66.00  77.00  78.57   74
 32  ω    111.00 136.00   0.50    0.45    --   66.00  75.00 -38.68   50
 33  ω     43.00  78.00   0.50    0.45    --   66.00  77.00 133.21   70
 34  ω     45.00  71.00   0.50    0.45    --   66.00  75.00 -38.68   52
 35  ω     44.00  71.00   0.50    0.45    --   66.00  77.00 101.07   54
 36  ω     47.00  84.00   0.50    0.45    --   70.00  77.00 -26.16   74
 37  ω     49.00  75.00   0.50    0.45    --   70.00  75.00 116.07   52
 38  ω     47.00  73.00   0.50    0.45    --   70.00  77.00-135.25   52
 39  ω     48.00  85.00   0.50    0.45    --   70.00  75.00 -96.75   74
 40  ω    -82.00 -52.00   0.50    1.80    --  -74.00 -74.00 -85.26   60
 41  ω    -77.00 -52.00   0.50    1.80    --  -74.00 -75.00 -25.19   50
 42  ω    -77.00 -52.00   0.50    1.80    --  -74.00 -75.00  42.35   50
 43  ω   -140.00-114.00   0.50    1.80    --  -74.00 -75.00 -25.19   52
 44  ω    -84.00 -58.00   0.50    1.80    --  -78.00 -69.00 150.47   52
 45  ω    -83.00 -57.00   0.50    1.80    --  -78.00 -72.00 179.79   52
 46  ω    -82.00 -56.00   0.50    1.80    --  -78.00 -74.00  13.16   52
 47  ω    -89.00 -64.00   0.50    1.80    --  -86.00 -74.00-167.53   50
 48  ω    -93.00 -63.00   0.50    1.80    --  -86.00 -76.00  78.97   60
 49  ω   -155.00-129.00   0.50    1.80    --  -86.00 -76.00  78.97   52
 50  ω   -138.00-112.00   0.50    1.80    --  -86.25 -77.00 150.00   52
 51  ω   -102.00 -64.00   0.50    1.80    --  -86.25 -76.00  63.87   76
 52  ω   -142.00-116.00   0.50    1.80    --  -86.25 -76.00  63.87   52
 53  ω   -103.00 -65.00   0.50    1.80    --  -86.25 -76.00  47.46   76
 54  ω    -89.00 -63.00   0.50    1.80    --  -86.25 -77.00-180.00   52
 55  ω   -158.00-124.00   0.50    1.80    --  -86.25 -76.00  47.46   68
 56  ω    -93.00 -68.00   0.50    1.80    --  -86.25 -66.00 149.96   50
 57  ω   -157.00-107.00   0.50    1.80    --  -86.25 -66.00 149.96  100
 58  ω    -91.00 -65.00   0.50    1.80    --  -86.25 -77.00-120.00   52
 59  ω    -98.00 -64.00   0.50    1.80    --  -86.25 -75.00 126.89   68
 60  ω   -111.00 -65.00   0.50    1.80    --  -86.25 -74.00 109.24   92
 61  ω   -110.00 -65.00   0.50    1.80    --  -86.25 -74.00   5.51   90
 62  ω    -95.00 -68.00   0.50    1.80    --  -86.25 -66.00 -63.00   54
 63  ω   -151.00-126.00   0.50    1.80    --  -86.25 -66.00 -63.00   50
 64  ω   -105.00 -65.00   0.50    1.80    --  -86.25 -72.00-137.28   80
 65  ω    -89.00 -63.00   0.50    1.80    --  -86.25 -77.00 150.00   52
 66  ω    -91.00 -65.00   0.50    1.80    --  -86.25 -74.00 -99.37   52
 67  ω   -124.00 -99.00   0.50    1.80    --  -86.25 -66.00 -63.00   50
 68  ω    -97.00 -65.00   0.50    1.80    --  -86.25 -75.00-146.67   64
 69  ω   -102.00 -64.00   0.50    1.80    --  -86.25 -75.00 -11.74   76
 70  ω   -158.00 -64.00   0.50    1.80    --  -86.25 -76.00 -87.01  188
 71  ω    -97.00 -63.00   0.50    1.80    --  -86.25 -77.00 -30.00   68
 72  ω    -89.00 -64.00   0.50    1.80    --  -86.25 -75.00 -55.41   50
 73  ω    -96.00 -65.00   0.50    1.80    --  -86.25 -74.00  88.34   62
 74  ω   -155.00-110.00   0.50    1.80    --  -86.25 -77.00 -30.00   90
 75  ω     70.00 162.00   0.50    1.80    --   90.00  71.00 136.13  184
 76  ω     81.00 166.00   0.50    1.80    --   94.00  53.00  -1.33  170
 77  ω     72.00  98.00   0.50    1.80    --  107.74 -99.00-120.00   52
 78  ω     36.00  63.00   0.50    1.80    --  107.74 -99.00-120.00   54
 79  ω     36.00 106.00   0.50    1.80    --  107.74 -99.00-180.00  140
 80  ω     96.00 173.00   0.50    1.80    --  107.74  57.00  60.00  154
 81  ω     67.00 111.00   0.50    1.80    --  107.74-125.00-180.00   88
 82  ω     37.00 100.00   0.50    1.80    --  107.74 -77.00-180.00  126
 83  ω     85.00 177.00   0.50    1.80    --  107.74  77.00-120.00  184
 84  ω     35.00  61.00   0.50    1.80    --  107.74-125.00-180.00   52
 85  ω     75.00 101.00   0.50    1.80    --  107.74 -99.00 -30.00   52
 86  ω     38.00  72.00   0.50    1.80    --  107.74 -99.00 -30.00   68
 87  ω    101.00 174.00   0.50    1.80    --  107.74  57.00 -60.00  146
 88  ω     93.00 165.00   0.50    1.80    --  107.74  57.00-180.00  144
 89  ω     35.00 105.00   0.50    1.80    --  107.74 -99.00  30.00  140
 90  ω    141.00 177.00   0.50    1.80    --  107.74  77.00   0.00   72
 91  ω     85.00 134.00   0.50    1.80    --  107.74  77.00   0.00   98
 92  ω     36.00  63.00   0.50    1.80    --  107.74 -99.00  90.00   54
 93  ω     92.00 177.00   0.50    1.80    --  107.74  77.00-150.00  170
 94  ω     39.00 106.00   0.50    1.80    --  107.74 -99.00 120.00  134
 95  ω     81.00 111.00   0.50    1.80    --  107.74-125.00 -60.00   60
 96  ω     36.00 106.00   0.50    1.80    --  107.74 -99.00 -60.00  140
 97  ω    113.00 178.00   0.50    1.80    --  107.74  77.00  30.00  130
 98  ω     48.00  76.00   0.50    1.80    --  107.74-125.00 -60.00   56
 99  ω     89.00 173.00   0.50    1.80    --  107.74  77.00 -90.00  168
100  ω     86.00 164.00   0.50    1.80    --  107.74  77.00  90.00  156
101  ω     41.00  68.00   0.50    1.80    --  107.74 -57.00 -60.00   54
102  ω     86.00 173.00   0.50    1.80    --  107.74  77.00 150.00  174
103  ω    124.00 168.00   0.50    1.80    --  107.74  19.00-120.00   88
;
_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      -0.0330344000
_diffrn_orient_matrix_UB_12      -0.0871857000
_diffrn_orient_matrix_UB_13      -0.0084501000
_diffrn_orient_matrix_UB_21      0.0736079000
_diffrn_orient_matrix_UB_22      0.0149815000
_diffrn_orient_matrix_UB_23      -0.0911328000
_diffrn_orient_matrix_UB_31      0.1245711000
_diffrn_orient_matrix_UB_32      -0.0811569000
_diffrn_orient_matrix_UB_33      0.0534367000
_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         0.908
_reflns_Friedel_fraction_full    0.907
_reflns_Friedel_fraction_max     0.907
_reflns_number_gt                14396
_reflns_number_total             15364
_reflns_odcompleteness_completeness 99.86
_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         0.223
_refine_diff_density_min         -0.198
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details 
;
 Flack x determined using 6290 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1267
_refine_ls_number_reflns         15364
_refine_ls_number_restraints     513
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0367
_refine_ls_restrained_S_all      1.058
_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)+(0.0581P)²+0.2331P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.0966
_refine_special_details          
'A number of the interstitial THF molecules were positionally disordered and modeled as split sites. SIMU and RIGU restraints were applied to the disordered sites to help maintain reasonable ADP and bond length values. Details abot the site occupancies for disordered site can be found in the CIF.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
2. Restrained distances
 C101-C100 = C101-C115 = C99-C100 = C115-C116 = C107-C108 = C107-C118 = C108-
 C109 = C118-C117 = C110-C109 = C110-C117 = C114_$1-C113_$1 = C114_$1-C120_$1 =
 C112_$1-C113_$1 = C112_$1-C120_$1 = C111_$1-C112_$1 = C119_$1-C112_$1 = C106-
 C105 = C106-C121 = C104-C105 = C104-C121
 1.49962 with sigma of 0.02
 O11-C99 = O11-C102 = O11-C116 = O14A_$1-C114_$1 = O14B_$1-C114_$1 = O14A_$1-
 C111_$1 = O14B_$1-C119_$1
 1.44674 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O11 \\sim C100 \\sim C99 \\sim C101 \\sim C102 \\sim C115 \\sim C116: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O13 \\sim C107 \\sim C108 \\sim C109 \\sim C110 \\sim C117 \\sim C118: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O14B \\sim C111 \\sim C112 \\sim C113 \\sim C114 \\sim C119 \\sim O14A \\sim
C120: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
2A
C103 \\sim C104 \\sim C105 \\sim C121 \\sim C106 \\sim O12: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 O11, C100, C99, C101, C102, C115, C116
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O13, C107, C108, C109, C110, C117, C118
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O14B, C111, C112, C113, C114, C119, O14A, C120
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O12, C103, C104, C106, C105, C121
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(H10M)=Sof(H10N)=Sof(C115)=Sof(H11W)=Sof(H11X)=Sof(C116)=Sof(H11Y)=Sof(HC)=
 1-FVAR(1)
 Sof(C99)=Sof(H99A)=Sof(H99B)=Sof(C100)=Sof(H10I)=Sof(H10J)=Sof(H10K)=
 Sof(H10L)=FVAR(1)
 Sof(H10C)=Sof(H10D)=Sof(H11Q)=Sof(H11R)=Sof(C117)=Sof(H11S)=Sof(H11T)=
 Sof(C118)=Sof(H11U)=Sof(H11V)=1-FVAR(4)
 Sof(H10A)=Sof(H10B)=Sof(C108)=Sof(H10E)=Sof(H10F)=Sof(C109)=Sof(H10G)=
 Sof(H10H)=Sof(H11O)=Sof(H11P)=FVAR(4)
 Sof(H11E)=Sof(H11F)=Sof(H11K)=Sof(H11L)=Sof(O14B)=Sof(C119)=Sof(H11M)=
 Sof(H11N)=Sof(C120)=Sof(H12A)=Sof(H12B)=1-FVAR(5)
 Sof(O14A)=Sof(C111)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(H11D)=Sof(C113)=
 Sof(H11G)=Sof(H11H)=Sof(H11I)=Sof(H11J)=FVAR(5)
 Sof(H10U)=Sof(H10V)=Sof(HA)=Sof(HB)=Sof(C121)=Sof(H12C)=Sof(H12D)=1-FVAR(6)
 Sof(H10S)=Sof(H10T)=Sof(C105)=Sof(H10W)=Sof(H10X)=Sof(H10Y)=Sof(H)=FVAR(6)
6.a Secondary CH2 refined with riding coordinates:
 C91(H91A,H91B), C92(H92A,H92B), C93(H93A,H93B), C94(H94A,H94B), C107(H10A,
 H10B), C107(H10C,H10D), C108(H10E,H10F), C109(H10G,H10H), C110(H11O,H11P),
 C110(H11Q,H11R), C117(H11S,H11T), C118(H11U,H11V), C103(H10Q,H10R), C104(H10S,
 H10T), C104(H10U,H10V), C105(H10W,H10X), C106(H10Y,H), C106(HA,HB), C121(H12C,
 H12D), C95(H95A,H95B), C96(H96A,H96B), C97(H97A,H97B), C98(H98A,H98B),
 C99(H99A,H99B), C100(H10I,H10J), C101(H10K,H10L), C101(H10M,H10N), C102(H10O,
 H10P), C115(H11W,H11X), C116(H11Y,HC), C111(H11A,H11B), C112(H11C,H11D),
 C112(H11E,H11F), C113(H11G,H11H), C114(H11I,H11J), C114(H11K,H11L), C119(H11M,
 H11N), C120(H12A,H12B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14),
 C17(H17), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C27(H27), C28(H28),
  C29(H29), C30(H30), C33(H33), C34(H34), C37(H37), C38(H38), C39(H39),
 C40(H40), C43(H43), C44(H44), C47(H47), C48(H48), C49(H49), C50(H50), C53(H53),
  C54(H54), C57(H57), C58(H58), C59(H59), C60(H60), C63(H63), C64(H64),
 C67(H67), C68(H68), C69(H69), C70(H70), C73(H73), C74(H74), C77(H77), C78(H78),
  C79(H79), C80(H80), N2(H2), C86(H86), C87(H87), C88(H88), C89(H89), C90(H90),
 N1(H1), C81(H81), C82(H82), C83(H83), C84(H84), C85(H85)
;
_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 0.84178(16) 0.26015(13) 0.74884(12) 0.0235(4) Uani 1 1 d . . . . .
O2 O 0.62108(16) 0.38462(13) 0.73706(12) 0.0246(4) Uani 1 1 d . . . . .
O3 O 0.68049(16) 0.21747(13) 0.72075(12) 0.0239(4) Uani 1 1 d . . . . .
O4 O 0.71872(16) 0.37309(13) 0.60353(12) 0.0240(4) Uani 1 1 d . . . . .
C1 C 0.8311(2) 0.3638(2) 0.83233(17) 0.0230(5) Uani 1 1 d . . . . .
C2 C 0.8921(2) 0.31751(19) 0.77129(16) 0.0226(5) Uani 1 1 d . . . . .
C3 C 1.0128(2) 0.3230(2) 0.73387(17) 0.0250(5) Uani 1 1 d . . . . .
H3 H 1.056423 0.285413 0.696518 0.030 Uiso 1 1 calc R U . . .
C4 C 1.0668(2) 0.3818(2) 0.75104(18) 0.0268(5) Uani 1 1 d . . . . .
H4 H 1.149608 0.382666 0.727635 0.032 Uiso 1 1 calc R U . . .
C5 C 1.0009(2) 0.4419(2) 0.80353(17) 0.0265(5) Uani 1 1 d . . . . .
C6 C 0.8814(2) 0.4332(2) 0.84483(17) 0.0241(5) Uani 1 1 d . . . . .
C7 C 0.8146(3) 0.4971(2) 0.89369(18) 0.0267(5) Uani 1 1 d . . . . .
H7 H 0.736127 0.491224 0.922972 0.032 Uiso 1 1 calc R U . . .
C8 C 0.8612(3) 0.5676(2) 0.89950(19) 0.0309(6) Uani 1 1 d . . . . .
H8 H 0.813458 0.611243 0.930996 0.037 Uiso 1 1 calc R U . . .
C9 C 0.9798(3) 0.5755(2) 0.85887(19) 0.0336(6) Uani 1 1 d . . . . .
H9 H 1.012161 0.623654 0.863770 0.040 Uiso 1 1 calc R U . . .
C10 C 1.0474(3) 0.5140(2) 0.81272(18) 0.0303(6) Uani 1 1 d . . . . .
H10 H 1.127365 0.519337 0.786097 0.036 Uiso 1 1 calc R U . . .
C11 C 0.7142(2) 0.34217(19) 0.88090(17) 0.0239(5) Uani 1 1 d . . . . .
C12 C 0.6146(2) 0.35379(19) 0.83036(17) 0.0233(5) Uani 1 1 d . . . . .
C13 C 0.5004(2) 0.3376(2) 0.87328(19) 0.0267(5) Uani 1 1 d . . . . .
H13 H 0.431955 0.348015 0.837060 0.032 Uiso 1 1 calc R U . . .
C14 C 0.4878(2) 0.3072(2) 0.9663(2) 0.0291(6) Uani 1 1 d . . . . .
H14 H 0.409090 0.299828 0.993896 0.035 Uiso 1 1 calc R U . . .
C15 C 0.5906(3) 0.2865(2) 1.02222(19) 0.0295(6) Uani 1 1 d . . . . .
C16 C 0.7064(2) 0.3028(2) 0.97904(18) 0.0250(5) Uani 1 1 d . . . . .
C17 C 0.8118(3) 0.2730(2) 1.03752(18) 0.0280(6) Uani 1 1 d . . . . .
H17 H 0.890085 0.282179 1.010728 0.034 Uiso 1 1 calc R U . . .
C18 C 0.8032(3) 0.2314(2) 1.13114(19) 0.0333(6) Uani 1 1 d . . . . .
H18 H 0.875710 0.210956 1.168355 0.040 Uiso 1 1 calc R U . . .
C19 C 0.6872(3) 0.2187(2) 1.1730(2) 0.0379(7) Uani 1 1 d . . . . .
H19 H 0.681056 0.191202 1.238127 0.045 Uiso 1 1 calc R U . . .
C20 C 0.5841(3) 0.2461(2) 1.1194(2) 0.0355(6) Uani 1 1 d . . . . .
H20 H 0.506129 0.237837 1.147925 0.043 Uiso 1 1 calc R U . . .
C21 C 0.6047(2) 0.24817(19) 0.57527(18) 0.0234(5) Uani 1 1 d . . . . .
C22 C 0.5862(2) 0.22812(19) 0.66762(17) 0.0230(5) Uani 1 1 d . . . . .
C23 C 0.4705(3) 0.2151(2) 0.71113(19) 0.0272(5) Uani 1 1 d . . . . .
H23 H 0.461009 0.199035 0.775303 0.033 Uiso 1 1 calc R U . . .
C24 C 0.3728(2) 0.2255(2) 0.66119(19) 0.0284(6) Uani 1 1 d . . . . .
H24 H 0.296820 0.214481 0.691338 0.034 Uiso 1 1 calc R U . . .
C25 C 0.3832(2) 0.2523(2) 0.56535(19) 0.0268(5) Uani 1 1 d . . . . .
C26 C 0.5000(2) 0.2651(2) 0.52071(18) 0.0239(5) Uani 1 1 d . . . . .
C27 C 0.5052(3) 0.2974(2) 0.42381(19) 0.0275(6) Uani 1 1 d . . . . .
H27 H 0.580422 0.308925 0.392657 0.033 Uiso 1 1 calc R U . . .
C28 C 0.4040(3) 0.3122(2) 0.37434(19) 0.0312(6) Uani 1 1 d . . . . .
H28 H 0.410355 0.332833 0.309497 0.037 Uiso 1 1 calc R U . . .
C29 C 0.2901(3) 0.2972(2) 0.4185(2) 0.0333(6) Uani 1 1 d . . . . .
H29 H 0.220602 0.306941 0.383613 0.040 Uiso 1 1 calc R U . . .
C30 C 0.2804(3) 0.2686(2) 0.5116(2) 0.0312(6) Uani 1 1 d . . . . .
H30 H 0.203198 0.259417 0.540817 0.037 Uiso 1 1 calc R U . . .
C31 C 0.7296(2) 0.2576(2) 0.53288(17) 0.0228(5) Uani 1 1 d . . . . .
C32 C 0.7784(2) 0.32302(19) 0.54651(17) 0.0231(5) Uani 1 1 d . . . . .
C33 C 0.8873(2) 0.3446(2) 0.49823(18) 0.0275(5) Uani 1 1 d . . . . .
H33 H 0.917352 0.392061 0.506681 0.033 Uiso 1 1 calc R U . . .
C34 C 0.9495(2) 0.2972(2) 0.43942(18) 0.0291(6) Uani 1 1 d . . . . .
H34 H 1.019364 0.315228 0.404491 0.035 Uiso 1 1 calc R U . . .
C35 C 0.9109(2) 0.2215(2) 0.42984(17) 0.0266(5) Uani 1 1 d . . . . .
C36 C 0.8019(2) 0.1997(2) 0.47852(17) 0.0244(5) Uani 1 1 d . . . . .
C37 C 0.7701(3) 0.1191(2) 0.47254(19) 0.0289(6) Uani 1 1 d . . . . .
H37 H 0.698611 0.102227 0.505756 0.035 Uiso 1 1 calc R U . . .
C38 C 0.8398(3) 0.0652(2) 0.4202(2) 0.0335(6) Uani 1 1 d . . . . .
H38 H 0.817185 0.010847 0.418094 0.040 Uiso 1 1 calc R U . . .
C39 C 0.9452(3) 0.0899(2) 0.3691(2) 0.0342(6) Uani 1 1 d . . . . .
H39 H 0.991828 0.053864 0.331186 0.041 Uiso 1 1 calc R U . . .
C40 C 0.9802(3) 0.1659(2) 0.37433(19) 0.0319(6) Uani 1 1 d . . . . .
H40 H 1.051786 0.181659 0.340359 0.038 Uiso 1 1 calc R U . . .
B1 B 0.7157(3) 0.3108(2) 0.70147(19) 0.0225(6) Uani 1 1 d . . . . .
O5 O 0.12015(16) 0.86801(14) 0.21611(11) 0.0246(4) Uani 1 1 d . . . . .
O6 O 0.33955(16) 0.73990(13) 0.23811(11) 0.0231(4) Uani 1 1 d . . . . .
O7 O 0.18377(16) 0.70508(13) 0.19182(11) 0.0238(4) Uani 1 1 d . . . . .
O8 O 0.23455(16) 0.85997(13) 0.08769(11) 0.0232(4) Uani 1 1 d . . . . .
C41 C 0.2052(2) 0.83552(19) 0.35964(17) 0.0225(5) Uani 1 1 d . . . . .
C42 C 0.1088(2) 0.84354(19) 0.30796(17) 0.0230(5) Uani 1 1 d . . . . .
C43 C -0.0077(2) 0.8302(2) 0.34936(18) 0.0249(5) Uani 1 1 d . . . . .
H43 H -0.073814 0.838213 0.312447 0.030 Uiso 1 1 calc R U . . .
C44 C -0.0262(2) 0.8059(2) 0.44145(18) 0.0260(5) Uani 1 1 d . . . . .
H44 H -0.105919 0.799580 0.467662 0.031 Uiso 1 1 calc R U . . .
C45 C 0.0733(2) 0.7900(2) 0.49825(18) 0.0253(5) Uani 1 1 d . . . . .
C46 C 0.1906(2) 0.8038(2) 0.45747(17) 0.0242(5) Uani 1 1 d . . . . .
C47 C 0.2907(3) 0.7804(2) 0.51748(18) 0.0256(5) Uani 1 1 d . . . . .
H47 H 0.370605 0.787386 0.492374 0.031 Uiso 1 1 calc R U . . .
C48 C 0.2745(3) 0.7481(2) 0.61044(18) 0.0294(6) Uani 1 1 d . . . . .
H48 H 0.343307 0.732539 0.648934 0.035 Uiso 1 1 calc R U . . .
C49 C 0.1567(3) 0.7375(2) 0.65001(18) 0.0307(6) Uani 1 1 d . . . . .
H49 H 0.145572 0.716696 0.714605 0.037 Uiso 1 1 calc R U . . .
C50 C 0.0589(3) 0.7575(2) 0.59477(19) 0.0290(6) Uani 1 1 d . . . . .
H50 H -0.019984 0.749469 0.621512 0.035 Uiso 1 1 calc R U . . .
C51 C 0.3259(2) 0.85219(19) 0.31346(16) 0.0213(5) Uani 1 1 d . . . . .
C52 C 0.3906(2) 0.79839(19) 0.25832(16) 0.0214(5) Uani 1 1 d . . . . .
C53 C 0.5146(2) 0.7989(2) 0.22445(17) 0.0237(5) Uani 1 1 d . . . . .
H53 H 0.559967 0.757434 0.190609 0.028 Uiso 1 1 calc R U . . .
C54 C 0.5695(2) 0.8584(2) 0.23996(17) 0.0253(5) Uani 1 1 d . . . . .
H54 H 0.654713 0.854871 0.220049 0.030 Uiso 1 1 calc R U . . .
C55 C 0.5003(2) 0.9256(2) 0.28564(16) 0.0237(5) Uani 1 1 d . . . . .
C56 C 0.3767(2) 0.9231(2) 0.32247(16) 0.0234(5) Uani 1 1 d . . . . .
C57 C 0.3062(2) 0.9946(2) 0.36350(17) 0.0256(5) Uani 1 1 d . . . . .
H57 H 0.224590 0.993368 0.389441 0.031 Uiso 1 1 calc R U . . .
C58 C 0.3541(3) 1.0658(2) 0.36632(18) 0.0291(6) Uani 1 1 d . . . . .
H58 H 0.304010 1.114444 0.392405 0.035 Uiso 1 1 calc R U . . .
C59 C 0.4767(3) 1.0674(2) 0.33096(18) 0.0311(6) Uani 1 1 d . . . . .
H59 H 0.509354 1.116285 0.333893 0.037 Uiso 1 1 calc R U . . .
C60 C 0.5480(3) 0.9982(2) 0.29250(17) 0.0283(6) Uani 1 1 d . . . . .
H60 H 0.631252 0.998655 0.269869 0.034 Uiso 1 1 calc R U . . .
C61 C 0.1067(2) 0.75562(19) 0.04073(17) 0.0225(5) Uani 1 1 d . . . . .
C62 C 0.0881(2) 0.72653(19) 0.13459(17) 0.0227(5) Uani 1 1 d . . . . .
C63 C -0.0297(2) 0.7153(2) 0.17510(18) 0.0258(5) Uani 1 1 d . . . . .
H63 H -0.038274 0.691315 0.240035 0.031 Uiso 1 1 calc R U . . .
C64 C -0.1306(2) 0.7386(2) 0.12141(18) 0.0272(5) Uani 1 1 d . . . . .
H64 H -0.207999 0.728295 0.149341 0.033 Uiso 1 1 calc R U . . .
C65 C -0.1213(2) 0.7779(2) 0.02463(18) 0.0251(5) Uani 1 1 d . . . . .
C66 C -0.0015(2) 0.78661(19) -0.01683(17) 0.0227(5) Uani 1 1 d . . . . .
C67 C 0.0022(2) 0.8313(2) -0.11411(18) 0.0252(5) Uani 1 1 d . . . . .
H67 H 0.080376 0.838404 -0.143128 0.030 Uiso 1 1 calc R U . . .
C68 C -0.1042(3) 0.8646(2) -0.16740(19) 0.0298(6) Uani 1 1 d . . . . .
H68 H -0.098767 0.893889 -0.232532 0.036 Uiso 1 1 calc R U . . .
C69 C -0.2215(3) 0.8557(2) -0.12641(19) 0.0319(6) Uani 1 1 d . . . . .
H69 H -0.295236 0.879610 -0.163658 0.038 Uiso 1 1 calc R U . . .
C70 C -0.2289(2) 0.8124(2) -0.03243(19) 0.0291(6) Uani 1 1 d . . . . .
H70 H -0.307932 0.805414 -0.005121 0.035 Uiso 1 1 calc R U . . .
C71 C 0.2354(2) 0.7602(2) 0.00255(16) 0.0216(5) Uani 1 1 d . . . . .
C72 C 0.2924(2) 0.81411(19) 0.02741(16) 0.0217(5) Uani 1 1 d . . . . .
C73 C 0.4085(2) 0.8279(2) -0.01214(17) 0.0248(5) Uani 1 1 d . . . . .
H73 H 0.443774 0.867512 0.004187 0.030 Uiso 1 1 calc R U . . .
C74 C 0.4709(2) 0.7849(2) -0.07361(18) 0.0277(6) Uani 1 1 d . . . . .
H74 H 0.547311 0.797200 -0.101538 0.033 Uiso 1 1 calc R U . . .
C75 C 0.4226(2) 0.7220(2) -0.09624(17) 0.0249(5) Uani 1 1 d . . . . .
C76 C 0.3049(2) 0.7079(2) -0.05649(17) 0.0234(5) Uani 1 1 d . . . . .
C77 C 0.2641(2) 0.6389(2) -0.07602(18) 0.0260(5) Uani 1 1 d . . . . .
H77 H 0.186764 0.627083 -0.049883 0.031 Uiso 1 1 calc R U . . .
C78 C 0.3339(3) 0.5890(2) -0.13169(19) 0.0298(6) Uani 1 1 d . . . . .
H78 H 0.305276 0.542325 -0.142616 0.036 Uiso 1 1 calc R U . . .
C79 C 0.4475(3) 0.6063(2) -0.17279(19) 0.0311(6) Uani 1 1 d . . . . .
H79 H 0.494048 0.573064 -0.212738 0.037 Uiso 1 1 calc R U . . .
C80 C 0.4907(2) 0.6711(2) -0.15505(18) 0.0287(6) Uani 1 1 d . . . . .
H80 H 0.567754 0.682260 -0.182677 0.034 Uiso 1 1 calc R U . . .
B2 B 0.2196(3) 0.7939(2) 0.18338(19) 0.0217(5) Uani 1 1 d . . . . .
N2 N 0.3965(2) 0.54501(19) 0.40859(17) 0.0345(5) Uani 1 1 d . . . . .
H2 H 0.442359 0.551610 0.358226 0.041 Uiso 1 1 calc R U . . .
C86 C 0.2705(3) 0.5650(2) 0.4023(2) 0.0331(6) Uani 1 1 d . . . . .
H86 H 0.231689 0.585354 0.344897 0.040 Uiso 1 1 calc R U . . .
C87 C 0.1979(3) 0.5556(2) 0.4805(2) 0.0426(8) Uani 1 1 d . . . . .
H87 H 0.108223 0.567990 0.478920 0.051 Uiso 1 1 calc R U . . .
C88 C 0.2612(4) 0.5267(3) 0.5634(2) 0.0543(10) Uani 1 1 d . . . . .
H88 H 0.213374 0.521037 0.618329 0.065 Uiso 1 1 calc R U . . .
C89 C 0.3911(4) 0.5069(3) 0.5651(2) 0.0494(9) Uani 1 1 d . . . . .
H89 H 0.433912 0.487361 0.620786 0.059 Uiso 1 1 calc R U . . .
C90 C 0.4562(3) 0.5156(2) 0.4871(2) 0.0436(7) Uani 1 1 d . . . . .
H90 H 0.546613 0.500642 0.487642 0.052 Uiso 1 1 calc R U . . .
N1 N 0.7799(2) 0.08699(17) 0.89842(15) 0.0265(5) Uani 1 1 d . . . . .
H1 H 0.761418 0.115973 0.839190 0.032 Uiso 1 1 calc R U . . .
C81 C 0.6846(3) 0.0754(2) 0.95840(19) 0.0309(6) Uani 1 1 d . . . . .
H81 H 0.599297 0.097097 0.936713 0.037 Uiso 1 1 calc R U . . .
C82 C 0.7100(3) 0.0322(2) 1.0507(2) 0.0384(7) Uani 1 1 d . . . . .
H82 H 0.642822 0.024119 1.093646 0.046 Uiso 1 1 calc R U . . .
C83 C 0.8347(3) 0.0006(2) 1.0807(2) 0.0394(7) Uani 1 1 d . . . . .
H83 H 0.853514 -0.028670 1.144760 0.047 Uiso 1 1 calc R U . . .
C84 C 0.9322(3) 0.0115(2) 1.0178(2) 0.0362(7) Uani 1 1 d . . . . .
H84 H 1.018485 -0.011595 1.038142 0.043 Uiso 1 1 calc R U . . .
C85 C 0.9023(3) 0.0563(2) 0.9250(2) 0.0309(6) Uani 1 1 d . . . . .
H85 H 0.967683 0.065243 0.880538 0.037 Uiso 1 1 calc R U . . .
O9 O 0.1057(2) 0.06921(19) 0.74829(16) 0.0511(6) Uani 1 1 d . . . . .
C91 C 0.2284(3) -0.0105(2) 0.7596(2) 0.0335(6) Uani 1 1 d . . . . .
H91A H 0.243632 -0.059519 0.824796 0.040 Uiso 1 1 calc R U . . .
H91B H 0.297545 0.020240 0.740395 0.040 Uiso 1 1 calc R U . . .
C92 C 0.2272(3) -0.0668(2) 0.69932(19) 0.0328(6) Uani 1 1 d . . . . .
H92A H 0.197385 -0.126578 0.733814 0.039 Uiso 1 1 calc R U . . .
H92B H 0.313595 -0.091780 0.674324 0.039 Uiso 1 1 calc R U . . .
C93 C 0.1317(3) 0.0179(3) 0.6232(2) 0.0396(7) Uani 1 1 d . . . . .
H93A H 0.174689 0.060872 0.573143 0.048 Uiso 1 1 calc R U . . .
H93B H 0.088504 -0.012329 0.597163 0.048 Uiso 1 1 calc R U . . .
C94 C 0.0372(3) 0.0811(2) 0.6732(2) 0.0357(6) Uani 1 1 d . . . . .
H94A H 0.003020 0.155381 0.631275 0.043 Uiso 1 1 calc R U . . .
H94B H -0.035837 0.055307 0.695854 0.043 Uiso 1 1 calc R U . . .
O13 O 0.5604(2) 0.5341(2) 0.26395(16) 0.0564(6) Uani 1 1 d . U . . .
C107 C 0.5142(4) 0.5425(3) 0.1802(2) 0.0550(9) Uani 1 1 d D U . . .
H10A H 0.465000 0.615653 0.141516 0.066 Uiso 0.735(8) 1 calc R U P A 1
H10B H 0.459649 0.499203 0.192799 0.066 Uiso 0.735(8) 1 calc R U P A 1
H10C H 0.451839 0.505059 0.198014 0.066 Uiso 0.265(8) 1 calc R U P A 2
H10D H 0.464541 0.617026 0.146150 0.066 Uiso 0.265(8) 1 calc R U P A 2
C108 C 0.6432(7) 0.4999(6) 0.1344(4) 0.0585(16) Uani 0.735(8) 1 d D U P A 1
H10E H 0.632408 0.464419 0.096933 0.070 Uiso 0.735(8) 1 calc R U P A 1
H10F H 0.676208 0.556543 0.094971 0.070 Uiso 0.735(8) 1 calc R U P A 1
C109 C 0.7325(5) 0.4230(4) 0.2168(3) 0.0509(12) Uani 0.735(8) 1 d D U P A 1
H10G H 0.714275 0.357109 0.247366 0.061 Uiso 0.735(8) 1 calc R U P A 1
H10H H 0.824444 0.407809 0.199781 0.061 Uiso 0.735(8) 1 calc R U P A 1
C110 C 0.6958(3) 0.4840(3) 0.2728(3) 0.0530(8) Uani 1 1 d D U . . .
H11O H 0.720613 0.438273 0.337947 0.064 Uiso 0.735(8) 1 calc R U P A 1
H11P H 0.739285 0.536270 0.251497 0.064 Uiso 0.735(8) 1 calc R U P A 1
H11Q H 0.722016 0.408681 0.312200 0.064 Uiso 0.265(8) 1 calc R U P A 2
H11R H 0.739138 0.518424 0.293716 0.064 Uiso 0.265(8) 1 calc R U P A 2
C117 C 0.7146(16) 0.5089(15) 0.1568(11) 0.065(3) Uani 0.265(8) 1 d D U P A 2
H11S H 0.724805 0.577750 0.123737 0.078 Uiso 0.265(8) 1 calc R U P A 2
H11T H 0.793435 0.455430 0.147660 0.078 Uiso 0.265(8) 1 calc R U P A 2
C118 C 0.5981(16) 0.5078(18) 0.1172(13) 0.056(3) Uani 0.265(8) 1 d D U P A 2
H11U H 0.577932 0.557575 0.052526 0.067 Uiso 0.265(8) 1 calc R U P A 2
H11V H 0.605041 0.437348 0.124161 0.067 Uiso 0.265(8) 1 calc R U P A 2
O12 O 0.8790(2) 0.5836(2) 0.49538(18) 0.0514(6) Uani 1 1 d . U . . .
C103 C 0.8185(3) 0.5867(3) 0.5804(2) 0.0441(7) Uani 1 1 d . U . . .
H10Q H 0.840270 0.635290 0.597684 0.053 Uiso 1 1 calc R U . . .
H10R H 0.847853 0.516534 0.630461 0.053 Uiso 1 1 calc R U . . .
C104 C 0.6760(3) 0.6232(2) 0.5645(2) 0.0413(7) Uani 1 1 d D U . . .
H10S H 0.646196 0.563990 0.578643 0.050 Uiso 0.713(10) 1 calc R U P B 1
H10T H 0.627187 0.663636 0.601724 0.050 Uiso 0.713(10) 1 calc R U P B 1
H10U H 0.632045 0.692443 0.567479 0.050 Uiso 0.287(10) 1 calc R U P B 2
H10V H 0.637337 0.572998 0.609785 0.050 Uiso 0.287(10) 1 calc R U P B 2
C105 C 0.6633(4) 0.6897(4) 0.4652(3) 0.0357(11) Uani 0.713(10) 1 d D U P B 1
H10W H 0.660729 0.760428 0.453904 0.043 Uiso 0.713(10) 1 calc R U P B 1
H10X H 0.584644 0.695209 0.438503 0.043 Uiso 0.713(10) 1 calc R U P B 1
C106 C 0.7830(3) 0.6330(3) 0.4259(3) 0.0566(9) Uani 1 1 d D U . . .
H10Y H 0.767730 0.580768 0.409899 0.068 Uiso 0.713(10) 1 calc R U P B 1
H H 0.809315 0.682557 0.369838 0.068 Uiso 0.713(10) 1 calc R U P B 1
HA H 0.776479 0.706747 0.392425 0.068 Uiso 0.287(10) 1 calc R U P B 2
HB H 0.808721 0.598899 0.381388 0.068 Uiso 0.287(10) 1 calc R U P B 2
C121 C 0.6683(11) 0.6290(13) 0.4595(8) 0.046(2) Uani 0.287(10) 1 d D U P B 2
H12C H 0.655312 0.566490 0.461025 0.055 Uiso 0.287(10) 1 calc R U P B 2
H12D H 0.597947 0.692041 0.422821 0.055 Uiso 0.287(10) 1 calc R U P B 2
O10 O 0.6901(2) 0.84439(19) 0.58052(16) 0.0455(5) Uani 1 1 d . . . . .
C95 C 0.7126(3) 0.8750(3) 0.6490(2) 0.0385(7) Uani 1 1 d . . . . .
H95A H 0.783525 0.903685 0.630411 0.046 Uiso 1 1 calc R U . . .
H95B H 0.736502 0.814373 0.708465 0.046 Uiso 1 1 calc R U . . .
C96 C 0.5870(3) 0.9585(2) 0.6584(2) 0.0343(6) Uani 1 1 d . . . . .
H96A H 0.540829 0.929542 0.714908 0.041 Uiso 1 1 calc R U . . .
H96B H 0.603718 1.018549 0.659228 0.041 Uiso 1 1 calc R U . . .
C97 C 0.5114(3) 0.9895(2) 0.57267(19) 0.0315(6) Uani 1 1 d . . . . .
H97A H 0.417344 1.013459 0.582781 0.038 Uiso 1 1 calc R U . . .
H97B H 0.533264 1.044684 0.519406 0.038 Uiso 1 1 calc R U . . .
C98 C 0.5567(3) 0.8879(2) 0.5595(2) 0.0354(6) Uani 1 1 d . . . . .
H98A H 0.511271 0.840936 0.601375 0.043 Uiso 1 1 calc R U . . .
H98B H 0.541309 0.900354 0.495240 0.043 Uiso 1 1 calc R U . . .
O11 O 0.3822(2) 0.0972(2) 0.97952(18) 0.0595(7) Uani 1 1 d D U . . .
C99 C 0.2861(6) 0.1488(7) 0.9135(5) 0.0561(18) Uani 0.655(13) 1 d D U P C 1
H99A H 0.311102 0.124632 0.862324 0.067 Uiso 0.655(13) 1 calc R U P C 1
H99B H 0.268262 0.224862 0.888496 0.067 Uiso 0.655(13) 1 calc R U P C 1
C100 C 0.1698(5) 0.1235(5) 0.9614(3) 0.0351(14) Uani 0.655(13) 1 d D U P C 1
H10I H 0.170455 0.056690 0.962688 0.042 Uiso 0.655(13) 1 calc R U P C 1
H10J H 0.088946 0.179481 0.931574 0.042 Uiso 0.655(13) 1 calc R U P C 1
C101 C 0.1866(3) 0.1155(3) 1.0618(2) 0.0477(7) Uani 1 1 d D U . . .
H10K H 0.148210 0.184335 1.066198 0.057 Uiso 0.655(13) 1 calc R U P C 1
H10L H 0.148335 0.066090 1.108856 0.057 Uiso 0.655(13) 1 calc R U P C 1
H10M H 0.153753 0.056762 1.083210 0.057 Uiso 0.345(13) 1 calc R U P C 2
H10N H 0.147542 0.157416 1.099393 0.057 Uiso 0.345(13) 1 calc R U P C 2
C102 C 0.3314(3) 0.0750(3) 1.0706(2) 0.0429(7) Uani 1 1 d D U . . .
H10O H 0.359024 0.109676 1.101601 0.052 Uiso 1 1 calc R U . . .
H10P H 0.363111 -0.001015 1.107389 0.052 Uiso 1 1 calc R U . . .
C115 C 0.1570(10) 0.1743(12) 0.9729(7) 0.048(2) Uani 0.345(13) 1 d D U P C 2
H11W H 0.154003 0.246226 0.957303 0.058 Uiso 0.345(13) 1 calc R U P C 2
H11X H 0.072667 0.176949 0.957172 0.058 Uiso 0.345(13) 1 calc R U P C 2
C116 C 0.2633(13) 0.1212(12) 0.9234(9) 0.045(2) Uani 0.345(13) 1 d D U P C 2
H11Y H 0.267099 0.167663 0.858294 0.054 Uiso 0.345(13) 1 calc R U P C 2
HC H 0.254616 0.056603 0.926185 0.054 Uiso 0.345(13) 1 calc R U P C 2
O14A O 0.1376(5) 0.3418(3) 0.2394(2) 0.0545(12) Uani 0.616(5) 1 d . U P D 1
C111 C 0.0838(7) 0.4537(4) 0.2034(4) 0.0513(13) Uani 0.616(5) 1 d . U P D 1
H11A H 0.004420 0.476884 0.236585 0.062 Uiso 0.616(5) 1 calc R U P D 1
H11B H 0.146378 0.483075 0.210341 0.062 Uiso 0.616(5) 1 calc R U P D 1
C112 C 0.0558(4) 0.4866(3) 0.1096(3) 0.0587(9) Uani 1 1 d . U . . .
H11C H 0.073139 0.552099 0.073158 0.070 Uiso 0.616(5) 1 calc R U P D 1
H11D H -0.036191 0.499405 0.101333 0.070 Uiso 0.616(5) 1 calc R U P D 1
H11E H -0.022329 0.503887 0.145949 0.070 Uiso 0.384(5) 1 calc R U P D 2
H11F H 0.048263 0.545349 0.049338 0.070 Uiso 0.384(5) 1 calc R U P D 2
C113 C 0.1393(9) 0.4025(6) 0.0781(5) 0.069(2) Uani 0.616(5) 1 d . U P D 1
H11G H 0.090762 0.394283 0.035806 0.083 Uiso 0.616(5) 1 calc R U P D 1
H11H H 0.215585 0.418953 0.045727 0.083 Uiso 0.616(5) 1 calc R U P D 1
C114 C 0.1787(4) 0.3068(3) 0.1621(2) 0.0596(9) Uani 1 1 d . U . . .
H11I H 0.273237 0.271222 0.164083 0.071 Uiso 0.616(5) 1 calc R U P D 1
H11J H 0.136100 0.258248 0.164967 0.071 Uiso 0.616(5) 1 calc R U P D 1
H11K H 0.242566 0.265852 0.130123 0.071 Uiso 0.384(5) 1 calc R U P D 2
H11L H 0.140471 0.259074 0.211291 0.071 Uiso 0.384(5) 1 calc R U P D 2
O14B O 0.2438(9) 0.3440(5) 0.2033(5) 0.067(2) Uani 0.384(5) 1 d . U P D 2
C119 C 0.1856(12) 0.4554(8) 0.1647(8) 0.066(2) Uani 0.384(5) 1 d . U P D 2
H11M H 0.246177 0.486677 0.122337 0.080 Uiso 0.384(5) 1 calc R U P D 2
H11N H 0.164700 0.482089 0.214343 0.080 Uiso 0.384(5) 1 calc R U P D 2
C120 C 0.0810(16) 0.3849(9) 0.0990(11) 0.076(3) Uani 0.384(5) 1 d . U P D 2
H12A H 0.001560 0.366972 0.111504 0.091 Uiso 0.384(5) 1 calc R U P D 2
H12B H 0.108242 0.391861 0.035509 0.091 Uiso 0.384(5) 1 calc R U P D 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C2 1.358(3) . ?
O1 B1 1.472(3) . ?
O2 C12 1.364(3) . ?
O2 B1 1.467(3) . ?
O3 C22 1.365(3) . ?
O3 B1 1.490(3) . ?
O4 C32 1.363(3) . ?
O4 B1 1.457(3) . ?
C1 C2 1.384(4) . ?
C1 C6 1.438(3) . ?
C1 C11 1.494(3) . ?
C2 C3 1.413(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.360(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.419(4) . ?
C5 C6 1.429(3) . ?
C5 C10 1.422(4) . ?
C6 C7 1.417(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.376(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.414(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.361(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.381(4) . ?
C11 C16 1.430(4) . ?
C12 C13 1.414(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.364(4) . ?
C14 H14 0.9500 . ?
C14 C15 1.415(4) . ?
C15 C16 1.432(3) . ?
C15 C20 1.415(4) . ?
C16 C17 1.424(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.366(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.412(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.364(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.378(4) . ?
C21 C26 1.438(3) . ?
C21 C31 1.492(3) . ?
C22 C23 1.419(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.364(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.411(4) . ?
C25 C26 1.435(3) . ?
C25 C30 1.416(4) . ?
C26 C27 1.416(4) . ?
C27 H27 0.9500 . ?
C27 C28 1.365(4) . ?
C28 H28 0.9500 . ?
C28 C29 1.412(4) . ?
C29 H29 0.9500 . ?
C29 C30 1.365(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.381(3) . ?
C31 C36 1.437(3) . ?
C32 C33 1.414(3) . ?
C33 H33 0.9500 . ?
C33 C34 1.367(4) . ?
C34 H34 0.9500 . ?
C34 C35 1.419(4) . ?
C35 C36 1.419(3) . ?
C35 C40 1.421(4) . ?
C36 C37 1.418(4) . ?
C37 H37 0.9500 . ?
C37 C38 1.367(4) . ?
C38 H38 0.9500 . ?
C38 C39 1.412(4) . ?
C39 H39 0.9500 . ?
C39 C40 1.366(4) . ?
C40 H40 0.9500 . ?
O5 C42 1.355(3) . ?
O5 B2 1.465(3) . ?
O6 C52 1.359(3) . ?
O6 B2 1.468(3) . ?
O7 C62 1.361(3) . ?
O7 B2 1.477(3) . ?
O8 C72 1.363(3) . ?
O8 B2 1.465(3) . ?
C41 C42 1.385(4) . ?
C41 C46 1.436(3) . ?
C41 C51 1.497(3) . ?
C42 C43 1.419(3) . ?
C43 H43 0.9500 . ?
C43 C44 1.365(4) . ?
C44 H44 0.9500 . ?
C44 C45 1.420(4) . ?
C45 C46 1.425(3) . ?
C45 C50 1.416(4) . ?
C46 C47 1.421(4) . ?
C47 H47 0.9500 . ?
C47 C48 1.365(4) . ?
C48 H48 0.9500 . ?
C48 C49 1.411(4) . ?
C49 H49 0.9500 . ?
C49 C50 1.367(4) . ?
C50 H50 0.9500 . ?
C51 C52 1.387(3) . ?
C51 C56 1.435(3) . ?
C52 C53 1.416(3) . ?
C53 H53 0.9500 . ?
C53 C54 1.361(4) . ?
C54 H54 0.9500 . ?
C54 C55 1.420(4) . ?
C55 C56 1.430(3) . ?
C55 C60 1.422(4) . ?
C56 C57 1.418(4) . ?
C57 H57 0.9500 . ?
C57 C58 1.375(4) . ?
C58 H58 0.9500 . ?
C58 C59 1.411(4) . ?
C59 H59 0.9500 . ?
C59 C60 1.365(4) . ?
C60 H60 0.9500 . ?
C61 C62 1.385(3) . ?
C61 C66 1.436(3) . ?
C61 C71 1.495(3) . ?
C62 C63 1.419(3) . ?
C63 H63 0.9500 . ?
C63 C64 1.362(4) . ?
C64 H64 0.9500 . ?
C64 C65 1.412(4) . ?
C65 C66 1.433(3) . ?
C65 C70 1.413(4) . ?
C66 C67 1.416(4) . ?
C67 H67 0.9500 . ?
C67 C68 1.371(4) . ?
C68 H68 0.9500 . ?
C68 C69 1.406(4) . ?
C69 H69 0.9500 . ?
C69 C70 1.371(4) . ?
C70 H70 0.9500 . ?
C71 C72 1.388(3) . ?
C71 C76 1.435(3) . ?
C72 C73 1.408(3) . ?
C73 H73 0.9500 . ?
C73 C74 1.363(4) . ?
C74 H74 0.9500 . ?
C74 C75 1.419(4) . ?
C75 C76 1.427(3) . ?
C75 C80 1.415(4) . ?
C76 C77 1.423(3) . ?
C77 H77 0.9500 . ?
C77 C78 1.370(4) . ?
C78 H78 0.9500 . ?
C78 C79 1.406(4) . ?
C79 H79 0.9500 . ?
C79 C80 1.364(4) . ?
C80 H80 0.9500 . ?
N2 H2 0.8800 . ?
N2 C86 1.336(4) . ?
N2 C90 1.330(4) . ?
C86 H86 0.9500 . ?
C86 C87 1.375(4) . ?
C87 H87 0.9500 . ?
C87 C88 1.413(5) . ?
C88 H88 0.9500 . ?
C88 C89 1.371(6) . ?
C89 H89 0.9500 . ?
C89 C90 1.333(5) . ?
C90 H90 0.9500 . ?
N1 H1 0.8800 . ?
N1 C81 1.340(3) . ?
N1 C85 1.340(4) . ?
C81 H81 0.9500 . ?
C81 C82 1.365(4) . ?
C82 H82 0.9500 . ?
C82 C83 1.380(5) . ?
C83 H83 0.9500 . ?
C83 C84 1.382(5) . ?
C84 H84 0.9500 . ?
C84 C85 1.382(4) . ?
C85 H85 0.9500 . ?
O9 C91 1.423(4) . ?
O9 C94 1.424(4) . ?
C91 H91A 0.9900 . ?
C91 H91B 0.9900 . ?
C91 C92 1.521(4) . ?
C92 H92A 0.9900 . ?
C92 H92B 0.9900 . ?
C92 C93 1.523(4) . ?
C93 H93A 0.9900 . ?
C93 H93B 0.9900 . ?
C93 C94 1.515(4) . ?
C94 H94A 0.9900 . ?
C94 H94B 0.9900 . ?
O13 C107 1.440(4) . ?
O13 C110 1.416(4) . ?
C107 H10A 0.9900 . ?
C107 H10B 0.9900 . ?
C107 H10C 0.9900 . ?
C107 H10D 0.9900 . ?
C107 C108 1.559(7) . ?
C107 C118 1.402(16) . ?
C108 H10E 0.9900 . ?
C108 H10F 0.9900 . ?
C108 C109 1.525(8) . ?
C109 H10G 0.9900 . ?
C109 H10H 0.9900 . ?
C109 C110 1.446(6) . ?
C110 H11O 0.9900 . ?
C110 H11P 0.9900 . ?
C110 H11Q 0.9900 . ?
C110 H11R 0.9900 . ?
C110 C117 1.729(15) . ?
C117 H11S 0.9900 . ?
C117 H11T 0.9900 . ?
C117 C118 1.529(19) . ?
C118 H11U 0.9900 . ?
C118 H11V 0.9900 . ?
O12 C103 1.438(4) . ?
O12 C106 1.413(5) . ?
C103 H10Q 0.9900 . ?
C103 H10R 0.9900 . ?
C103 C104 1.501(5) . ?
C104 H10S 0.9900 . ?
C104 H10T 0.9900 . ?
C104 H10U 0.9900 . ?
C104 H10V 0.9900 . ?
C104 C105 1.477(5) . ?
C104 C121 1.652(12) . ?
C105 H10W 0.9900 . ?
C105 H10X 0.9900 . ?
C105 C106 1.507(6) . ?
C106 H10Y 0.9900 . ?
C106 H 0.9900 . ?
C106 HA 0.9900 . ?
C106 HB 0.9900 . ?
C106 C121 1.330(11) . ?
C121 H12C 0.9900 . ?
C121 H12D 0.9900 . ?
O10 C95 1.428(3) . ?
O10 C98 1.415(4) . ?
C95 H95A 0.9900 . ?
C95 H95B 0.9900 . ?
C95 C96 1.536(4) . ?
C96 H96A 0.9900 . ?
C96 H96B 0.9900 . ?
C96 C97 1.518(4) . ?
C97 H97A 0.9900 . ?
C97 H97B 0.9900 . ?
C97 C98 1.512(4) . ?
C98 H98A 0.9900 . ?
C98 H98B 0.9900 . ?
O11 C99 1.375(7) . ?
O11 C102 1.433(4) . ?
O11 C116 1.551(13) . ?
C99 H99A 0.9900 . ?
C99 H99B 0.9900 . ?
C99 C100 1.505(7) . ?
C100 H10I 0.9900 . ?
C100 H10J 0.9900 . ?
C100 C101 1.587(6) . ?
C101 H10K 0.9900 . ?
C101 H10L 0.9900 . ?
C101 H10M 0.9900 . ?
C101 H10N 0.9900 . ?
C101 C102 1.508(5) . ?
C101 C115 1.337(11) . ?
C102 H10O 0.9900 . ?
C102 H10P 0.9900 . ?
C115 H11W 0.9900 . ?
C115 H11X 0.9900 . ?
C115 C116 1.492(16) . ?
C116 H11Y 0.9900 . ?
C116 HC 0.9900 . ?
O14A C111 1.438(7) . ?
O14A C114 1.482(5) . ?
C111 H11A 0.9900 . ?
C111 H11B 0.9900 . ?
C111 C112 1.410(7) . ?
C112 H11C 0.9900 . ?
C112 H11D 0.9900 . ?
C112 H11E 0.9900 . ?
C112 H11F 0.9900 . ?
C112 C113 1.496(8) . ?
C112 C119 1.615(11) . ?
C112 C120 1.520(13) . ?
C113 H11G 0.9900 . ?
C113 H11H 0.9900 . ?
C113 C114 1.472(8) . ?
C114 H11I 0.9900 . ?
C114 H11J 0.9900 . ?
C114 H11K 0.9900 . ?
C114 H11L 0.9900 . ?
C114 O14B 1.413(8) . ?
C114 C120 1.405(13) . ?
O14B C119 1.434(12) . ?
C119 H11M 0.9900 . ?
C119 H11N 0.9900 . ?
C120 H12A 0.9900 . ?
C120 H12B 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
C2 O1 B1 119.35(19) . . ?
C12 O2 B1 116.84(19) . . ?
C22 O3 B1 117.99(19) . . ?
C32 O4 B1 118.39(19) . . ?
C2 C1 C6 118.4(2) . . ?
C2 C1 C11 119.1(2) . . ?
C6 C1 C11 122.5(2) . . ?
O1 C2 C1 121.4(2) . . ?
O1 C2 C3 117.2(2) . . ?
C1 C2 C3 121.3(2) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 C2 120.4(2) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 H4 119.6 . . ?
C3 C4 C5 120.7(2) . . ?
C5 C4 H4 119.6 . . ?
C4 C5 C6 119.1(2) . . ?
C4 C5 C10 121.8(2) . . ?
C10 C5 C6 119.0(2) . . ?
C5 C6 C1 119.2(2) . . ?
C7 C6 C1 122.5(2) . . ?
C7 C6 C5 118.2(2) . . ?
C6 C7 H7 119.4 . . ?
C8 C7 C6 121.2(2) . . ?
C8 C7 H7 119.4 . . ?
C7 C8 H8 119.8 . . ?
C7 C8 C9 120.4(2) . . ?
C9 C8 H8 119.8 . . ?
C8 C9 H9 120.1 . . ?
C10 C9 C8 119.8(2) . . ?
C10 C9 H9 120.1 . . ?
C5 C10 H10 119.3 . . ?
C9 C10 C5 121.4(2) . . ?
C9 C10 H10 119.3 . . ?
C12 C11 C1 119.3(2) . . ?
C12 C11 C16 118.9(2) . . ?
C16 C11 C1 121.7(2) . . ?
O2 C12 C11 121.2(2) . . ?
O2 C12 C13 117.7(2) . . ?
C11 C12 C13 121.0(2) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 C12 120.5(2) . . ?
C14 C13 H13 119.7 . . ?
C13 C14 H14 119.6 . . ?
C13 C14 C15 120.8(2) . . ?
C15 C14 H14 119.6 . . ?
C14 C15 C16 118.8(2) . . ?
C14 C15 C20 121.8(2) . . ?
C20 C15 C16 119.3(3) . . ?
C11 C16 C15 119.6(2) . . ?
C17 C16 C11 123.0(2) . . ?
C17 C16 C15 117.3(2) . . ?
C16 C17 H17 119.1 . . ?
C18 C17 C16 121.7(2) . . ?
C18 C17 H17 119.1 . . ?
C17 C18 H18 119.8 . . ?
C17 C18 C19 120.4(3) . . ?
C19 C18 H18 119.8 . . ?
C18 C19 H19 120.2 . . ?
C20 C19 C18 119.6(3) . . ?
C20 C19 H19 120.2 . . ?
C15 C20 H20 119.3 . . ?
C19 C20 C15 121.5(3) . . ?
C19 C20 H20 119.3 . . ?
C22 C21 C26 119.0(2) . . ?
C22 C21 C31 119.6(2) . . ?
C26 C21 C31 121.3(2) . . ?
O3 C22 C21 120.8(2) . . ?
O3 C22 C23 117.8(2) . . ?
C21 C22 C23 121.3(2) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 C22 120.3(2) . . ?
C24 C23 H23 119.9 . . ?
C23 C24 H24 119.6 . . ?
C23 C24 C25 120.9(2) . . ?
C25 C24 H24 119.6 . . ?
C24 C25 C26 119.3(2) . . ?
C24 C25 C30 121.7(2) . . ?
C30 C25 C26 118.9(2) . . ?
C25 C26 C21 119.0(2) . . ?
C27 C26 C21 122.9(2) . . ?
C27 C26 C25 118.0(2) . . ?
C26 C27 H27 119.4 . . ?
C28 C27 C26 121.2(2) . . ?
C28 C27 H27 119.4 . . ?
C27 C28 H28 119.6 . . ?
C27 C28 C29 120.7(3) . . ?
C29 C28 H28 119.6 . . ?
C28 C29 H29 120.2 . . ?
C30 C29 C28 119.7(2) . . ?
C30 C29 H29 120.2 . . ?
C25 C30 H30 119.3 . . ?
C29 C30 C25 121.3(2) . . ?
C29 C30 H30 119.3 . . ?
C32 C31 C21 119.5(2) . . ?
C32 C31 C36 118.6(2) . . ?
C36 C31 C21 121.9(2) . . ?
O4 C32 C31 120.7(2) . . ?
O4 C32 C33 117.9(2) . . ?
C31 C32 C33 121.2(2) . . ?
C32 C33 H33 120.0 . . ?
C34 C33 C32 120.1(2) . . ?
C34 C33 H33 120.0 . . ?
C33 C34 H34 119.6 . . ?
C33 C34 C35 120.9(2) . . ?
C35 C34 H34 119.6 . . ?
C34 C35 C40 121.7(2) . . ?
C36 C35 C34 119.0(2) . . ?
C36 C35 C40 119.3(2) . . ?
C35 C36 C31 119.6(2) . . ?
C37 C36 C31 122.5(2) . . ?
C37 C36 C35 117.9(2) . . ?
C36 C37 H37 119.2 . . ?
C38 C37 C36 121.6(2) . . ?
C38 C37 H37 119.2 . . ?
C37 C38 H38 119.9 . . ?
C37 C38 C39 120.2(3) . . ?
C39 C38 H38 119.9 . . ?
C38 C39 H39 120.1 . . ?
C40 C39 C38 119.9(2) . . ?
C40 C39 H39 120.1 . . ?
C35 C40 H40 119.5 . . ?
C39 C40 C35 121.0(2) . . ?
C39 C40 H40 119.5 . . ?
O1 B1 O3 100.1(2) . . ?
O2 B1 O1 113.6(2) . . ?
O2 B1 O3 112.52(19) . . ?
O4 B1 O1 114.6(2) . . ?
O4 B1 O2 103.4(2) . . ?
O4 B1 O3 113.1(2) . . ?
C42 O5 B2 118.6(2) . . ?
C52 O6 B2 117.81(19) . . ?
C62 O7 B2 116.56(19) . . ?
C72 O8 B2 119.00(19) . . ?
C42 C41 C46 118.9(2) . . ?
C42 C41 C51 119.3(2) . . ?
C46 C41 C51 121.5(2) . . ?
O5 C42 C41 121.6(2) . . ?
O5 C42 C43 117.7(2) . . ?
C41 C42 C43 120.7(2) . . ?
C42 C43 H43 119.5 . . ?
C44 C43 C42 121.0(2) . . ?
C44 C43 H43 119.5 . . ?
C43 C44 H44 119.9 . . ?
C43 C44 C45 120.3(2) . . ?
C45 C44 H44 119.9 . . ?
C44 C45 C46 119.3(2) . . ?
C50 C45 C44 120.8(2) . . ?
C50 C45 C46 119.9(2) . . ?
C45 C46 C41 119.5(2) . . ?
C47 C46 C41 123.0(2) . . ?
C47 C46 C45 117.4(2) . . ?
C46 C47 H47 119.3 . . ?
C48 C47 C46 121.5(2) . . ?
C48 C47 H47 119.3 . . ?
C47 C48 H48 119.6 . . ?
C47 C48 C49 120.8(3) . . ?
C49 C48 H48 119.6 . . ?
C48 C49 H49 120.2 . . ?
C50 C49 C48 119.6(2) . . ?
C50 C49 H49 120.2 . . ?
C45 C50 H50 119.5 . . ?
C49 C50 C45 120.9(2) . . ?
C49 C50 H50 119.5 . . ?
C52 C51 C41 118.9(2) . . ?
C52 C51 C56 118.3(2) . . ?
C56 C51 C41 122.8(2) . . ?
O6 C52 C51 121.1(2) . . ?
O6 C52 C53 117.7(2) . . ?
C51 C52 C53 121.1(2) . . ?
C52 C53 H53 119.7 . . ?
C54 C53 C52 120.6(2) . . ?
C54 C53 H53 119.7 . . ?
C53 C54 H54 119.7 . . ?
C53 C54 C55 120.6(2) . . ?
C55 C54 H54 119.7 . . ?
C54 C55 C56 119.0(2) . . ?
C54 C55 C60 121.9(2) . . ?
C60 C55 C56 119.1(2) . . ?
C55 C56 C51 119.5(2) . . ?
C57 C56 C51 122.3(2) . . ?
C57 C56 C55 118.1(2) . . ?
C56 C57 H57 119.5 . . ?
C58 C57 C56 121.0(2) . . ?
C58 C57 H57 119.5 . . ?
C57 C58 H58 119.6 . . ?
C57 C58 C59 120.8(2) . . ?
C59 C58 H58 119.6 . . ?
C58 C59 H59 120.2 . . ?
C60 C59 C58 119.6(2) . . ?
C60 C59 H59 120.2 . . ?
C55 C60 H60 119.4 . . ?
C59 C60 C55 121.3(2) . . ?
C59 C60 H60 119.4 . . ?
C62 C61 C66 118.3(2) . . ?
C62 C61 C71 119.1(2) . . ?
C66 C61 C71 122.5(2) . . ?
O7 C62 C61 121.0(2) . . ?
O7 C62 C63 117.5(2) . . ?
C61 C62 C63 121.5(2) . . ?
C62 C63 H63 119.8 . . ?
C64 C63 C62 120.4(2) . . ?
C64 C63 H63 119.8 . . ?
C63 C64 H64 119.7 . . ?
C63 C64 C65 120.6(2) . . ?
C65 C64 H64 119.7 . . ?
C64 C65 C66 119.4(2) . . ?
C64 C65 C70 121.4(2) . . ?
C70 C65 C66 119.2(2) . . ?
C65 C66 C61 119.5(2) . . ?
C67 C66 C61 122.7(2) . . ?
C67 C66 C65 117.7(2) . . ?
C66 C67 H67 119.2 . . ?
C68 C67 C66 121.6(2) . . ?
C68 C67 H67 119.2 . . ?
C67 C68 H68 119.7 . . ?
C67 C68 C69 120.5(2) . . ?
C69 C68 H68 119.7 . . ?
C68 C69 H69 120.2 . . ?
C70 C69 C68 119.7(2) . . ?
C70 C69 H69 120.2 . . ?
C65 C70 H70 119.3 . . ?
C69 C70 C65 121.3(2) . . ?
C69 C70 H70 119.3 . . ?
C72 C71 C61 119.0(2) . . ?
C72 C71 C76 118.3(2) . . ?
C76 C71 C61 122.6(2) . . ?
O8 C72 C71 121.0(2) . . ?
O8 C72 C73 117.6(2) . . ?
C71 C72 C73 121.3(2) . . ?
C72 C73 H73 119.6 . . ?
C74 C73 C72 120.7(2) . . ?
C74 C73 H73 119.6 . . ?
C73 C74 H74 119.7 . . ?
C73 C74 C75 120.6(2) . . ?
C75 C74 H74 119.7 . . ?
C74 C75 C76 118.9(2) . . ?
C80 C75 C74 121.3(2) . . ?
C80 C75 C76 119.7(2) . . ?
C75 C76 C71 119.7(2) . . ?
C77 C76 C71 123.0(2) . . ?
C77 C76 C75 117.2(2) . . ?
C76 C77 H77 119.3 . . ?
C78 C77 C76 121.5(2) . . ?
C78 C77 H77 119.3 . . ?
C77 C78 H78 119.7 . . ?
C77 C78 C79 120.6(2) . . ?
C79 C78 H78 119.7 . . ?
C78 C79 H79 120.2 . . ?
C80 C79 C78 119.7(2) . . ?
C80 C79 H79 120.2 . . ?
C75 C80 H80 119.4 . . ?
C79 C80 C75 121.2(2) . . ?
C79 C80 H80 119.4 . . ?
O5 B2 O6 113.78(19) . . ?
O5 B2 O7 113.32(19) . . ?
O6 B2 O7 101.2(2) . . ?
O8 B2 O5 102.2(2) . . ?
O8 B2 O6 113.98(19) . . ?
O8 B2 O7 112.86(19) . . ?
C86 N2 H2 118.4 . . ?
C90 N2 H2 118.4 . . ?
C90 N2 C86 123.3(3) . . ?
N2 C86 H86 120.6 . . ?
N2 C86 C87 118.8(3) . . ?
C87 C86 H86 120.6 . . ?
C86 C87 H87 121.2 . . ?
C86 C87 C88 117.7(3) . . ?
C88 C87 H87 121.2 . . ?
C87 C88 H88 119.7 . . ?
C89 C88 C87 120.6(3) . . ?
C89 C88 H88 119.7 . . ?
C88 C89 H89 120.7 . . ?
C90 C89 C88 118.7(3) . . ?
C90 C89 H89 120.7 . . ?
N2 C90 C89 121.0(3) . . ?
N2 C90 H90 119.5 . . ?
C89 C90 H90 119.5 . . ?
C81 N1 H1 118.7 . . ?
C81 N1 C85 122.7(2) . . ?
C85 N1 H1 118.7 . . ?
N1 C81 H81 120.0 . . ?
N1 C81 C82 120.0(3) . . ?
C82 C81 H81 120.0 . . ?
C81 C82 H82 120.5 . . ?
C81 C82 C83 119.1(3) . . ?
C83 C82 H82 120.5 . . ?
C82 C83 H83 120.0 . . ?
C82 C83 C84 120.1(3) . . ?
C84 C83 H83 120.0 . . ?
C83 C84 H84 120.5 . . ?
C83 C84 C85 119.1(3) . . ?
C85 C84 H84 120.5 . . ?
N1 C85 C84 119.1(3) . . ?
N1 C85 H85 120.5 . . ?
C84 C85 H85 120.5 . . ?
C91 O9 C94 110.1(2) . . ?
O9 C91 H91A 110.4 . . ?
O9 C91 H91B 110.4 . . ?
O9 C91 C92 106.7(2) . . ?
H91A C91 H91B 108.6 . . ?
C92 C91 H91A 110.4 . . ?
C92 C91 H91B 110.4 . . ?
C91 C92 H92A 111.3 . . ?
C91 C92 H92B 111.3 . . ?
C91 C92 C93 102.4(2) . . ?
H92A C92 H92B 109.2 . . ?
C93 C92 H92A 111.3 . . ?
C93 C92 H92B 111.3 . . ?
C92 C93 H93A 111.3 . . ?
C92 C93 H93B 111.3 . . ?
H93A C93 H93B 109.2 . . ?
C94 C93 C92 102.5(2) . . ?
C94 C93 H93A 111.3 . . ?
C94 C93 H93B 111.3 . . ?
O9 C94 C93 107.0(2) . . ?
O9 C94 H94A 110.3 . . ?
O9 C94 H94B 110.3 . . ?
C93 C94 H94A 110.3 . . ?
C93 C94 H94B 110.3 . . ?
H94A C94 H94B 108.6 . . ?
C110 O13 C107 110.7(3) . . ?
O13 C107 H10A 111.5 . . ?
O13 C107 H10B 111.5 . . ?
O13 C107 H10C 106.9 . . ?
O13 C107 H10D 106.9 . . ?
O13 C107 C108 101.2(4) . . ?
H10A C107 H10B 109.3 . . ?
H10C C107 H10D 106.7 . . ?
C108 C107 H10A 111.5 . . ?
C108 C107 H10B 111.5 . . ?
C118 C107 O13 121.9(8) . . ?
C118 C107 H10C 106.9 . . ?
C118 C107 H10D 106.9 . . ?
C107 C108 H10E 111.2 . . ?
C107 C108 H10F 111.2 . . ?
H10E C108 H10F 109.1 . . ?
C109 C108 C107 102.9(4) . . ?
C109 C108 H10E 111.2 . . ?
C109 C108 H10F 111.2 . . ?
C108 C109 H10G 112.0 . . ?
C108 C109 H10H 112.0 . . ?
H10G C109 H10H 109.7 . . ?
C110 C109 C108 98.9(4) . . ?
C110 C109 H10G 112.0 . . ?
C110 C109 H10H 112.0 . . ?
O13 C110 C109 107.1(3) . . ?
O13 C110 H11O 110.3 . . ?
O13 C110 H11P 110.3 . . ?
O13 C110 H11Q 113.1 . . ?
O13 C110 H11R 113.1 . . ?
O13 C110 C117 93.1(6) . . ?
C109 C110 H11O 110.3 . . ?
C109 C110 H11P 110.3 . . ?
H11O C110 H11P 108.5 . . ?
H11Q C110 H11R 110.5 . . ?
C117 C110 H11Q 113.1 . . ?
C117 C110 H11R 113.1 . . ?
C110 C117 H11S 109.5 . . ?
C110 C117 H11T 109.5 . . ?
H11S C117 H11T 108.1 . . ?
C118 C117 C110 110.8(11) . . ?
C118 C117 H11S 109.5 . . ?
C118 C117 H11T 109.5 . . ?
C107 C118 C117 92.5(12) . . ?
C107 C118 H11U 113.2 . . ?
C107 C118 H11V 113.2 . . ?
C117 C118 H11U 113.2 . . ?
C117 C118 H11V 113.2 . . ?
H11U C118 H11V 110.6 . . ?
C106 O12 C103 108.7(2) . . ?
O12 C103 H10Q 110.4 . . ?
O12 C103 H10R 110.4 . . ?
O12 C103 C104 106.6(3) . . ?
H10Q C103 H10R 108.6 . . ?
C104 C103 H10Q 110.4 . . ?
C104 C103 H10R 110.4 . . ?
C103 C104 H10S 111.4 . . ?
C103 C104 H10T 111.4 . . ?
C103 C104 H10U 111.3 . . ?
C103 C104 H10V 111.3 . . ?
C103 C104 C121 102.3(4) . . ?
H10S C104 H10T 109.3 . . ?
H10U C104 H10V 109.2 . . ?
C105 C104 C103 101.9(3) . . ?
C105 C104 H10S 111.4 . . ?
C105 C104 H10T 111.4 . . ?
C121 C104 H10U 111.3 . . ?
C121 C104 H10V 111.3 . . ?
C104 C105 H10W 111.1 . . ?
C104 C105 H10X 111.1 . . ?
C104 C105 C106 103.1(3) . . ?
H10W C105 H10X 109.1 . . ?
C106 C105 H10W 111.1 . . ?
C106 C105 H10X 111.1 . . ?
O12 C106 C105 106.0(3) . . ?
O12 C106 H10Y 110.5 . . ?
O12 C106 H 110.5 . . ?
O12 C106 HA 109.1 . . ?
O12 C106 HB 109.1 . . ?
C105 C106 H10Y 110.5 . . ?
C105 C106 H 110.5 . . ?
H10Y C106 H 108.7 . . ?
HA C106 HB 107.8 . . ?
C121 C106 O12 112.4(6) . . ?
C121 C106 HA 109.1 . . ?
C121 C106 HB 109.1 . . ?
C104 C121 H12C 111.2 . . ?
C104 C121 H12D 111.2 . . ?
C106 C121 C104 102.7(8) . . ?
C106 C121 H12C 111.2 . . ?
C106 C121 H12D 111.2 . . ?
H12C C121 H12D 109.1 . . ?
C98 O10 C95 108.5(2) . . ?
O10 C95 H95A 110.3 . . ?
O10 C95 H95B 110.3 . . ?
O10 C95 C96 107.1(2) . . ?
H95A C95 H95B 108.5 . . ?
C96 C95 H95A 110.3 . . ?
C96 C95 H95B 110.3 . . ?
C95 C96 H96A 111.2 . . ?
C95 C96 H96B 111.2 . . ?
H96A C96 H96B 109.2 . . ?
C97 C96 C95 102.6(2) . . ?
C97 C96 H96A 111.2 . . ?
C97 C96 H96B 111.2 . . ?
C96 C97 H97A 111.5 . . ?
C96 C97 H97B 111.5 . . ?
H97A C97 H97B 109.3 . . ?
C98 C97 C96 101.4(2) . . ?
C98 C97 H97A 111.5 . . ?
C98 C97 H97B 111.5 . . ?
O10 C98 C97 104.8(2) . . ?
O10 C98 H98A 110.8 . . ?
O10 C98 H98B 110.8 . . ?
C97 C98 H98A 110.8 . . ?
C97 C98 H98B 110.8 . . ?
H98A C98 H98B 108.9 . . ?
C99 O11 C102 111.9(4) . . ?
C102 O11 C116 101.4(6) . . ?
O11 C99 H99A 110.6 . . ?
O11 C99 H99B 110.6 . . ?
O11 C99 C100 105.6(5) . . ?
H99A C99 H99B 108.7 . . ?
C100 C99 H99A 110.6 . . ?
C100 C99 H99B 110.6 . . ?
C99 C100 H10I 111.3 . . ?
C99 C100 H10J 111.3 . . ?
C99 C100 C101 102.1(5) . . ?
H10I C100 H10J 109.2 . . ?
C101 C100 H10I 111.3 . . ?
C101 C100 H10J 111.3 . . ?
C100 C101 H10K 111.6 . . ?
C100 C101 H10L 111.6 . . ?
H10K C101 H10L 109.4 . . ?
H10M C101 H10N 108.6 . . ?
C102 C101 C100 100.7(3) . . ?
C102 C101 H10K 111.6 . . ?
C102 C101 H10L 111.6 . . ?
C102 C101 H10M 110.3 . . ?
C102 C101 H10N 110.3 . . ?
C115 C101 H10M 110.3 . . ?
C115 C101 H10N 110.3 . . ?
C115 C101 C102 107.0(5) . . ?
O11 C102 C101 107.5(3) . . ?
O11 C102 H10O 110.2 . . ?
O11 C102 H10P 110.2 . . ?
C101 C102 H10O 110.2 . . ?
C101 C102 H10P 110.2 . . ?
H10O C102 H10P 108.5 . . ?
C101 C115 H11W 110.9 . . ?
C101 C115 H11X 110.9 . . ?
C101 C115 C116 104.1(10) . . ?
H11W C115 H11X 109.0 . . ?
C116 C115 H11W 110.9 . . ?
C116 C115 H11X 110.9 . . ?
O11 C116 H11Y 111.6 . . ?
O11 C116 HC 111.6 . . ?
C115 C116 O11 100.9(9) . . ?
C115 C116 H11Y 111.6 . . ?
C115 C116 HC 111.6 . . ?
H11Y C116 HC 109.4 . . ?
C111 O14A C114 109.4(4) . . ?
O14A C111 H11A 110.4 . . ?
O14A C111 H11B 110.4 . . ?
H11A C111 H11B 108.6 . . ?
C112 C111 O14A 106.4(4) . . ?
C112 C111 H11A 110.4 . . ?
C112 C111 H11B 110.4 . . ?
C111 C112 H11C 110.1 . . ?
C111 C112 H11D 110.1 . . ?
C111 C112 C113 108.1(5) . . ?
H11C C112 H11D 108.4 . . ?
H11E C112 H11F 109.6 . . ?
C113 C112 H11C 110.1 . . ?
C113 C112 H11D 110.1 . . ?
C119 C112 H11E 111.9 . . ?
C119 C112 H11F 111.9 . . ?
C120 C112 H11E 111.9 . . ?
C120 C112 H11F 111.9 . . ?
C120 C112 C119 99.5(7) . . ?
C112 C113 H11G 110.6 . . ?
C112 C113 H11H 110.6 . . ?
H11G C113 H11H 108.8 . . ?
C114 C113 C112 105.6(4) . . ?
C114 C113 H11G 110.6 . . ?
C114 C113 H11H 110.6 . . ?
O14A C114 H11I 110.7 . . ?
O14A C114 H11J 110.7 . . ?
C113 C114 O14A 105.3(4) . . ?
C113 C114 H11I 110.7 . . ?
C113 C114 H11J 110.7 . . ?
H11I C114 H11J 108.8 . . ?
H11K C114 H11L 107.6 . . ?
O14B C114 H11K 108.6 . . ?
O14B C114 H11L 108.6 . . ?
C120 C114 H11K 108.6 . . ?
C120 C114 H11L 108.6 . . ?
C120 C114 O14B 114.6(7) . . ?
C114 O14B C119 105.9(7) . . ?
C112 C119 H11M 109.9 . . ?
C112 C119 H11N 109.9 . . ?
O14B C119 C112 108.7(7) . . ?
O14B C119 H11M 109.9 . . ?
O14B C119 H11N 109.9 . . ?
H11M C119 H11N 108.3 . . ?
C112 C120 H12A 110.1 . . ?
C112 C120 H12B 110.1 . . ?
C114 C120 C112 107.8(8) . . ?
C114 C120 H12A 110.1 . . ?
C114 C120 H12B 110.1 . . ?
H12A C120 H12B 108.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C2 C3 C4 177.9(2) . . . . ?
O2 C12 C13 C14 -179.7(2) . . . . ?
O3 C22 C23 C24 179.6(2) . . . . ?
O4 C32 C33 C34 -179.2(2) . . . . ?
C1 C2 C3 C4 -5.7(4) . . . . ?
C1 C6 C7 C8 -175.8(2) . . . . ?
C1 C11 C12 O2 0.0(4) . . . . ?
C1 C11 C12 C13 -177.8(2) . . . . ?
C1 C11 C16 C15 178.0(2) . . . . ?
C1 C11 C16 C17 -5.7(4) . . . . ?
C2 O1 B1 O2 -41.0(3) . . . . ?
C2 O1 B1 O3 -161.11(18) . . . . ?
C2 O1 B1 O4 77.6(3) . . . . ?
C2 C1 C6 C5 -7.9(4) . . . . ?
C2 C1 C6 C7 169.5(2) . . . . ?
C2 C1 C11 C12 -50.7(3) . . . . ?
C2 C1 C11 C16 125.0(3) . . . . ?
C2 C3 C4 C5 -2.6(4) . . . . ?
C3 C4 C5 C6 5.2(4) . . . . ?
C3 C4 C5 C10 -171.9(3) . . . . ?
C4 C5 C6 C1 0.1(4) . . . . ?
C4 C5 C6 C7 -177.4(2) . . . . ?
C4 C5 C10 C9 176.2(3) . . . . ?
C5 C6 C7 C8 1.6(4) . . . . ?
C6 C1 C2 O1 -172.9(2) . . . . ?
C6 C1 C2 C3 10.8(4) . . . . ?
C6 C1 C11 C12 127.8(3) . . . . ?
C6 C1 C11 C16 -56.6(3) . . . . ?
C6 C5 C10 C9 -0.8(4) . . . . ?
C6 C7 C8 C9 -2.0(4) . . . . ?
C7 C8 C9 C10 0.8(4) . . . . ?
C8 C9 C10 C5 0.6(4) . . . . ?
C10 C5 C6 C1 177.3(2) . . . . ?
C10 C5 C6 C7 -0.2(4) . . . . ?
C11 C1 C2 O1 5.7(4) . . . . ?
C11 C1 C2 C3 -170.7(2) . . . . ?
C11 C1 C6 C5 173.6(2) . . . . ?
C11 C1 C6 C7 -9.0(4) . . . . ?
C11 C12 C13 C14 -1.9(4) . . . . ?
C11 C16 C17 C18 -177.1(3) . . . . ?
C12 O2 B1 O1 -43.5(3) . . . . ?
C12 O2 B1 O3 69.3(3) . . . . ?
C12 O2 B1 O4 -168.28(18) . . . . ?
C12 C11 C16 C15 -6.3(4) . . . . ?
C12 C11 C16 C17 170.0(2) . . . . ?
C12 C13 C14 C15 -3.0(4) . . . . ?
C13 C14 C15 C16 3.0(4) . . . . ?
C13 C14 C15 C20 -174.3(3) . . . . ?
C14 C15 C16 C11 1.7(4) . . . . ?
C14 C15 C16 C17 -174.8(2) . . . . ?
C14 C15 C20 C19 174.8(3) . . . . ?
C15 C16 C17 C18 -0.7(4) . . . . ?
C16 C11 C12 O2 -175.8(2) . . . . ?
C16 C11 C12 C13 6.5(4) . . . . ?
C16 C15 C20 C19 -2.5(4) . . . . ?
C16 C17 C18 C19 -1.2(4) . . . . ?
C17 C18 C19 C20 1.4(4) . . . . ?
C18 C19 C20 C15 0.5(5) . . . . ?
C20 C15 C16 C11 179.1(2) . . . . ?
C20 C15 C16 C17 2.6(4) . . . . ?
C21 C22 C23 C24 -2.1(4) . . . . ?
C21 C26 C27 C28 179.7(2) . . . . ?
C21 C31 C32 O4 4.8(4) . . . . ?
C21 C31 C32 C33 -171.7(2) . . . . ?
C21 C31 C36 C35 171.7(2) . . . . ?
C21 C31 C36 C37 -9.5(4) . . . . ?
C22 O3 B1 O1 -162.21(19) . . . . ?
C22 O3 B1 O2 76.9(3) . . . . ?
C22 O3 B1 O4 -39.9(3) . . . . ?
C22 C21 C26 C25 -5.0(4) . . . . ?
C22 C21 C26 C27 172.9(2) . . . . ?
C22 C21 C31 C32 -50.7(3) . . . . ?
C22 C21 C31 C36 128.8(3) . . . . ?
C22 C23 C24 C25 -1.9(4) . . . . ?
C23 C24 C25 C26 2.2(4) . . . . ?
C23 C24 C25 C30 -176.8(3) . . . . ?
C24 C25 C26 C21 1.2(4) . . . . ?
C24 C25 C26 C27 -176.7(2) . . . . ?
C24 C25 C30 C29 178.3(3) . . . . ?
C25 C26 C27 C28 -2.4(4) . . . . ?
C26 C21 C22 O3 -176.3(2) . . . . ?
C26 C21 C22 C23 5.5(4) . . . . ?
C26 C21 C31 C32 126.0(3) . . . . ?
C26 C21 C31 C36 -54.5(4) . . . . ?
C26 C25 C30 C29 -0.8(4) . . . . ?
C26 C27 C28 C29 1.0(4) . . . . ?
C27 C28 C29 C30 0.7(4) . . . . ?
C28 C29 C30 C25 -0.8(4) . . . . ?
C30 C25 C26 C21 -179.8(2) . . . . ?
C30 C25 C26 C27 2.3(4) . . . . ?
C31 C21 C22 O3 0.5(4) . . . . ?
C31 C21 C22 C23 -177.8(2) . . . . ?
C31 C21 C26 C25 178.3(2) . . . . ?
C31 C21 C26 C27 -3.8(4) . . . . ?
C31 C32 C33 C34 -2.6(4) . . . . ?
C31 C36 C37 C38 179.8(3) . . . . ?
C32 O4 B1 O1 68.6(3) . . . . ?
C32 O4 B1 O2 -167.26(18) . . . . ?
C32 O4 B1 O3 -45.2(3) . . . . ?
C32 C31 C36 C35 -8.8(4) . . . . ?
C32 C31 C36 C37 170.0(2) . . . . ?
C32 C33 C34 C35 -3.7(4) . . . . ?
C33 C34 C35 C36 3.5(4) . . . . ?
C33 C34 C35 C40 -175.2(3) . . . . ?
C34 C35 C36 C31 2.8(4) . . . . ?
C34 C35 C36 C37 -176.1(2) . . . . ?
C34 C35 C40 C39 177.0(3) . . . . ?
C35 C36 C37 C38 -1.4(4) . . . . ?
C36 C31 C32 O4 -174.7(2) . . . . ?
C36 C31 C32 C33 8.8(4) . . . . ?
C36 C35 C40 C39 -1.7(4) . . . . ?
C36 C37 C38 C39 -0.9(4) . . . . ?
C37 C38 C39 C40 2.0(4) . . . . ?
C38 C39 C40 C35 -0.7(4) . . . . ?
C40 C35 C36 C31 -178.4(2) . . . . ?
C40 C35 C36 C37 2.7(4) . . . . ?
B1 O1 C2 C1 62.9(3) . . . . ?
B1 O1 C2 C3 -120.6(2) . . . . ?
B1 O2 C12 C11 68.4(3) . . . . ?
B1 O2 C12 C13 -113.7(2) . . . . ?
B1 O3 C22 C21 66.3(3) . . . . ?
B1 O3 C22 C23 -115.3(2) . . . . ?
B1 O4 C32 C31 65.9(3) . . . . ?
B1 O4 C32 C33 -117.5(2) . . . . ?
O5 C42 C43 C44 -179.7(2) . . . . ?
O6 C52 C53 C54 178.0(2) . . . . ?
O7 C62 C63 C64 178.0(2) . . . . ?
O8 C72 C73 C74 -179.4(2) . . . . ?
C41 C42 C43 C44 -2.1(4) . . . . ?
C41 C46 C47 C48 -178.4(2) . . . . ?
C41 C51 C52 O6 6.9(3) . . . . ?
C41 C51 C52 C53 -170.3(2) . . . . ?
C41 C51 C56 C55 172.4(2) . . . . ?
C41 C51 C56 C57 -10.3(4) . . . . ?
C42 O5 B2 O6 -36.5(3) . . . . ?
C42 O5 B2 O7 78.3(3) . . . . ?
C42 O5 B2 O8 -159.91(19) . . . . ?
C42 C41 C46 C45 -5.4(4) . . . . ?
C42 C41 C46 C47 171.6(2) . . . . ?
C42 C41 C51 C52 -50.5(3) . . . . ?
C42 C41 C51 C56 128.4(3) . . . . ?
C42 C43 C44 C45 -2.2(4) . . . . ?
C43 C44 C45 C46 2.5(4) . . . . ?
C43 C44 C45 C50 -175.4(2) . . . . ?
C44 C45 C46 C41 1.3(4) . . . . ?
C44 C45 C46 C47 -175.9(2) . . . . ?
C44 C45 C50 C49 177.0(2) . . . . ?
C45 C46 C47 C48 -1.4(4) . . . . ?
C46 C41 C42 O5 -176.6(2) . . . . ?
C46 C41 C42 C43 5.8(4) . . . . ?
C46 C41 C51 C52 124.8(2) . . . . ?
C46 C41 C51 C56 -56.3(3) . . . . ?
C46 C45 C50 C49 -1.0(4) . . . . ?
C46 C47 C48 C49 -0.4(4) . . . . ?
C47 C48 C49 C50 1.6(4) . . . . ?
C48 C49 C50 C45 -0.9(4) . . . . ?
C50 C45 C46 C41 179.2(2) . . . . ?
C50 C45 C46 C47 2.1(4) . . . . ?
C51 C41 C42 O5 -1.2(4) . . . . ?
C51 C41 C42 C43 -178.8(2) . . . . ?
C51 C41 C46 C45 179.3(2) . . . . ?
C51 C41 C46 C47 -3.7(4) . . . . ?
C51 C52 C53 C54 -4.7(4) . . . . ?
C51 C56 C57 C58 -176.1(2) . . . . ?
C52 O6 B2 O5 -47.8(3) . . . . ?
C52 O6 B2 O7 -169.64(17) . . . . ?
C52 O6 B2 O8 68.9(3) . . . . ?
C52 C51 C56 C55 -8.6(3) . . . . ?
C52 C51 C56 C57 168.6(2) . . . . ?
C52 C53 C54 C55 -3.7(4) . . . . ?
C53 C54 C55 C56 5.6(4) . . . . ?
C53 C54 C55 C60 -171.8(2) . . . . ?
C54 C55 C56 C51 0.7(3) . . . . ?
C54 C55 C56 C57 -176.7(2) . . . . ?
C54 C55 C60 C59 175.4(3) . . . . ?
C55 C56 C57 C58 1.2(4) . . . . ?
C56 C51 C52 O6 -172.0(2) . . . . ?
C56 C51 C52 C53 10.7(4) . . . . ?
C56 C55 C60 C59 -2.0(4) . . . . ?
C56 C57 C58 C59 -2.0(4) . . . . ?
C57 C58 C59 C60 0.8(4) . . . . ?
C58 C59 C60 C55 1.2(4) . . . . ?
C60 C55 C56 C51 178.1(2) . . . . ?
C60 C55 C56 C57 0.7(3) . . . . ?
C61 C62 C63 C64 -3.6(4) . . . . ?
C61 C66 C67 C68 -177.0(2) . . . . ?
C61 C71 C72 O8 1.9(3) . . . . ?
C61 C71 C72 C73 -174.9(2) . . . . ?
C61 C71 C76 C75 175.2(2) . . . . ?
C61 C71 C76 C77 -6.7(4) . . . . ?
C62 O7 B2 O5 69.6(3) . . . . ?
C62 O7 B2 O6 -168.16(18) . . . . ?
C62 O7 B2 O8 -46.0(3) . . . . ?
C62 C61 C66 C65 -5.4(3) . . . . ?
C62 C61 C66 C67 171.0(2) . . . . ?
C62 C61 C71 C72 -50.0(3) . . . . ?
C62 C61 C71 C76 127.8(3) . . . . ?
C62 C63 C64 C65 -2.4(4) . . . . ?
C63 C64 C65 C66 4.2(4) . . . . ?
C63 C64 C65 C70 -173.5(2) . . . . ?
C64 C65 C66 C61 -0.3(3) . . . . ?
C64 C65 C66 C67 -176.9(2) . . . . ?
C64 C65 C70 C69 176.5(3) . . . . ?
C65 C66 C67 C68 -0.5(4) . . . . ?
C66 C61 C62 O7 -174.3(2) . . . . ?
C66 C61 C62 C63 7.4(4) . . . . ?
C66 C61 C71 C72 126.0(3) . . . . ?
C66 C61 C71 C76 -56.2(3) . . . . ?
C66 C65 C70 C69 -1.3(4) . . . . ?
C66 C67 C68 C69 0.4(4) . . . . ?
C67 C68 C69 C70 -0.7(4) . . . . ?
C68 C69 C70 C65 1.1(4) . . . . ?
C70 C65 C66 C61 177.5(2) . . . . ?
C70 C65 C66 C67 0.9(3) . . . . ?
C71 C61 C62 O7 1.9(3) . . . . ?
C71 C61 C62 C63 -176.4(2) . . . . ?
C71 C61 C66 C65 178.6(2) . . . . ?
C71 C61 C66 C67 -5.0(4) . . . . ?
C71 C72 C73 C74 -2.6(4) . . . . ?
C71 C76 C77 C78 -179.0(2) . . . . ?
C72 O8 B2 O5 -161.99(18) . . . . ?
C72 O8 B2 O6 74.8(3) . . . . ?
C72 O8 B2 O7 -39.9(3) . . . . ?
C72 C71 C76 C75 -7.0(4) . . . . ?
C72 C71 C76 C77 171.1(2) . . . . ?
C72 C73 C74 C75 -2.5(4) . . . . ?
C73 C74 C75 C76 2.5(4) . . . . ?
C73 C74 C75 C80 -175.7(3) . . . . ?
C74 C75 C76 C71 2.3(4) . . . . ?
C74 C75 C76 C77 -176.0(2) . . . . ?
C74 C75 C80 C79 176.5(3) . . . . ?
C75 C76 C77 C78 -0.9(4) . . . . ?
C76 C71 C72 O8 -176.0(2) . . . . ?
C76 C71 C72 C73 7.2(4) . . . . ?
C76 C75 C80 C79 -1.7(4) . . . . ?
C76 C77 C78 C79 -1.2(4) . . . . ?
C77 C78 C79 C80 1.8(4) . . . . ?
C78 C79 C80 C75 -0.4(4) . . . . ?
C80 C75 C76 C71 -179.5(2) . . . . ?
C80 C75 C76 C77 2.3(4) . . . . ?
B2 O5 C42 C41 66.0(3) . . . . ?
B2 O5 C42 C43 -116.4(2) . . . . ?
B2 O6 C52 C51 64.6(3) . . . . ?
B2 O6 C52 C53 -118.0(2) . . . . ?
B2 O7 C62 C61 68.6(3) . . . . ?
B2 O7 C62 C63 -113.1(2) . . . . ?
B2 O8 C72 C71 66.0(3) . . . . ?
B2 O8 C72 C73 -117.1(2) . . . . ?
N2 C86 C87 C88 1.1(4) . . . . ?
C86 N2 C90 C89 -1.7(5) . . . . ?
C86 C87 C88 C89 -1.4(4) . . . . ?
C87 C88 C89 C90 0.2(5) . . . . ?
C88 C89 C90 N2 1.4(5) . . . . ?
C90 N2 C86 C87 0.4(4) . . . . ?
N1 C81 C82 C83 -0.4(4) . . . . ?
C81 N1 C85 C84 -0.5(4) . . . . ?
C81 C82 C83 C84 -0.8(4) . . . . ?
C82 C83 C84 C85 1.4(4) . . . . ?
C83 C84 C85 N1 -0.7(4) . . . . ?
C85 N1 C81 C82 1.1(4) . . . . ?
O9 C91 C92 C93 28.0(3) . . . . ?
C91 O9 C94 C93 -10.4(3) . . . . ?
C91 C92 C93 C94 -32.9(3) . . . . ?
C92 C93 C94 O9 27.4(3) . . . . ?
C94 O9 C91 C92 -11.4(3) . . . . ?
O13 C107 C108 C109 29.6(6) . . . . ?
O13 C107 C118 C117 -18.8(18) . . . . ?
O13 C110 C117 C118 -32.9(14) . . . . ?
C107 O13 C110 C109 -22.6(4) . . . . ?
C107 O13 C110 C117 19.6(7) . . . . ?
C107 C108 C109 C110 -42.1(6) . . . . ?
C108 C109 C110 O13 39.9(5) . . . . ?
C110 O13 C107 C108 -5.4(5) . . . . ?
C110 O13 C107 C118 -2.4(13) . . . . ?
C110 C117 C118 C107 30.1(17) . . . . ?
O12 C103 C104 C105 -29.6(4) . . . . ?
O12 C103 C104 C121 5.2(7) . . . . ?
O12 C106 C121 C104 27.9(11) . . . . ?
C103 O12 C106 C105 13.1(4) . . . . ?
C103 O12 C106 C121 -26.3(9) . . . . ?
C103 C104 C105 C106 36.5(4) . . . . ?
C103 C104 C121 C106 -19.7(10) . . . . ?
C104 C105 C106 O12 -31.6(4) . . . . ?
C106 O12 C103 C104 10.3(4) . . . . ?
O10 C95 C96 C97 -14.9(3) . . . . ?
C95 O10 C98 C97 31.7(3) . . . . ?
C95 C96 C97 C98 32.3(3) . . . . ?
C96 C97 C98 O10 -39.9(3) . . . . ?
C98 O10 C95 C96 -10.3(3) . . . . ?
O11 C99 C100 C101 33.9(9) . . . . ?
C99 O11 C102 C101 1.1(6) . . . . ?
C99 C100 C101 C102 -31.8(6) . . . . ?
C100 C101 C102 O11 19.6(4) . . . . ?
C101 C115 C116 O11 -44.3(15) . . . . ?
C102 O11 C99 C100 -22.9(9) . . . . ?
C102 O11 C116 C115 35.4(12) . . . . ?
C102 C101 C115 C116 34.9(14) . . . . ?
C115 C101 C102 O11 -11.5(9) . . . . ?
C116 O11 C102 C101 -16.0(7) . . . . ?
O14A C111 C112 C113 -23.2(7) . . . . ?
C111 O14A C114 C113 -3.7(7) . . . . ?
C111 C112 C113 C114 20.9(8) . . . . ?
C112 C113 C114 O14A -10.1(8) . . . . ?
C114 O14A C111 C112 16.8(6) . . . . ?
C114 O14B C119 C112 11.7(10) . . . . ?
O14B C114 C120 C112 -12.0(15) . . . . ?
C119 C112 C120 C114 17.0(13) . . . . ?
C120 C112 C119 O14B -17.7(11) . . . . ?
C120 C114 O14B C119 -0.2(12) . . . . ?

_olex2_exptl_crystal_mounting_method 'MiTeGen 75 micron MicroLoop'
_olex2_submission_original_sample_id kre21_06
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   4854
_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 1.949
_oxdiff_exptl_absorpt_empirical_full_min 0.671
# start Validation Reply Form
_vrf_PLAT089_R-8                 
;
PROBLEM: Poor Data / Parameter Ratio (Zmax < 18) ........       6.36 Note  
RESPONSE: Due to the amount of disorder in the structure.
;
_vrf_PLAT112_R-8                 
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem         I         87 %Fit  
RESPONSE: Platon did not suggest any higher symmetry.
;
_vrf_PLAT243_R-8                 
;
PROBLEM: High   'Solvent' Ueq as Compared to Neighbors of         O9 Check 
RESPONSE: Due to the disorder about the tetrahydrofuran molecules in the
          structure.
;
_vrf_PLAT250_R-8                 
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.1 Note  
RESPONSE: Due to the disorder about the tetrahydrofuran molecules in the
          structure.
;
_vrf_PLAT340_R-8                 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.00422 Ang.  
RESPONSE: Due to the disorder about the tetrahydrofuran molecules in the
          structure and the resulting data/parameter ratio.
;
_vrf_PLAT911_R-8                 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.597         11 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_R-8_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2058925'
loop_
_audit_author_name
_audit_author_address
'Daniel Unruh'
;Texas Tech University
United States of America
;
_audit_update_record             
;
2021-02-01 deposited with the CCDC.	2021-03-23 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT260_R-8                 
;
PROBLEM: Large Average Ueq of Residue Including      Cl3B      0.103 Check 
RESPONSE: Due to the highly disordered nature of this interstitial 
          dichloromethane molecule.
;
_vrf_PLAT911_R-8                 
;
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             2020-09-18
_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
loop_
_audit_author_email
Shipra.Garg@ttu.edu
daniel.unruh@ttu.edu
Clemens.krempner@ttu.edu
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C40 H24 B O4, C16 H34 N4 P, 2(C H2 Cl2)'
_chemical_formula_sum            'C58 H62 B Cl4 N4 O4 P'
_chemical_formula_weight         1062.69
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C118  H130  B2  N10  O12  P6  '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   10.93710(10)
_cell_length_b                   19.13750(10)
_cell_length_c                   12.85790(10)
_cell_angle_alpha                90
_cell_angle_beta                 92.1820(10)
_cell_angle_gamma                90
_cell_volume                     2689.32(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    54483
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      77.3430
_cell_measurement_theta_min      3.4310
_shelx_estimated_absorpt_T_max   0.554
_shelx_estimated_absorpt_T_min   0.504
_exptl_absorpt_coefficient_mu    2.681
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.375
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.82a (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_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1116
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 -1 0 0.1418
1 5 8 0.1296
7 4 0 0.1339
6 1 -4 0.1223
2 -3 -8 0.1215
-1 -5 -7 0.1302
-1 -10 5 0.1263
-6 0 5 0.1533
-4 10 1 0.1607
-1 12 -2 0.1310
3 8 -5 0.1388
6 0 -5 0.1272
6 -6 -3 0.1193
4 -11 0 0.1149
-1 -11 4 0.1215
5 9 -1 0.1425
1 12 3 0.1328
-5 -9 1 0.1298
-1 -12 -3 0.1198
4 -5 -6 0.1188
2 -10 -5 0.1229
1 12 -1 0.1288
0 12 0 0.1365
3 -11 -2 0.1171
0 -12 0 0.1216
7 -4 0 0.1218
0 -5 8 0.1297
-6 5 -3 0.1531
-2 6 -7 0.1413
1 4 -8 0.1204
-7 -1 0 0.1403
-2 -2 -8 0.1348
1 -1 -8 0.1203
0 1 8 0.1224
6 2 3 0.1438
-6 3 -3 0.1447
-2 3 -8 0.1344
0 -3 8 0.1204
7 -2 0 0.1204
-5 -8 -1 0.1372
0 -9 -6 0.1196
-6 -6 0 0.1364
0 11 3 0.1361

_exptl_crystal_recrystallization_method 'Slow evaporation from dichloromethane'
_exptl_crystal_size_max          0.296
_exptl_crystal_size_mid          0.254
_exptl_crystal_size_min          0.25
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
-1.9981 -0.9999 -0.0035 -0.0378 -0.1896 -0.2201
0.7562 4.8777 7.5851 0.2078 0.8657 -0.4553
6.7724 3.7045 -0.0187 0.1537 0.6453 0.7483
6.1081 0.7041 -4.4989 0.0260 0.1131 0.9932
2.3643 -3.2147 -7.6684 -0.1389 -0.5762 0.8054
-1.4076 -5.1023 -7.3594 -0.2170 -0.9044 0.3674
-0.6738 -10.1299 4.7885 -0.8821 0.2108 -0.4212
-5.6938 -0.1837 5.2359 -0.0090 0.0010 -1.0000
-4.1419 10.0682 0.6485 0.8606 -0.1133 -0.4965
-1.3110 11.6415 -2.4074 0.9910 -0.1298 0.0338
2.9770 8.2884 -5.2637 0.7009 -0.0911 0.7075
5.6976 0.1871 -5.2299 0.0091 -0.0001 1.0000
5.6508 -6.0459 -3.2613 -0.5206 0.0692 0.8510
3.5754 -10.7283 0.0697 -0.9160 0.1205 0.3826
-0.7547 -10.8205 4.0288 -0.9187 0.1200 -0.3763
4.6888 9.1953 -1.2443 0.6527 0.4500 0.6095
1.3908 11.5388 2.5559 0.8236 0.5667 -0.0231
-4.5693 -9.4174 1.0611 -0.6687 -0.4609 -0.5834
-1.2019 -11.5215 -2.7233 -0.8225 -0.5659 0.0558
4.3516 -5.2950 -5.7455 -0.3830 -0.2624 0.8857
1.9041 -9.5609 -4.9187 -0.6855 -0.4710 0.5552
1.0705 12.1133 -1.3904 0.9582 0.1784 0.2235
-0.1847 12.4100 -0.2563 0.9831 0.1828 0.0047
2.7886 -11.0137 -2.1651 -0.8754 -0.1623 0.4553
0.1750 -12.4100 0.2651 -0.9831 -0.1828 -0.0064
6.7588 -3.7907 -0.0248 -0.4342 0.5090 0.7432
0.0780 -4.8986 7.6591 -0.5472 0.6391 -0.5404
-5.8719 5.1501 -2.9079 0.5846 -0.6844 -0.4357
-1.9038 5.5335 -7.0386 0.6211 -0.7258 0.2957
1.0960 4.3042 -7.7646 0.4790 -0.5590 0.6768
-7.0298 -1.2804 -0.4853 0.0524 -0.6712 -0.7394
-2.0984 -1.6757 -7.7941 0.0751 -0.9430 0.3243
0.9431 -1.2371 -8.2665 0.0577 -0.7188 0.6928
0.2821 1.4456 8.2643 -0.0662 0.8274 -0.5577
6.2961 1.6502 3.4119 -0.0701 0.8902 0.4501
-6.2486 2.9338 -3.1593 0.4236 -0.7801 -0.4604
-1.7984 3.1673 -7.7022 0.4472 -0.8217 0.3533
-0.0117 -2.7764 8.1290 -0.3887 0.7137 -0.5827
6.9625 -2.2021 0.4004 -0.3226 0.5950 0.7362
-5.0407 -8.4730 -1.2276 -0.5368 -0.6996 -0.4715
0.1528 -8.5233 -6.0719 -0.5443 -0.7109 0.4454
-6.2873 -5.7186 -0.2250 -0.3165 -0.6628 -0.6787
0.2857 11.2663 3.4833 0.8051 0.5543 -0.2110

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            65152
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.735
_diffrn_reflns_theta_min         3.440
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     26.00 121.00   0.50    0.05    --   48.15  77.00 -30.00  190
  2  ω     26.00 121.00   0.50    0.05    --   48.15  77.00 -90.00  190
  3  ω     33.00 121.00   0.50    0.05    --   48.15  57.00-120.00  176
  4  ω     26.00  95.00   0.50    0.05    --   48.15  77.00  60.00  138
  5  ω     33.00 121.00   0.50    0.05    --   48.15  57.00  60.00  176
  6  ω     26.00 121.00   0.50    0.05    --   48.15  77.00 120.00  190
  7  ω     26.00 121.00   0.50    0.05    --   48.15  77.00 150.00  190
  8  ω     88.00 178.00   0.50    0.15    --  107.75 136.00  44.00  180
  9  ω     95.00 178.00   0.50    0.15    --  107.75 125.00 120.00  166
 10  ω     95.00 178.00   0.50    0.15    --  107.75 125.00 150.00  166
 11  ω     95.00 178.00   0.50    0.15    --  107.75 125.00  90.00  166
 12  ω     90.00 178.00   0.50    0.15    --  107.75 133.00-134.00  176
 13  ω     95.00 178.00   0.50    0.15    --  107.75 125.00-180.00  166
 14  ω     95.00 178.00   0.50    0.15    --  107.75  30.00  30.00  166
 15  ω     94.00 178.00   0.50    0.15    --  107.75  15.00 -30.00  168
 16  ω     94.00 178.00   0.50    0.15    --  107.75  15.00 120.00  168
 17  ω     35.00  73.00   0.50    0.15    --  107.75 -61.00 150.00   76
 18  ω     35.00 107.00   0.50    0.15    --  107.75 -77.00 150.00  144
 19  ω     35.00 107.00   0.50    0.15    --  107.75 -77.00 120.00  144
 20  ω     35.00  73.00   0.50    0.15    --  107.75 -61.00  60.00   76
 21  ω    -26.00  28.00   0.50    0.05    --   48.15 -19.00-180.00  108
 22  ω     35.00  73.00   0.50    0.15    --  107.75 -61.00-150.00   76
 23  ω     35.00 106.00   0.50    0.15    --  107.75 -94.00-150.00  142
 24  ω     35.00 112.00   0.50    0.15    --  107.75-125.00-180.00  154
 25  ω     41.00 102.00   0.50    0.05    --   48.15-136.00 -20.00  122
 26  ω     35.00 112.00   0.50    0.15    --  107.75-125.00 -90.00  154
 27  ω     35.00 107.00   0.50    0.15    --  107.75-102.00 -45.52  144
 28  ω     35.00 106.00   0.50    0.15    --  107.75 -94.00-180.00  142
 29  ω     41.00 120.00   0.50    0.15    --  107.75-136.00 -20.00  158
 30  ω     35.00 106.00   0.50    0.15    --  107.75 -94.00 -30.00  142
 31  ω     35.00 106.00   0.50    0.15    --  107.75 -94.00   0.00  142
 32  ω     35.00 106.00   0.50    0.15    --  107.75 -94.00  60.00  142
 33  ω     39.00 100.00   0.50    0.05    --   48.15-133.00 158.00  122
 34  ω     39.00 118.00   0.50    0.15    --  107.75-133.00 158.00  158
 35  ω    -94.00 -19.00   0.50    0.05    --  -48.15 136.00  44.00  150
 36  ω    -86.00 -13.00   0.50    0.15    --  -86.25 125.00 120.00  146
 37  ω    -94.00 -19.00   0.50    0.15    --  -86.25 136.00  44.00  150
 38  ω    -92.00 -17.00   0.50    0.15    --  -86.25 133.00-134.00  150
 39  ω    -92.00 -17.00   0.50    0.05    --  -48.15 133.00-134.00  150
 40  ω    -49.00 -14.00   0.50    0.15    --  -86.25  45.00   0.00   70
 41  ω    -49.00 -14.00   0.50    0.15    --  -86.25  45.00  30.00   70
 42  ω    -49.00 -14.00   0.50    0.15    --  -86.25  45.00  90.00   70
 43  ω    -69.00 -13.00   0.50    0.15    --  -86.25  61.00 120.00  112
 44  ω    -49.00 -14.00   0.50    0.15    --  -86.25  45.00  60.00   70
 45  ω    -49.00 -14.00   0.50    0.15    --  -86.25  45.00 -90.00   70
 46  ω    -49.00 -14.00   0.50    0.15    --  -86.25  45.00-120.00   70
 47  ω    -24.00  27.00   0.50    0.05    --  -48.15  19.00-120.00  102
 48  ω    -24.00  27.00   0.50    0.05    --  -48.15  19.00 -90.00  102
 49  ω    -24.00  27.00   0.50    0.05    --  -48.15  19.00 -30.00  102
 50  ω    -24.00  27.00   0.50    0.05    --  -48.15  19.00  30.00  102
 51  ω    -24.00  27.00   0.50    0.05    --  -48.15  19.00  90.00  102
 52  ω    -24.00  27.00   0.50    0.05    --  -48.15  19.00 150.00  102
 53  ω   -121.00 -66.00   0.50    0.05    --  -48.15-136.00 -20.00  110
 54  ω   -159.00 -66.00   0.50    0.15    --  -86.25-136.00 -20.00  186
 55  ω   -121.00 -68.00   0.50    0.05    --  -48.15-133.00 158.00  106
 56  ω   -159.00 -68.00   0.50    0.15    --  -86.25-133.00 158.00  182
;
_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      -0.0202987000
_diffrn_orient_matrix_UB_12      0.0784846000
_diffrn_orient_matrix_UB_13      -0.0210457000
_diffrn_orient_matrix_UB_21      0.0857223000
_diffrn_orient_matrix_UB_22      0.0179487000
_diffrn_orient_matrix_UB_23      0.0940488000
_diffrn_orient_matrix_UB_31      0.1100054000
_diffrn_orient_matrix_UB_32      0.0005394000
_diffrn_orient_matrix_UB_33      -0.0713377000
_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         0.911
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.956
_reflns_number_gt                10949
_reflns_number_total             11148
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_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 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details 
;
 Flack x determined using 5073 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     742
_refine_ls_number_reflns         11148
_refine_ls_number_restraints     221
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0361
_refine_ls_restrained_S_all      1.073
_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)+(0.0524P)²+1.1552P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.0937
_refine_special_details          
'The intersitial dichloromethane molecules were positionally disordered over multiple sites. To help maintain reasonable ADP values and bond lengths, SIMU and free variable DFIX restraints were used.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl1A-C56A = Cl2A-C56A = Cl1B-C56B = Cl2B-C56B
 1.76328 with sigma of 0.02
 Cl3A-C57A = Cl4A-C57A = Cl3B-C57B = Cl4B-C57B
 1.76328 with sigma of 0.02
 Cl3C-C57C = Cl4C-C57C
 1.76328 with sigma of 0.02
 Cl1A-Cl2A = Cl1B-Cl2B = Cl3A-Cl4A = Cl3B-Cl4B = Cl3C-Cl4C
 2.93183 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl3A \\sim Cl4A \\sim C57A \\sim Cl3B \\sim Cl4B \\sim C57B \\sim Cl3C \\sim
Cl4C \\sim C57C: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
Cl1A \\sim Cl2A \\sim Cl1B \\sim Cl2B \\sim C56A \\sim C56B: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
4. Others
 1*[Sof(Cl3A)+Sof(Cl4A)+Sof(C57A)+Sof(H57A)+Sof(H57B)]+1*[Sof(Cl3B)+Sof(Cl4B)+
 Sof(C57B)+Sof(H57C)+Sof(H57D)]+1*[Sof(Cl3C)+Sof(Cl4C)+Sof(C57C)+Sof(H57E)+
 Sof(H57F)]=1 with esd of 0
 Sof(Cl1B)=Sof(Cl2B)=Sof(C56B)=Sof(H56C)=Sof(H56D)=1-FVAR(1)
 Sof(Cl1A)=Sof(Cl2A)=Sof(C56A)=Sof(H56A)=Sof(H56B)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=FVAR(2)
 Sof(Cl3A)=Sof(Cl4A)=Sof(C57A)=Sof(H57A)=Sof(H57B)=FVAR(3)
 Sof(Cl3B)=Sof(Cl4B)=Sof(C57B)=Sof(H57C)=Sof(H57D)=FVAR(4)
 Sof(Cl3C)=Sof(Cl4C)=Sof(C57C)=Sof(H57E)=Sof(H57F)=FVAR(5)
5.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,
 H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B),
 C15(H15A,H15B), C16(H16A,H16B), C56A(H56A,H56B), C56B(H56C,H56D), C57A(H57A,
 H57B), C57B(H57C,H57D), C57C(H57E,H57F)
5.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C29(H29),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C39(H39), C40(H40), C41(H41),
  C42(H42), C44(H44), C45(H45), C48(H48), C49(H49), C51(H51), C52(H52),
 C53(H53), C54(H54)
5.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.57198(15) 0.47096(9) 0.46781(13) 0.0178(3) Uani 1 1 d . . . . .
O2 O 0.47599(15) 0.38666(9) 0.34644(13) 0.0168(3) Uani 1 1 d . . . . .
O3 O 0.54216(15) 0.34649(9) 0.50599(13) 0.0175(3) Uani 1 1 d . . . . .
O4 O 0.37861(16) 0.43393(9) 0.50056(13) 0.0174(3) Uani 1 1 d . . . . .
C17 C 0.6624(2) 0.48234(12) 0.40126(19) 0.0164(5) Uani 1 1 d . . . . .
C18 C 0.6388(2) 0.49395(12) 0.29616(18) 0.0153(4) Uani 1 1 d . . . . .
C019 C 0.4596(2) 0.54812(13) 0.19014(18) 0.0162(5) Uani 1 1 d . . . . .
C19 C 0.7401(2) 0.50198(12) 0.22935(19) 0.0158(4) Uani 1 1 d . . . . .
C20 C 0.7253(2) 0.50350(13) 0.11891(19) 0.0176(5) Uani 1 1 d . . . . .
H20 H 0.647280 0.499122 0.088161 0.021 Uiso 1 1 calc R U . . .
C21 C 0.8235(2) 0.51126(15) 0.0571(2) 0.0225(5) Uani 1 1 d . . . . .
H21 H 0.811516 0.511727 -0.014938 0.027 Uiso 1 1 calc R U . . .
C22 C 0.9431(2) 0.51859(15) 0.1017(2) 0.0245(5) Uani 1 1 d . . . . .
H22 H 1.009143 0.525542 0.059444 0.029 Uiso 1 1 calc R U . . .
C23 C 0.9607(2) 0.51538(14) 0.2075(2) 0.0221(5) Uani 1 1 d . . . . .
H23 H 1.039479 0.519378 0.236604 0.027 Uiso 1 1 calc R U . . .
C24 C 0.8614(2) 0.50609(13) 0.2734(2) 0.0181(5) Uani 1 1 d . . . . .
C25 C 0.8797(2) 0.49924(14) 0.3831(2) 0.0204(5) Uani 1 1 d . . . . .
H25 H 0.958091 0.503669 0.413029 0.024 Uiso 1 1 calc R U . . .
C26 C 0.7839(2) 0.48628(13) 0.44486(19) 0.0191(5) Uani 1 1 d . . . . .
H26 H 0.797820 0.479946 0.516031 0.023 Uiso 1 1 calc R U . . .
C27 C 0.5105(2) 0.49272(13) 0.25363(18) 0.0156(5) Uani 1 1 d . . . . .
C28 C 0.4362(2) 0.43689(13) 0.27778(17) 0.0154(5) Uani 1 1 d . . . . .
C29 C 0.3182(2) 0.42889(13) 0.22977(18) 0.0177(5) Uani 1 1 d . . . . .
H29 H 0.271721 0.389600 0.244037 0.021 Uiso 1 1 calc R U . . .
C30 C 0.2725(2) 0.47851(14) 0.16274(19) 0.0183(5) Uani 1 1 d . . . . .
H30 H 0.197027 0.471507 0.128612 0.022 Uiso 1 1 calc R U . . .
C31 C 0.3391(2) 0.54070(13) 0.14458(18) 0.0168(5) Uani 1 1 d . . . . .
C32 C 0.2873(2) 0.59734(14) 0.08611(19) 0.0195(5) Uani 1 1 d . . . . .
H32 H 0.209302 0.592574 0.055542 0.023 Uiso 1 1 calc R U . . .
C33 C 0.3495(2) 0.65844(15) 0.07391(19) 0.0213(5) Uani 1 1 d . . . . .
H33 H 0.313357 0.695166 0.036681 0.026 Uiso 1 1 calc R U . . .
C34 C 0.4687(2) 0.66559(14) 0.11800(18) 0.0197(5) Uani 1 1 d . . . . .
H34 H 0.511600 0.706973 0.108927 0.024 Uiso 1 1 calc R U . . .
C35 C 0.5222(2) 0.61197(13) 0.17428(19) 0.0180(5) Uani 1 1 d . . . . .
H35 H 0.601043 0.617627 0.202602 0.022 Uiso 1 1 calc R U . . .
C36 C 0.5510(2) 0.34677(13) 0.61204(18) 0.0163(5) Uani 1 1 d . . . . .
C37 C 0.4481(2) 0.34530(12) 0.67103(18) 0.0156(4) Uani 1 1 d . . . . .
C38 C 0.4645(2) 0.35071(12) 0.78237(19) 0.0163(5) Uani 1 1 d . . . . .
C39 C 0.3655(2) 0.36245(14) 0.8491(2) 0.0201(5) Uani 1 1 d . . . . .
H39 H 0.286268 0.364837 0.820403 0.024 Uiso 1 1 calc R U . . .
C40 C 0.3839(3) 0.37028(15) 0.9541(2) 0.0245(5) Uani 1 1 d . . . . .
H40 H 0.317378 0.378195 0.995492 0.029 Uiso 1 1 calc R U . . .
C41 C 0.5027(3) 0.36649(16) 1.0002(2) 0.0269(6) Uani 1 1 d . . . . .
H41 H 0.514369 0.370905 1.071958 0.032 Uiso 1 1 calc R U . . .
C42 C 0.6005(2) 0.35630(15) 0.9391(2) 0.0233(5) Uani 1 1 d . . . . .
H42 H 0.678766 0.353974 0.969772 0.028 Uiso 1 1 calc R U . . .
C43 C 0.5848(2) 0.34919(13) 0.82949(19) 0.0186(5) Uani 1 1 d . . . . .
C44 C 0.6864(2) 0.34458(14) 0.7651(2) 0.0209(5) Uani 1 1 d . . . . .
H44 H 0.764886 0.341161 0.795114 0.025 Uiso 1 1 calc R U . . .
C45 C 0.6704(2) 0.34509(13) 0.6593(2) 0.0188(5) Uani 1 1 d . . . . .
H45 H 0.738272 0.344331 0.617881 0.023 Uiso 1 1 calc R U . . .
C46 C 0.3240(2) 0.34377(13) 0.61930(18) 0.0159(5) Uani 1 1 d . . . . .
C47 C 0.2958(2) 0.38996(13) 0.53870(19) 0.0166(5) Uani 1 1 d . . . . .
C48 C 0.1737(2) 0.39734(13) 0.49891(19) 0.0186(5) Uani 1 1 d . . . . .
H48 H 0.156051 0.429678 0.446466 0.022 Uiso 1 1 calc R U . . .
C49 C 0.0814(2) 0.35745(14) 0.5367(2) 0.0214(5) Uani 1 1 d . . . . .
H49 H 0.001012 0.365160 0.513393 0.026 Uiso 1 1 calc R U . . .
C50 C 0.1076(2) 0.30474(14) 0.6109(2) 0.0194(5) Uani 1 1 d . . . . .
C51 C 0.0150(2) 0.25888(15) 0.6453(2) 0.0263(6) Uani 1 1 d . . . . .
H51 H -0.065469 0.265539 0.621444 0.032 Uiso 1 1 calc R U . . .
C52 C 0.0419(3) 0.20524(15) 0.7125(2) 0.0283(6) Uani 1 1 d . . . . .
H52 H -0.019742 0.175857 0.734388 0.034 Uiso 1 1 calc R U . . .
C53 C 0.1640(3) 0.19484(14) 0.7484(2) 0.0241(5) Uani 1 1 d . . . . .
H53 H 0.183032 0.157583 0.792587 0.029 Uiso 1 1 calc R U . . .
C54 C 0.2548(2) 0.23898(13) 0.7190(2) 0.0194(5) Uani 1 1 d . . . . .
H54 H 0.334506 0.231415 0.744406 0.023 Uiso 1 1 calc R U . . .
C55 C 0.2305(2) 0.29626(13) 0.65049(19) 0.0176(5) Uani 1 1 d . . . . .
B1 B 0.4926(2) 0.40934(15) 0.4557(2) 0.0166(5) Uani 1 1 d . . . . .
P1 P 0.44582(5) 0.66610(3) 0.63997(4) 0.01582(13) Uani 1 1 d . . . . .
N1 N 0.3888(2) 0.73747(11) 0.68860(17) 0.0186(4) Uani 1 1 d . . . . .
H1 H 0.427(3) 0.7720(19) 0.667(3) 0.022 Uiso 1 1 d . U . . .
N2 N 0.3899(2) 0.63338(11) 0.53178(16) 0.0187(4) Uani 1 1 d . . . . .
N3 N 0.4253(2) 0.60379(11) 0.72519(16) 0.0196(4) Uani 1 1 d . . . . .
N4 N 0.5859(2) 0.68900(12) 0.61636(17) 0.0207(4) Uani 1 1 d . . . . .
C1 C 0.2603(2) 0.75629(14) 0.7143(2) 0.0197(5) Uani 1 1 d . . . . .
C2 C 0.2718(3) 0.81636(16) 0.7915(3) 0.0310(6) Uani 1 1 d . . . . .
H2A H 0.312327 0.800284 0.854599 0.046 Uiso 1 1 calc R U . . .
H2B H 0.191705 0.833258 0.806597 0.046 Uiso 1 1 calc R U . . .
H2C H 0.318459 0.853438 0.762174 0.046 Uiso 1 1 calc R U . . .
C3 C 0.1916(3) 0.69630(15) 0.7643(2) 0.0244(5) Uani 1 1 d . . . . .
H3A H 0.191963 0.656265 0.719290 0.037 Uiso 1 1 calc R U . . .
H3B H 0.108756 0.710262 0.774939 0.037 Uiso 1 1 calc R U . . .
H3C H 0.231050 0.684674 0.829980 0.037 Uiso 1 1 calc R U . . .
C4 C 0.1911(3) 0.78015(17) 0.6152(2) 0.0309(6) Uani 1 1 d . . . . .
H4A H 0.234463 0.818021 0.584406 0.046 Uiso 1 1 calc R U . . .
H4B H 0.110671 0.795504 0.632072 0.046 Uiso 1 1 calc R U . . .
H4C H 0.184653 0.741940 0.566978 0.046 Uiso 1 1 calc R U . . .
C5 C 0.4126(2) 0.66450(16) 0.42843(18) 0.0238(5) Uani 1 1 d . . . . .
H5A H 0.476523 0.639369 0.393880 0.029 Uiso 1 1 calc R U . . .
H5B H 0.435886 0.713247 0.435075 0.029 Uiso 1 1 calc R U . . .
C6 C 0.2908(3) 0.65694(15) 0.36944(19) 0.0246(5) Uani 1 1 d . . . . .
H6A H 0.301233 0.655498 0.294899 0.030 Uiso 1 1 calc R U . . .
H6B H 0.235791 0.694886 0.385459 0.030 Uiso 1 1 calc R U . . .
C7 C 0.2438(3) 0.58737(15) 0.4094(2) 0.0246(5) Uani 1 1 d . . . . .
H7A H 0.283545 0.548458 0.376173 0.029 Uiso 1 1 calc R U . . .
H7B H 0.155976 0.583364 0.397272 0.029 Uiso 1 1 calc R U . . .
C8 C 0.2773(2) 0.58967(14) 0.5259(2) 0.0204(5) Uani 1 1 d . . . . .
H8A H 0.212378 0.610866 0.564471 0.025 Uiso 1 1 calc R U . . .
H8B H 0.293371 0.543144 0.553088 0.025 Uiso 1 1 calc R U . . .
C9 C 0.4442(3) 0.61534(16) 0.8390(2) 0.0268(6) Uani 1 1 d . . . . .
H9A H 0.371653 0.602194 0.875422 0.032 Uiso 1 1 calc R U . . .
H9B H 0.462172 0.664102 0.853421 0.032 Uiso 1 1 calc R U . . .
C10 C 0.5531(3) 0.56902(19) 0.8734(3) 0.0406(8) Uani 1 1 d . . . . .
H10A H 0.619323 0.597224 0.903231 0.049 Uiso 1 1 calc R U . . .
H10B H 0.528819 0.535244 0.924955 0.049 Uiso 1 1 calc R U . . .
C11 C 0.5929(3) 0.53238(16) 0.7760(2) 0.0309(6) Uani 1 1 d . . . . .
H11A H 0.618031 0.484720 0.790984 0.037 Uiso 1 1 calc R U . . .
H11B H 0.659861 0.557057 0.745024 0.037 Uiso 1 1 calc R U . . .
C12 C 0.4783(3) 0.53402(14) 0.7046(2) 0.0238(5) Uani 1 1 d . . . . .
H12A H 0.498819 0.529350 0.632238 0.029 Uiso 1 1 calc R U . . .
H12B H 0.421975 0.497023 0.722055 0.029 Uiso 1 1 calc R U . . .
C13 C 0.6646(3) 0.65216(17) 0.5420(2) 0.0317(6) Uani 1 1 d . . . . .
H13A H 0.659446 0.674093 0.473933 0.038 Uiso 1 1 calc R U . . .
H13B H 0.641358 0.603428 0.534937 0.038 Uiso 1 1 calc R U . . .
C14 C 0.7924(3) 0.6592(2) 0.5912(3) 0.0393(7) Uani 1 1 d . . . . .
H14A H 0.810586 0.620922 0.638707 0.047 Uiso 1 1 calc R U . . .
H14B H 0.853528 0.660346 0.538546 0.047 Uiso 1 1 calc R U . . .
C15 C 0.7882(3) 0.72771(18) 0.6487(3) 0.0357(7) Uani 1 1 d . . . . .
H15A H 0.797332 0.766778 0.601551 0.043 Uiso 1 1 calc R U . . .
H15B H 0.852134 0.730042 0.702958 0.043 Uiso 1 1 calc R U . . .
C16 C 0.6622(3) 0.72795(16) 0.6949(3) 0.0300(6) Uani 1 1 d . . . . .
H16A H 0.663637 0.704514 0.761796 0.036 Uiso 1 1 calc R U . . .
H16B H 0.632272 0.775248 0.703250 0.036 Uiso 1 1 calc R U . . .
Cl1A Cl 1.00339(11) 0.52775(7) 0.67178(11) 0.0416(4) Uani 0.627(2) 1 d D U P A
1
Cl2A Cl 1.0683(2) 0.45152(14) 0.86192(13) 0.0830(8) Uani 0.627(2) 1 d D U P A 1
C56A C 1.1216(7) 0.4829(5) 0.7449(7) 0.0428(16) Uani 0.627(2) 1 d D U P A 1
H56A H 1.151182 0.444190 0.704187 0.051 Uiso 0.627(2) 1 calc R U P A 1
H56B H 1.189498 0.514546 0.759060 0.051 Uiso 0.627(2) 1 calc R U P A 1
Cl1B Cl 1.1503(2) 0.51143(13) 0.85644(17) 0.0404(6) Uani 0.373(2) 1 d D U P A 2
Cl2B Cl 0.9252(2) 0.4723(2) 0.7409(2) 0.0667(9) Uani 0.373(2) 1 d D U P A 2
C56B C 1.0855(13) 0.4876(11) 0.7343(14) 0.053(3) Uani 0.373(2) 1 d D U P A 2
H56C H 1.125068 0.445581 0.710110 0.063 Uiso 0.373(2) 1 calc R U P A 2
H56D H 1.099533 0.524545 0.684517 0.063 Uiso 0.373(2) 1 calc R U P A 2
Cl3A Cl -0.0527(2) 0.83090(10) 0.92204(18) 0.0559(5) Uani 0.649(4) 1 d D U P B
1
Cl4A Cl -0.0774(4) 0.68284(15) 0.9557(3) 0.1202(15) Uani 0.649(4) 1 d D U P B 1
C57A C -0.1039(12) 0.7667(6) 1.0065(10) 0.091(2) Uani 0.649(4) 1 d D U P B 1
H57A H -0.190731 0.772837 1.016347 0.110 Uiso 0.649(4) 1 calc R U P B 1
H57B H -0.061387 0.771385 1.073711 0.110 Uiso 0.649(4) 1 calc R U P B 1
Cl3B Cl -0.0154(8) 0.8429(4) 0.9744(8) 0.102(2) Uani 0.280(4) 1 d D U P C 2
Cl4B Cl -0.1329(10) 0.6978(5) 0.9512(7) 0.115(2) Uani 0.280(4) 1 d D U P C 2
C57B C -0.068(3) 0.7674(13) 1.029(2) 0.091(3) Uani 0.280(4) 1 d D U P C 2
H57C H -0.129004 0.780903 1.077706 0.110 Uiso 0.280(4) 1 calc R U P C 2
H57D H 0.000057 0.747563 1.069655 0.110 Uiso 0.280(4) 1 calc R U P C 2
Cl3C Cl 0.063(2) 0.7340(12) 1.0428(16) 0.095(4) Uani 0.072(2) 1 d D U P D 3
Cl4C Cl -0.127(2) 0.7845(14) 0.9020(19) 0.103(3) Uani 0.072(2) 1 d D U P D 3
C57C C -0.028(6) 0.807(3) 1.010(5) 0.091(3) Uani 0.072(2) 1 d D U P D 3
H57E H 0.023654 0.846350 0.991834 0.109 Uiso 0.072(2) 1 calc R U P D 3
H57F H -0.075614 0.820880 1.068738 0.109 Uiso 0.072(2) 1 calc R U P D 3


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C17 1.350(3) . ?
O1 B1 1.469(3) . ?
O2 C28 1.365(3) . ?
O2 B1 1.475(3) . ?
O3 C36 1.363(3) . ?
O3 B1 1.460(3) . ?
O4 C47 1.343(3) . ?
O4 B1 1.471(3) . ?
C17 C18 1.384(3) . ?
C17 C26 1.424(3) . ?
C18 C19 1.436(3) . ?
C18 C27 1.486(3) . ?
C019 C27 1.438(3) . ?
C019 C31 1.428(3) . ?
C019 C35 1.419(3) . ?
C19 C20 1.423(3) . ?
C19 C24 1.425(3) . ?
C20 H20 0.9300 . ?
C20 C21 1.369(4) . ?
C21 H21 0.9300 . ?
C21 C22 1.415(4) . ?
C22 H22 0.9300 . ?
C22 C23 1.368(4) . ?
C23 H23 0.9300 . ?
C23 C24 1.414(4) . ?
C24 C25 1.424(4) . ?
C25 H25 0.9300 . ?
C25 C26 1.361(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.385(3) . ?
C28 C29 1.417(3) . ?
C29 H29 0.9300 . ?
C29 C30 1.364(4) . ?
C30 H30 0.9300 . ?
C30 C31 1.419(4) . ?
C31 C32 1.425(3) . ?
C32 H32 0.9300 . ?
C32 C33 1.365(4) . ?
C33 H33 0.9300 . ?
C33 C34 1.408(3) . ?
C34 H34 0.9300 . ?
C34 C35 1.373(4) . ?
C35 H35 0.9300 . ?
C36 C37 1.380(3) . ?
C36 C45 1.420(3) . ?
C37 C38 1.440(3) . ?
C37 C46 1.489(3) . ?
C38 C39 1.424(3) . ?
C38 C43 1.428(3) . ?
C39 H39 0.9300 . ?
C39 C40 1.365(4) . ?
C40 H40 0.9300 . ?
C40 C41 1.410(4) . ?
C41 H41 0.9300 . ?
C41 C42 1.366(4) . ?
C42 H42 0.9300 . ?
C42 C43 1.420(3) . ?
C43 C44 1.414(4) . ?
C44 H44 0.9300 . ?
C44 C45 1.365(4) . ?
C45 H45 0.9300 . ?
C46 C47 1.388(3) . ?
C46 C55 1.437(3) . ?
C47 C48 1.419(3) . ?
C48 H48 0.9300 . ?
C48 C49 1.369(4) . ?
C49 H49 0.9300 . ?
C49 C50 1.410(4) . ?
C50 C51 1.423(4) . ?
C50 C55 1.428(3) . ?
C51 H51 0.9300 . ?
C51 C52 1.367(4) . ?
C52 H52 0.9300 . ?
C52 C53 1.411(4) . ?
C53 H53 0.9300 . ?
C53 C54 1.368(4) . ?
C54 H54 0.9300 . ?
C54 C55 1.425(4) . ?
P1 N1 1.635(2) . ?
P1 N2 1.624(2) . ?
P1 N3 1.641(2) . ?
P1 N4 1.633(2) . ?
N1 H1 0.83(4) . ?
N1 C1 1.500(3) . ?
N2 C5 1.486(3) . ?
N2 C8 1.488(3) . ?
N3 C9 1.487(3) . ?
N3 C12 1.483(3) . ?
N4 C13 1.489(4) . ?
N4 C16 1.485(4) . ?
C1 C2 1.522(4) . ?
C1 C3 1.527(4) . ?
C1 C4 1.526(4) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.515(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.524(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.529(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.537(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.514(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.525(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.518(4) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.506(5) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.521(4) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
Cl1A C56A 1.789(6) . ?
Cl2A C56A 1.741(10) . ?
C56A H56A 0.9700 . ?
C56A H56B 0.9700 . ?
Cl1B C56B 1.759(16) . ?
Cl2B C56B 1.783(15) . ?
C56B H56C 0.9700 . ?
C56B H56D 0.9700 . ?
Cl3A C57A 1.746(10) . ?
Cl4A C57A 1.761(12) . ?
C57A H57A 0.9700 . ?
C57A H57B 0.9700 . ?
Cl3B C57B 1.71(2) . ?
Cl4B C57B 1.80(2) . ?
C57B H57C 0.9700 . ?
C57B H57D 0.9700 . ?
Cl3C C57C 1.76(3) . ?
Cl4C C57C 1.78(3) . ?
C57C H57E 0.9700 . ?
C57C H57F 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C17 O1 B1 120.43(19) . . ?
C28 O2 B1 115.69(18) . . ?
C36 O3 B1 116.79(19) . . ?
C47 O4 B1 122.44(19) . . ?
O1 C17 C18 122.1(2) . . ?
O1 C17 C26 117.0(2) . . ?
C18 C17 C26 120.8(2) . . ?
C17 C18 C19 118.8(2) . . ?
C17 C18 C27 119.7(2) . . ?
C19 C18 C27 121.4(2) . . ?
C31 C019 C27 119.4(2) . . ?
C35 C019 C27 122.5(2) . . ?
C35 C019 C31 118.0(2) . . ?
C20 C19 C18 122.6(2) . . ?
C20 C19 C24 117.7(2) . . ?
C24 C19 C18 119.8(2) . . ?
C19 C20 H20 119.3 . . ?
C21 C20 C19 121.3(2) . . ?
C21 C20 H20 119.3 . . ?
C20 C21 H21 119.7 . . ?
C20 C21 C22 120.6(2) . . ?
C22 C21 H21 119.7 . . ?
C21 C22 H22 120.3 . . ?
C23 C22 C21 119.4(2) . . ?
C23 C22 H22 120.3 . . ?
C22 C23 H23 119.3 . . ?
C22 C23 C24 121.3(2) . . ?
C24 C23 H23 119.3 . . ?
C23 C24 C19 119.6(2) . . ?
C23 C24 C25 121.6(2) . . ?
C25 C24 C19 118.8(2) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 C24 120.8(2) . . ?
C26 C25 H25 119.6 . . ?
C17 C26 H26 119.7 . . ?
C25 C26 C17 120.5(2) . . ?
C25 C26 H26 119.7 . . ?
C019 C27 C18 122.5(2) . . ?
C28 C27 C18 118.9(2) . . ?
C28 C27 C019 118.5(2) . . ?
O2 C28 C27 120.8(2) . . ?
O2 C28 C29 117.9(2) . . ?
C27 C28 C29 121.2(2) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 C28 120.4(2) . . ?
C30 C29 H29 119.8 . . ?
C29 C30 H30 119.7 . . ?
C29 C30 C31 120.6(2) . . ?
C31 C30 H30 119.7 . . ?
C30 C31 C019 119.1(2) . . ?
C30 C31 C32 121.9(2) . . ?
C32 C31 C019 118.9(2) . . ?
C31 C32 H32 119.2 . . ?
C33 C32 C31 121.5(2) . . ?
C33 C32 H32 119.2 . . ?
C32 C33 H33 120.2 . . ?
C32 C33 C34 119.7(2) . . ?
C34 C33 H33 120.2 . . ?
C33 C34 H34 119.7 . . ?
C35 C34 C33 120.6(2) . . ?
C35 C34 H34 119.7 . . ?
C019 C35 H35 119.3 . . ?
C34 C35 C019 121.4(2) . . ?
C34 C35 H35 119.3 . . ?
O3 C36 C37 121.4(2) . . ?
O3 C36 C45 117.2(2) . . ?
C37 C36 C45 121.3(2) . . ?
C36 C37 C38 118.2(2) . . ?
C36 C37 C46 120.2(2) . . ?
C38 C37 C46 121.5(2) . . ?
C39 C38 C37 122.8(2) . . ?
C39 C38 C43 117.2(2) . . ?
C43 C38 C37 119.9(2) . . ?
C38 C39 H39 119.1 . . ?
C40 C39 C38 121.8(2) . . ?
C40 C39 H39 119.1 . . ?
C39 C40 H40 119.7 . . ?
C39 C40 C41 120.6(2) . . ?
C41 C40 H40 119.7 . . ?
C40 C41 H41 120.2 . . ?
C42 C41 C40 119.6(2) . . ?
C42 C41 H41 120.2 . . ?
C41 C42 H42 119.4 . . ?
C41 C42 C43 121.2(2) . . ?
C43 C42 H42 119.4 . . ?
C42 C43 C38 119.6(2) . . ?
C44 C43 C38 119.0(2) . . ?
C44 C43 C42 121.3(2) . . ?
C43 C44 H44 119.7 . . ?
C45 C44 C43 120.6(2) . . ?
C45 C44 H44 119.7 . . ?
C36 C45 H45 119.8 . . ?
C44 C45 C36 120.5(2) . . ?
C44 C45 H45 119.8 . . ?
C47 C46 C37 119.6(2) . . ?
C47 C46 C55 118.1(2) . . ?
C55 C46 C37 122.3(2) . . ?
O4 C47 C46 122.5(2) . . ?
O4 C47 C48 116.4(2) . . ?
C46 C47 C48 120.8(2) . . ?
C47 C48 H48 119.6 . . ?
C49 C48 C47 120.8(2) . . ?
C49 C48 H48 119.6 . . ?
C48 C49 H49 119.8 . . ?
C48 C49 C50 120.4(2) . . ?
C50 C49 H49 119.8 . . ?
C49 C50 C51 121.5(2) . . ?
C49 C50 C55 119.1(2) . . ?
C51 C50 C55 119.4(2) . . ?
C50 C51 H51 119.3 . . ?
C52 C51 C50 121.4(3) . . ?
C52 C51 H51 119.3 . . ?
C51 C52 H52 120.3 . . ?
C51 C52 C53 119.4(2) . . ?
C53 C52 H52 120.3 . . ?
C52 C53 H53 119.6 . . ?
C54 C53 C52 120.7(2) . . ?
C54 C53 H53 119.6 . . ?
C53 C54 H54 119.2 . . ?
C53 C54 C55 121.7(2) . . ?
C55 C54 H54 119.2 . . ?
C50 C55 C46 119.9(2) . . ?
C54 C55 C46 122.7(2) . . ?
C54 C55 C50 117.3(2) . . ?
O1 B1 O2 112.8(2) . . ?
O1 B1 O4 101.99(19) . . ?
O3 B1 O1 114.0(2) . . ?
O3 B1 O2 102.11(19) . . ?
O3 B1 O4 113.3(2) . . ?
O4 B1 O2 113.1(2) . . ?
N1 P1 N3 106.73(11) . . ?
N2 P1 N1 120.86(11) . . ?
N2 P1 N3 103.61(11) . . ?
N2 P1 N4 105.65(11) . . ?
N4 P1 N1 102.76(12) . . ?
N4 P1 N3 118.19(12) . . ?
P1 N1 H1 110(2) . . ?
C1 N1 P1 131.20(18) . . ?
C1 N1 H1 111(2) . . ?
C5 N2 P1 122.78(18) . . ?
C5 N2 C8 110.3(2) . . ?
C8 N2 P1 122.95(16) . . ?
C9 N3 P1 122.13(18) . . ?
C12 N3 P1 118.10(17) . . ?
C12 N3 C9 105.6(2) . . ?
C13 N4 P1 124.19(19) . . ?
C16 N4 P1 120.99(19) . . ?
C16 N4 C13 110.5(2) . . ?
N1 C1 C2 105.7(2) . . ?
N1 C1 C3 113.1(2) . . ?
N1 C1 C4 109.1(2) . . ?
C2 C1 C3 108.8(2) . . ?
C2 C1 C4 110.2(2) . . ?
C4 C1 C3 109.9(2) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 H5A 111.0 . . ?
N2 C5 H5B 111.0 . . ?
N2 C5 C6 103.6(2) . . ?
H5A C5 H5B 109.0 . . ?
C6 C5 H5A 111.0 . . ?
C6 C5 H5B 111.0 . . ?
C5 C6 H6A 111.3 . . ?
C5 C6 H6B 111.3 . . ?
C5 C6 C7 102.5(2) . . ?
H6A C6 H6B 109.2 . . ?
C7 C6 H6A 111.3 . . ?
C7 C6 H6B 111.3 . . ?
C6 C7 H7A 111.1 . . ?
C6 C7 H7B 111.1 . . ?
C6 C7 C8 103.5(2) . . ?
H7A C7 H7B 109.0 . . ?
C8 C7 H7A 111.1 . . ?
C8 C7 H7B 111.1 . . ?
N2 C8 C7 103.5(2) . . ?
N2 C8 H8A 111.1 . . ?
N2 C8 H8B 111.1 . . ?
C7 C8 H8A 111.1 . . ?
C7 C8 H8B 111.1 . . ?
H8A C8 H8B 109.0 . . ?
N3 C9 H9A 110.5 . . ?
N3 C9 H9B 110.5 . . ?
N3 C9 C10 106.0(2) . . ?
H9A C9 H9B 108.7 . . ?
C10 C9 H9A 110.5 . . ?
C10 C9 H9B 110.5 . . ?
C9 C10 H10A 110.6 . . ?
C9 C10 H10B 110.6 . . ?
H10A C10 H10B 108.7 . . ?
C11 C10 C9 105.8(2) . . ?
C11 C10 H10A 110.6 . . ?
C11 C10 H10B 110.6 . . ?
C10 C11 H11A 111.1 . . ?
C10 C11 H11B 111.1 . . ?
C10 C11 C12 103.5(2) . . ?
H11A C11 H11B 109.0 . . ?
C12 C11 H11A 111.1 . . ?
C12 C11 H11B 111.1 . . ?
N3 C12 C11 103.2(2) . . ?
N3 C12 H12A 111.1 . . ?
N3 C12 H12B 111.1 . . ?
C11 C12 H12A 111.1 . . ?
C11 C12 H12B 111.1 . . ?
H12A C12 H12B 109.1 . . ?
N4 C13 H13A 111.0 . . ?
N4 C13 H13B 111.0 . . ?
N4 C13 C14 103.6(2) . . ?
H13A C13 H13B 109.0 . . ?
C14 C13 H13A 111.0 . . ?
C14 C13 H13B 111.0 . . ?
C13 C14 H14A 111.0 . . ?
C13 C14 H14B 111.0 . . ?
H14A C14 H14B 109.0 . . ?
C15 C14 C13 103.7(3) . . ?
C15 C14 H14A 111.0 . . ?
C15 C14 H14B 111.0 . . ?
C14 C15 H15A 111.0 . . ?
C14 C15 H15B 111.0 . . ?
C14 C15 C16 103.8(2) . . ?
H15A C15 H15B 109.0 . . ?
C16 C15 H15A 111.0 . . ?
C16 C15 H15B 111.0 . . ?
N4 C16 C15 103.1(2) . . ?
N4 C16 H16A 111.1 . . ?
N4 C16 H16B 111.1 . . ?
C15 C16 H16A 111.1 . . ?
C15 C16 H16B 111.1 . . ?
H16A C16 H16B 109.1 . . ?
Cl1A C56A H56A 109.4 . . ?
Cl1A C56A H56B 109.4 . . ?
Cl2A C56A Cl1A 111.2(4) . . ?
Cl2A C56A H56A 109.4 . . ?
Cl2A C56A H56B 109.4 . . ?
H56A C56A H56B 108.0 . . ?
Cl1B C56B Cl2B 111.4(9) . . ?
Cl1B C56B H56C 109.4 . . ?
Cl1B C56B H56D 109.4 . . ?
Cl2B C56B H56C 109.4 . . ?
Cl2B C56B H56D 109.4 . . ?
H56C C56B H56D 108.0 . . ?
Cl3A C57A Cl4A 110.5(7) . . ?
Cl3A C57A H57A 109.6 . . ?
Cl3A C57A H57B 109.6 . . ?
Cl4A C57A H57A 109.6 . . ?
Cl4A C57A H57B 109.6 . . ?
H57A C57A H57B 108.1 . . ?
Cl3B C57B Cl4B 122.0(16) . . ?
Cl3B C57B H57C 106.8 . . ?
Cl3B C57B H57D 106.8 . . ?
Cl4B C57B H57C 106.8 . . ?
Cl4B C57B H57D 106.8 . . ?
H57C C57B H57D 106.7 . . ?
Cl3C C57C Cl4C 108(2) . . ?
Cl3C C57C H57E 110.1 . . ?
Cl3C C57C H57F 110.1 . . ?
Cl4C C57C H57E 110.1 . . ?
Cl4C C57C H57F 110.1 . . ?
H57E C57C H57F 108.4 . . ?

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
O1 C17 C18 C19 -176.7(2) . . . . ?
O1 C17 C18 C27 -1.1(3) . . . . ?
O1 C17 C26 C25 -178.5(2) . . . . ?
O2 C28 C29 C30 178.2(2) . . . . ?
O3 C36 C37 C38 -175.7(2) . . . . ?
O3 C36 C37 C46 -0.4(4) . . . . ?
O3 C36 C45 C44 -179.4(2) . . . . ?
O4 C47 C48 C49 -176.6(2) . . . . ?
C17 O1 B1 O2 -30.3(3) . . . . ?
C17 O1 B1 O3 85.6(3) . . . . ?
C17 O1 B1 O4 -151.9(2) . . . . ?
C17 C18 C19 C20 170.3(2) . . . . ?
C17 C18 C19 C24 -7.3(3) . . . . ?
C17 C18 C27 C019 128.9(2) . . . . ?
C17 C18 C27 C28 -49.6(3) . . . . ?
C18 C17 C26 C25 -2.2(4) . . . . ?
C18 C19 C20 C21 180.0(2) . . . . ?
C18 C19 C24 C23 -178.8(2) . . . . ?
C18 C19 C24 C25 2.5(4) . . . . ?
C18 C27 C28 O2 5.5(3) . . . . ?
C18 C27 C28 C29 -172.5(2) . . . . ?
C019 C27 C28 O2 -173.1(2) . . . . ?
C019 C27 C28 C29 8.9(3) . . . . ?
C019 C31 C32 C33 -0.8(4) . . . . ?
C19 C18 C27 C019 -55.6(3) . . . . ?
C19 C18 C27 C28 125.9(2) . . . . ?
C19 C20 C21 C22 -0.5(4) . . . . ?
C19 C24 C25 C26 2.5(4) . . . . ?
C20 C19 C24 C23 3.5(4) . . . . ?
C20 C19 C24 C25 -175.2(2) . . . . ?
C20 C21 C22 C23 2.3(4) . . . . ?
C21 C22 C23 C24 -1.1(4) . . . . ?
C22 C23 C24 C19 -1.8(4) . . . . ?
C22 C23 C24 C25 176.8(3) . . . . ?
C23 C24 C25 C26 -176.2(3) . . . . ?
C24 C19 C20 C21 -2.4(4) . . . . ?
C24 C25 C26 C17 -2.8(4) . . . . ?
C26 C17 C18 C19 7.2(3) . . . . ?
C26 C17 C18 C27 -177.2(2) . . . . ?
C27 C18 C19 C20 -5.2(4) . . . . ?
C27 C18 C19 C24 177.2(2) . . . . ?
C27 C019 C31 C30 -0.2(3) . . . . ?
C27 C019 C31 C32 176.9(2) . . . . ?
C27 C019 C35 C34 -176.4(2) . . . . ?
C27 C28 C29 C30 -3.8(3) . . . . ?
C28 O2 B1 O1 -53.6(3) . . . . ?
C28 O2 B1 O3 -176.42(18) . . . . ?
C28 O2 B1 O4 61.5(3) . . . . ?
C28 C29 C30 C31 -3.6(4) . . . . ?
C29 C30 C31 C019 5.5(3) . . . . ?
C29 C30 C31 C32 -171.6(2) . . . . ?
C30 C31 C32 C33 176.3(2) . . . . ?
C31 C019 C27 C18 174.6(2) . . . . ?
C31 C019 C27 C28 -6.8(3) . . . . ?
C31 C019 C35 C34 0.8(3) . . . . ?
C31 C32 C33 C34 1.4(4) . . . . ?
C32 C33 C34 C35 -0.9(4) . . . . ?
C33 C34 C35 C019 -0.2(4) . . . . ?
C35 C019 C27 C18 -8.3(4) . . . . ?
C35 C019 C27 C28 170.3(2) . . . . ?
C35 C019 C31 C30 -177.5(2) . . . . ?
C35 C019 C31 C32 -0.3(3) . . . . ?
C36 O3 B1 O1 67.5(3) . . . . ?
C36 O3 B1 O2 -170.44(19) . . . . ?
C36 O3 B1 O4 -48.5(3) . . . . ?
C36 C37 C38 C39 168.3(2) . . . . ?
C36 C37 C38 C43 -7.3(3) . . . . ?
C36 C37 C46 C47 -47.4(3) . . . . ?
C36 C37 C46 C55 133.3(3) . . . . ?
C37 C36 C45 C44 -2.5(4) . . . . ?
C37 C38 C39 C40 -177.2(3) . . . . ?
C37 C38 C43 C42 178.4(2) . . . . ?
C37 C38 C43 C44 2.0(4) . . . . ?
C37 C46 C47 O4 4.0(3) . . . . ?
C37 C46 C47 C48 -170.1(2) . . . . ?
C37 C46 C55 C50 169.3(2) . . . . ?
C37 C46 C55 C54 -11.9(4) . . . . ?
C38 C37 C46 C47 127.8(3) . . . . ?
C38 C37 C46 C55 -51.5(3) . . . . ?
C38 C39 C40 C41 -0.4(4) . . . . ?
C38 C43 C44 C45 3.3(4) . . . . ?
C39 C38 C43 C42 2.6(3) . . . . ?
C39 C38 C43 C44 -173.8(2) . . . . ?
C39 C40 C41 C42 1.3(4) . . . . ?
C40 C41 C42 C43 -0.2(4) . . . . ?
C41 C42 C43 C38 -1.8(4) . . . . ?
C41 C42 C43 C44 174.6(3) . . . . ?
C42 C43 C44 C45 -173.1(2) . . . . ?
C43 C38 C39 C40 -1.5(4) . . . . ?
C43 C44 C45 C36 -3.1(4) . . . . ?
C45 C36 C37 C38 7.6(4) . . . . ?
C45 C36 C37 C46 -177.1(2) . . . . ?
C46 C37 C38 C39 -6.9(4) . . . . ?
C46 C37 C38 C43 177.5(2) . . . . ?
C46 C47 C48 C49 -2.1(4) . . . . ?
C47 O4 B1 O1 -156.47(19) . . . . ?
C47 O4 B1 O2 82.1(3) . . . . ?
C47 O4 B1 O3 -33.5(3) . . . . ?
C47 C46 C55 C50 -10.0(3) . . . . ?
C47 C46 C55 C54 168.8(2) . . . . ?
C47 C48 C49 C50 -4.5(4) . . . . ?
C48 C49 C50 C51 -174.9(3) . . . . ?
C48 C49 C50 C55 3.6(4) . . . . ?
C49 C50 C51 C52 176.1(3) . . . . ?
C49 C50 C55 C46 3.7(4) . . . . ?
C49 C50 C55 C54 -175.2(2) . . . . ?
C50 C51 C52 C53 -0.2(5) . . . . ?
C51 C50 C55 C46 -177.8(2) . . . . ?
C51 C50 C55 C54 3.4(4) . . . . ?
C51 C52 C53 C54 1.9(4) . . . . ?
C52 C53 C54 C55 -0.8(4) . . . . ?
C53 C54 C55 C46 179.4(2) . . . . ?
C53 C54 C55 C50 -1.8(4) . . . . ?
C55 C46 C47 O4 -176.6(2) . . . . ?
C55 C46 C47 C48 9.3(3) . . . . ?
C55 C50 C51 C52 -2.4(4) . . . . ?
B1 O1 C17 C18 63.0(3) . . . . ?
B1 O1 C17 C26 -120.8(2) . . . . ?
B1 O2 C28 C27 68.1(3) . . . . ?
B1 O2 C28 C29 -113.8(2) . . . . ?
B1 O3 C36 C37 69.2(3) . . . . ?
B1 O3 C36 C45 -113.9(2) . . . . ?
B1 O4 C47 C46 58.9(3) . . . . ?
B1 O4 C47 C48 -126.7(2) . . . . ?
P1 N1 C1 C2 159.7(2) . . . . ?
P1 N1 C1 C3 40.7(3) . . . . ?
P1 N1 C1 C4 -81.9(3) . . . . ?
P1 N2 C5 C6 -140.85(19) . . . . ?
P1 N2 C8 C7 166.11(18) . . . . ?
P1 N3 C9 C10 -114.8(3) . . . . ?
P1 N3 C12 C11 102.0(2) . . . . ?
P1 N4 C13 C14 -146.4(2) . . . . ?
P1 N4 C16 C15 171.3(2) . . . . ?
N1 P1 N2 C5 74.6(2) . . . . ?
N1 P1 N2 C8 -80.7(2) . . . . ?
N1 P1 N3 C9 -40.9(2) . . . . ?
N1 P1 N3 C12 -174.94(19) . . . . ?
N1 P1 N4 C13 -159.4(2) . . . . ?
N1 P1 N4 C16 46.0(2) . . . . ?
N2 P1 N1 C1 53.7(3) . . . . ?
N2 P1 N3 C9 -169.5(2) . . . . ?
N2 P1 N3 C12 56.5(2) . . . . ?
N2 P1 N4 C13 -31.9(3) . . . . ?
N2 P1 N4 C16 173.6(2) . . . . ?
N2 C5 C6 C7 -35.4(3) . . . . ?
N3 P1 N1 C1 -64.1(3) . . . . ?
N3 P1 N2 C5 -166.1(2) . . . . ?
N3 P1 N2 C8 38.7(2) . . . . ?
N3 P1 N4 C13 83.4(2) . . . . ?
N3 P1 N4 C16 -71.1(2) . . . . ?
N3 C9 C10 C11 0.1(4) . . . . ?
N4 P1 N1 C1 170.9(2) . . . . ?
N4 P1 N2 C5 -41.1(2) . . . . ?
N4 P1 N2 C8 163.59(19) . . . . ?
N4 P1 N3 C9 74.1(2) . . . . ?
N4 P1 N3 C12 -59.9(2) . . . . ?
N4 C13 C14 C15 -30.6(3) . . . . ?
C5 N2 C8 C7 8.1(3) . . . . ?
C5 C6 C7 C8 40.9(3) . . . . ?
C6 C7 C8 N2 -30.1(3) . . . . ?
C8 N2 C5 C6 17.2(3) . . . . ?
C9 N3 C12 C11 -38.8(3) . . . . ?
C9 C10 C11 C12 -23.3(3) . . . . ?
C10 C11 C12 N3 38.2(3) . . . . ?
C12 N3 C9 C10 24.0(3) . . . . ?
C13 N4 C16 C15 13.6(3) . . . . ?
C13 C14 C15 C16 39.6(3) . . . . ?
C14 C15 C16 N4 -32.5(3) . . . . ?
C16 N4 C13 C14 10.5(3) . . . . ?

_olex2_date_sample_data_collection 2020-09-15
_olex2_date_sample_submission    2020-09-15
_olex2_exptl_crystal_mounting_method 'MiTeGen 100 um MicroLoop'
_olex2_submission_original_sample_id kre20_31
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   6723
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.298
_oxdiff_exptl_absorpt_empirical_full_min 0.776

# 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_RS-2
_database_code_depnum_ccdc_archive 'CCDC 2058924'
loop_
_audit_author_name
_audit_author_address
'Daniel Unruh'
;Texas Tech University
United States of America
;
_audit_update_record             
;
2021-02-01 deposited with the CCDC.	2021-03-23 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT911_RS-2                
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         61 Report
RESPONSE: These reflections were omitted during the absorption correction.
;
# end Validation Reply Form
_audit_creation_date             2021-01-15
_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
loop_
_audit_author_email
Shipra.Garg@ttu.edu
daniel.unruh@ttu.edu
Clemens.krempner@ttu.edu
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C26 H12 B F5 O2)'
_chemical_formula_sum            'C52 H24 B2 F10 O4'
_chemical_formula_weight         924.33
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   7.5800(2)
_cell_length_b                   15.1022(4)
_cell_length_c                   19.1160(4)
_cell_angle_alpha                98.515(2)
_cell_angle_beta                 97.647(2)
_cell_angle_gamma                92.998(2)
_cell_volume                     2139.13(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    13270
_cell_measurement_theta_min      2.348
_cell_measurement_theta_max      76.724
_shelx_estimated_absorpt_T_max   0.986
_shelx_estimated_absorpt_T_min   0.832
_exptl_absorpt_coefficient_mu    1.026
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             936
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-0.41 -4.84 11.60 0.0150
0.41 4.84 -11.60 0.0206
4.91 -1.27 -0.58 0.0898
-4.92 1.17 0.82 0.0954
0.13 7.25 6.66 0.0128
-0.13 -7.25 -6.66 0.0010
-0.41 -4.84 11.60 0.0150
0.41 4.84 -11.60 0.0206
4.91 -1.27 -0.58 0.0898
-4.92 1.17 0.82 0.0954
0.13 7.25 6.66 0.0128
-0.13 -7.25 -6.66 0.0010

_exptl_crystal_size_max          0.186
_exptl_crystal_size_mid          0.039
_exptl_crystal_size_min          0.014
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            37333
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         77.188
_diffrn_reflns_theta_min         2.361
_diffrn_ambient_temperature      99.95
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6932
_reflns_number_total             8671
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.0014(3)
_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   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         8671
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0508
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1003P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1382
_refine_ls_wR_factor_ref         0.1461
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C15(H15), C16(H16), C20(H20),
 C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C36(H36), C37(H37), C38(H38),
  C39(H39), C41(H41), C42(H42), C46(H46), C47(H47), C48(H48), C49(H49),
 C51(H51), C52(H52)
;
_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
F1 F -0.19609(14) 0.03483(7) 0.20728(6) 0.0335(2) Uani 1 1 d . . . . .
F2 F -0.15304(16) -0.07681(8) 0.30500(6) 0.0385(3) Uani 1 1 d . . . . .
F3 F -0.05511(16) -0.24537(7) 0.26748(6) 0.0397(3) Uani 1 1 d . . . . .
F4 F -0.00682(17) -0.30391(7) 0.13070(6) 0.0418(3) Uani 1 1 d . . . . .
F5 F -0.05719(15) -0.19493(7) 0.03176(6) 0.0340(2) Uani 1 1 d . . . . .
F6 F -0.18858(14) 0.28089(6) 0.59965(5) 0.0308(2) Uani 1 1 d . . . . .
F7 F -0.15146(15) 0.10571(7) 0.55658(6) 0.0372(3) Uani 1 1 d . . . . .
F8 F -0.07068(16) 0.04982(6) 0.42410(6) 0.0388(3) Uani 1 1 d . . . . .
F9 F -0.03615(16) 0.16966(7) 0.33298(6) 0.0375(3) Uani 1 1 d . . . . .
F10 F -0.08525(14) 0.34371(6) 0.37332(5) 0.0300(2) Uani 1 1 d . . . . .
O1 O -0.09009(15) 0.07654(8) 0.06634(6) 0.0265(3) Uani 1 1 d . . . . .
O2 O -0.25929(15) -0.04415(7) -0.00387(6) 0.0248(2) Uani 1 1 d . . . . .
O3 O -0.26273(14) 0.46771(7) 0.47499(6) 0.0227(2) Uani 1 1 d . . . . .
O4 O -0.05448(14) 0.46881(7) 0.57563(6) 0.0235(2) Uani 1 1 d . . . . .
C1 C -0.1278(2) -0.07518(11) 0.11607(9) 0.0240(3) Uani 1 1 d . . . . .
C2 C -0.1513(2) -0.04899(11) 0.18655(9) 0.0260(3) Uani 1 1 d . . . . .
C3 C -0.1300(2) -0.10511(12) 0.23758(9) 0.0289(4) Uani 1 1 d . . . . .
C4 C -0.0816(2) -0.19101(12) 0.21833(10) 0.0302(4) Uani 1 1 d . . . . .
C5 C -0.0571(2) -0.22044(11) 0.14897(10) 0.0300(4) Uani 1 1 d . . . . .
C6 C -0.0825(2) -0.16313(11) 0.09883(9) 0.0261(3) Uani 1 1 d . . . . .
C7 C 0.0244(2) 0.13825(11) 0.11450(9) 0.0251(3) Uani 1 1 d . . . . .
C8 C 0.1960(2) 0.12145(11) 0.13914(8) 0.0236(3) Uani 1 1 d . . . . .
C9 C 0.3128(2) 0.19539(10) 0.17842(9) 0.0241(3) Uani 1 1 d . . . . .
C10 C 0.4953(2) 0.18540(11) 0.20208(9) 0.0264(3) Uani 1 1 d . . . . .
H10 H 0.540761 0.127930 0.193591 0.032 Uiso 1 1 calc R U . . .
C11 C 0.6068(2) 0.25706(12) 0.23685(9) 0.0291(4) Uani 1 1 d . . . . .
H11 H 0.728312 0.248745 0.252404 0.035 Uiso 1 1 calc R U . . .
C12 C 0.5432(2) 0.34329(11) 0.24987(9) 0.0294(4) Uani 1 1 d . . . . .
H12 H 0.621637 0.392783 0.273892 0.035 Uiso 1 1 calc R U . . .
C13 C 0.3684(2) 0.35534(11) 0.22783(9) 0.0291(4) Uani 1 1 d . . . . .
H13 H 0.326307 0.413537 0.236570 0.035 Uiso 1 1 calc R U . . .
C14 C 0.2487(2) 0.28229(11) 0.19207(9) 0.0271(3) Uani 1 1 d . . . . .
C15 C 0.0673(2) 0.29342(11) 0.16787(10) 0.0302(4) Uani 1 1 d . . . . .
H15 H 0.021084 0.350356 0.178595 0.036 Uiso 1 1 calc R U . . .
C16 C -0.0416(2) 0.22331(12) 0.12938(10) 0.0298(4) Uani 1 1 d . . . . .
H16 H -0.162237 0.231939 0.112604 0.036 Uiso 1 1 calc R U . . .
C17 C -0.2964(2) 0.00580(11) -0.05935(9) 0.0242(3) Uani 1 1 d . . . . .
C18 C -0.2650(2) -0.03079(10) -0.12588(9) 0.0232(3) Uani 1 1 d . . . . .
C19 C -0.3039(2) 0.01892(11) -0.18392(9) 0.0247(3) Uani 1 1 d . . . . .
C20 C -0.2660(2) -0.01231(11) -0.25358(9) 0.0273(3) Uani 1 1 d . . . . .
H20 H -0.218969 -0.069196 -0.263434 0.033 Uiso 1 1 calc R U . . .
C21 C -0.2966(2) 0.03898(12) -0.30690(10) 0.0326(4) Uani 1 1 d . . . . .
H21 H -0.268588 0.017569 -0.353107 0.039 Uiso 1 1 calc R U . . .
C22 C -0.3688(2) 0.12266(12) -0.29420(10) 0.0341(4) Uani 1 1 d . . . . .
H22 H -0.388683 0.157568 -0.331583 0.041 Uiso 1 1 calc R U . . .
C23 C -0.4105(2) 0.15385(12) -0.22795(10) 0.0311(4) Uani 1 1 d . . . . .
H23 H -0.462612 0.209662 -0.220044 0.037 Uiso 1 1 calc R U . . .
C24 C -0.3767(2) 0.10369(11) -0.17060(10) 0.0269(4) Uani 1 1 d . . . . .
C25 C -0.4118(2) 0.13667(11) -0.10129(10) 0.0277(4) Uani 1 1 d . . . . .
H25 H -0.463671 0.192472 -0.092812 0.033 Uiso 1 1 calc R U . . .
C26 C -0.3722(2) 0.08947(11) -0.04589(9) 0.0264(3) Uani 1 1 d . . . . .
H26 H -0.395255 0.112449 0.000764 0.032 Uiso 1 1 calc R U . . .
C27 C -0.1373(2) 0.31912(10) 0.48846(9) 0.0228(3) Uani 1 1 d . . . . .
C28 C -0.1532(2) 0.25492(11) 0.53272(9) 0.0247(3) Uani 1 1 d . . . . .
C29 C -0.1348(2) 0.16518(11) 0.51183(10) 0.0277(4) Uani 1 1 d . . . . .
C30 C -0.0948(2) 0.13623(11) 0.44439(10) 0.0291(4) Uani 1 1 d . . . . .
C31 C -0.0782(2) 0.19747(11) 0.39779(9) 0.0273(3) Uani 1 1 d . . . . .
C32 C -0.1025(2) 0.28663(11) 0.42011(9) 0.0249(3) Uani 1 1 d . . . . .
C33 C -0.2902(2) 0.55783(10) 0.49613(9) 0.0217(3) Uani 1 1 d . . . . .
C34 C -0.2759(2) 0.61633(10) 0.44787(9) 0.0212(3) Uani 1 1 d . . . . .
C35 C -0.3081(2) 0.70879(10) 0.46914(9) 0.0221(3) Uani 1 1 d . . . . .
C36 C -0.2869(2) 0.77564(11) 0.42518(9) 0.0235(3) Uani 1 1 d . . . . .
H36 H -0.249554 0.759336 0.379803 0.028 Uiso 1 1 calc R U . . .
C37 C -0.3194(2) 0.86322(11) 0.44700(9) 0.0262(3) Uani 1 1 d . . . . .
H37 H -0.304289 0.906640 0.416634 0.031 Uiso 1 1 calc R U . . .
C38 C -0.3747(2) 0.88929(11) 0.51381(10) 0.0279(4) Uani 1 1 d . . . . .
H38 H -0.398449 0.949932 0.528146 0.034 Uiso 1 1 calc R U . . .
C39 C -0.3944(2) 0.82714(11) 0.55844(9) 0.0262(3) Uani 1 1 d . . . . .
H39 H -0.430998 0.845182 0.603719 0.031 Uiso 1 1 calc R U . . .
C40 C -0.3605(2) 0.73624(11) 0.53744(9) 0.0230(3) Uani 1 1 d . . . . .
C41 C -0.3765(2) 0.67194(11) 0.58363(9) 0.0247(3) Uani 1 1 d . . . . .
H41 H -0.411712 0.689830 0.629186 0.030 Uiso 1 1 calc R U . . .
C42 C -0.3421(2) 0.58478(11) 0.56373(9) 0.0228(3) Uani 1 1 d . . . . .
H42 H -0.353092 0.542406 0.595285 0.027 Uiso 1 1 calc R U . . .
C43 C 0.0641(2) 0.45013(10) 0.63193(9) 0.0222(3) Uani 1 1 d . . . . .
C44 C 0.2254(2) 0.41486(10) 0.62399(9) 0.0217(3) Uani 1 1 d . . . . .
C45 C 0.3458(2) 0.40912(10) 0.68775(9) 0.0222(3) Uani 1 1 d . . . . .
C46 C 0.5213(2) 0.38155(10) 0.68536(9) 0.0253(3) Uani 1 1 d . . . . .
H46 H 0.561521 0.366727 0.640376 0.030 Uiso 1 1 calc R U . . .
C47 C 0.6341(2) 0.37584(11) 0.74661(10) 0.0279(4) Uani 1 1 d . . . . .
H47 H 0.750379 0.356344 0.743541 0.033 Uiso 1 1 calc R U . . .
C48 C 0.5785(2) 0.39881(12) 0.81437(10) 0.0321(4) Uani 1 1 d . . . . .
H48 H 0.657177 0.394796 0.856640 0.039 Uiso 1 1 calc R U . . .
C49 C 0.4109(2) 0.42682(11) 0.81881(9) 0.0304(4) Uani 1 1 d . . . . .
H49 H 0.373622 0.441912 0.864326 0.037 Uiso 1 1 calc R U . . .
C50 C 0.2921(2) 0.43356(10) 0.75594(9) 0.0251(3) Uani 1 1 d . . . . .
C51 C 0.1218(2) 0.46698(11) 0.76030(9) 0.0267(3) Uani 1 1 d . . . . .
H51 H 0.083788 0.482576 0.805619 0.032 Uiso 1 1 calc R U . . .
C52 C 0.0124(2) 0.47683(11) 0.69958(9) 0.0248(3) Uani 1 1 d . . . . .
H52 H -0.099180 0.501810 0.702973 0.030 Uiso 1 1 calc R U . . .
B1 B -0.1549(2) -0.01005(12) 0.05894(10) 0.0234(4) Uani 1 1 d . . . . .
B2 B -0.1482(2) 0.42195(12) 0.51550(10) 0.0221(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
F1 C2 1.344(2) . ?
F2 C3 1.334(2) . ?
F3 C4 1.3388(19) . ?
F4 C5 1.346(2) . ?
F5 C6 1.3430(19) . ?
F6 C28 1.3479(19) . ?
F7 C29 1.3412(19) . ?
F8 C30 1.3343(19) . ?
F9 C31 1.333(2) . ?
F10 C32 1.3446(18) . ?
O1 C7 1.385(2) . ?
O1 B1 1.353(2) . ?
O2 C17 1.3973(19) . ?
O2 B1 1.362(2) . ?
O3 C33 1.3958(18) . ?
O3 B2 1.369(2) . ?
O4 C43 1.3802(19) . ?
O4 B2 1.348(2) . ?
C1 C2 1.384(2) . ?
C1 C6 1.392(2) . ?
C1 B1 1.575(2) . ?
C2 C3 1.383(2) . ?
C3 C4 1.378(3) . ?
C4 C5 1.375(3) . ?
C5 C6 1.385(2) . ?
C7 C8 1.373(2) . ?
C7 C16 1.407(2) . ?
C8 C9 1.438(2) . ?
C8 C18 1.490(2) 2 ?
C9 C10 1.420(2) . ?
C9 C14 1.423(2) . ?
C10 H10 0.9500 . ?
C10 C11 1.367(2) . ?
C11 H11 0.9500 . ?
C11 C12 1.411(2) . ?
C12 H12 0.9500 . ?
C12 C13 1.365(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.419(2) . ?
C14 C15 1.418(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.364(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.366(2) . ?
C17 C26 1.419(2) . ?
C18 C19 1.437(2) . ?
C19 C20 1.417(2) . ?
C19 C24 1.422(2) . ?
C20 H20 0.9500 . ?
C20 C21 1.372(2) . ?
C21 H21 0.9500 . ?
C21 C22 1.404(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.368(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.426(2) . ?
C24 C25 1.410(3) . ?
C25 H25 0.9500 . ?
C25 C26 1.371(2) . ?
C26 H26 0.9500 . ?
C27 C28 1.388(2) . ?
C27 C32 1.390(2) . ?
C27 B2 1.572(2) . ?
C28 C29 1.375(2) . ?
C29 C30 1.377(3) . ?
C30 C31 1.388(2) . ?
C31 C32 1.381(2) . ?
C33 C34 1.379(2) . ?
C33 C42 1.409(2) . ?
C34 C35 1.438(2) . ?
C34 C44 1.491(2) 2_566 ?
C35 C36 1.422(2) . ?
C35 C40 1.425(2) . ?
C36 H36 0.9500 . ?
C36 C37 1.372(2) . ?
C37 H37 0.9500 . ?
C37 C38 1.405(2) . ?
C38 H38 0.9500 . ?
C38 C39 1.374(2) . ?
C39 H39 0.9500 . ?
C39 C40 1.419(2) . ?
C40 C41 1.417(2) . ?
C41 H41 0.9500 . ?
C41 C42 1.364(2) . ?
C42 H42 0.9500 . ?
C43 C44 1.376(2) . ?
C43 C52 1.409(2) . ?
C44 C45 1.439(2) . ?
C45 C46 1.419(2) . ?
C45 C50 1.420(2) . ?
C46 H46 0.9500 . ?
C46 C47 1.371(2) . ?
C47 H47 0.9500 . ?
C47 C48 1.416(3) . ?
C48 H48 0.9500 . ?
C48 C49 1.369(3) . ?
C49 H49 0.9500 . ?
C49 C50 1.422(2) . ?
C50 C51 1.418(2) . ?
C51 H51 0.9500 . ?
C51 C52 1.366(2) . ?
C52 H52 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
B1 O1 C7 139.16(13) . . ?
B1 O2 C17 122.68(13) . . ?
B2 O3 C33 122.19(13) . . ?
B2 O4 C43 136.50(13) . . ?
C2 C1 C6 115.67(15) . . ?
C2 C1 B1 121.92(15) . . ?
C6 C1 B1 122.39(15) . . ?
F1 C2 C1 119.22(14) . . ?
F1 C2 C3 117.70(15) . . ?
C3 C2 C1 123.07(16) . . ?
F2 C3 C2 121.01(16) . . ?
F2 C3 C4 119.81(15) . . ?
C4 C3 C2 119.17(16) . . ?
F3 C4 C3 120.00(16) . . ?
F3 C4 C5 119.93(16) . . ?
C5 C4 C3 120.06(16) . . ?
F4 C5 C4 119.83(15) . . ?
F4 C5 C6 120.78(16) . . ?
C4 C5 C6 119.38(16) . . ?
F5 C6 C1 120.16(14) . . ?
F5 C6 C5 117.20(15) . . ?
C5 C6 C1 122.61(16) . . ?
O1 C7 C16 114.41(14) . . ?
C8 C7 O1 122.80(15) . . ?
C8 C7 C16 122.37(16) . . ?
C7 C8 C9 117.89(15) . . ?
C7 C8 C18 122.73(15) . 2 ?
C9 C8 C18 119.38(14) . 2 ?
C10 C9 C8 121.72(15) . . ?
C10 C9 C14 118.10(15) . . ?
C14 C9 C8 120.13(15) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 C9 121.13(16) . . ?
C11 C10 H10 119.4 . . ?
C10 C11 H11 119.7 . . ?
C10 C11 C12 120.64(16) . . ?
C12 C11 H11 119.7 . . ?
C11 C12 H12 120.1 . . ?
C13 C12 C11 119.78(16) . . ?
C13 C12 H12 120.1 . . ?
C12 C13 H13 119.5 . . ?
C12 C13 C14 121.05(16) . . ?
C14 C13 H13 119.5 . . ?
C13 C14 C9 119.28(16) . . ?
C15 C14 C9 118.67(15) . . ?
C15 C14 C13 122.04(16) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 C14 120.76(16) . . ?
C16 C15 H15 119.6 . . ?
C7 C16 H16 120.0 . . ?
C15 C16 C7 120.09(16) . . ?
C15 C16 H16 120.0 . . ?
O2 C17 C26 119.68(15) . . ?
C18 C17 O2 117.76(14) . . ?
C18 C17 C26 122.49(15) . . ?
C17 C18 C8 121.17(14) . 2 ?
C17 C18 C19 118.76(15) . . ?
C19 C18 C8 120.06(15) . 2 ?
C20 C19 C18 122.06(15) . . ?
C20 C19 C24 118.81(15) . . ?
C24 C19 C18 119.09(15) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 C19 120.51(16) . . ?
C21 C20 H20 119.7 . . ?
C20 C21 H21 119.5 . . ?
C20 C21 C22 121.00(17) . . ?
C22 C21 H21 119.5 . . ?
C21 C22 H22 120.0 . . ?
C23 C22 C21 119.93(16) . . ?
C23 C22 H22 120.0 . . ?
C22 C23 H23 119.6 . . ?
C22 C23 C24 120.86(17) . . ?
C24 C23 H23 119.6 . . ?
C19 C24 C23 118.86(17) . . ?
C25 C24 C19 119.59(15) . . ?
C25 C24 C23 121.54(16) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 C24 121.05(15) . . ?
C26 C25 H25 119.5 . . ?
C17 C26 H26 120.5 . . ?
C25 C26 C17 118.96(16) . . ?
C25 C26 H26 120.5 . . ?
C28 C27 C32 115.38(15) . . ?
C28 C27 B2 121.97(15) . . ?
C32 C27 B2 122.57(14) . . ?
F6 C28 C27 119.05(14) . . ?
F6 C28 C29 117.63(14) . . ?
C29 C28 C27 123.32(16) . . ?
F7 C29 C28 121.07(16) . . ?
F7 C29 C30 119.50(15) . . ?
C28 C29 C30 119.41(15) . . ?
F8 C30 C29 120.17(15) . . ?
F8 C30 C31 120.14(17) . . ?
C29 C30 C31 119.69(15) . . ?
F9 C31 C30 119.65(15) . . ?
F9 C31 C32 121.22(15) . . ?
C32 C31 C30 119.12(16) . . ?
F10 C32 C27 119.75(14) . . ?
F10 C32 C31 117.20(15) . . ?
C31 C32 C27 123.02(15) . . ?
O3 C33 C42 119.30(13) . . ?
C34 C33 O3 118.23(14) . . ?
C34 C33 C42 122.35(14) . . ?
C33 C34 C35 118.18(15) . . ?
C33 C34 C44 121.05(14) . 2_566 ?
C35 C34 C44 120.76(13) . 2_566 ?
C36 C35 C34 122.77(15) . . ?
C36 C35 C40 117.68(14) . . ?
C40 C35 C34 119.54(14) . . ?
C35 C36 H36 119.4 . . ?
C37 C36 C35 121.29(15) . . ?
C37 C36 H36 119.4 . . ?
C36 C37 H37 119.7 . . ?
C36 C37 C38 120.62(15) . . ?
C38 C37 H37 119.7 . . ?
C37 C38 H38 120.0 . . ?
C39 C38 C37 120.04(15) . . ?
C39 C38 H38 120.0 . . ?
C38 C39 H39 119.7 . . ?
C38 C39 C40 120.53(16) . . ?
C40 C39 H39 119.7 . . ?
C39 C40 C35 119.82(14) . . ?
C41 C40 C35 119.11(14) . . ?
C41 C40 C39 121.06(15) . . ?
C40 C41 H41 119.5 . . ?
C42 C41 C40 121.05(15) . . ?
C42 C41 H41 119.5 . . ?
C33 C42 H42 120.1 . . ?
C41 C42 C33 119.71(14) . . ?
C41 C42 H42 120.1 . . ?
O4 C43 C52 114.03(14) . . ?
C44 C43 O4 123.58(15) . . ?
C44 C43 C52 122.22(15) . . ?
C43 C44 C34 121.76(14) . 2_566 ?
C43 C44 C45 117.77(15) . . ?
C45 C44 C34 120.47(14) . 2_566 ?
C46 C45 C44 122.12(15) . . ?
C46 C45 C50 117.80(15) . . ?
C50 C45 C44 120.06(15) . . ?
C45 C46 H46 119.3 . . ?
C47 C46 C45 121.42(16) . . ?
C47 C46 H46 119.3 . . ?
C46 C47 H47 119.8 . . ?
C46 C47 C48 120.43(16) . . ?
C48 C47 H47 119.8 . . ?
C47 C48 H48 120.1 . . ?
C49 C48 C47 119.80(16) . . ?
C49 C48 H48 120.1 . . ?
C48 C49 H49 119.7 . . ?
C48 C49 C50 120.66(17) . . ?
C50 C49 H49 119.7 . . ?
C45 C50 C49 119.86(16) . . ?
C51 C50 C45 119.20(15) . . ?
C51 C50 C49 120.92(16) . . ?
C50 C51 H51 119.9 . . ?
C52 C51 C50 120.25(15) . . ?
C52 C51 H51 119.9 . . ?
C43 C52 H52 119.8 . . ?
C51 C52 C43 120.34(15) . . ?
C51 C52 H52 119.8 . . ?
O1 B1 O2 116.70(14) . . ?
O1 B1 C1 127.09(15) . . ?
O2 B1 C1 116.18(14) . . ?
O3 B2 C27 117.51(15) . . ?
O4 B2 O3 117.16(14) . . ?
O4 B2 C27 125.33(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
F1 C2 C3 F2 -0.1(2) . . . . ?
F1 C2 C3 C4 -179.07(15) . . . . ?
F2 C3 C4 F3 -1.0(3) . . . . ?
F2 C3 C4 C5 -179.79(15) . . . . ?
F3 C4 C5 F4 0.1(3) . . . . ?
F3 C4 C5 C6 -179.12(16) . . . . ?
F4 C5 C6 F5 0.9(2) . . . . ?
F4 C5 C6 C1 -177.47(15) . . . . ?
F6 C28 C29 F7 0.0(2) . . . . ?
F6 C28 C29 C30 -178.60(15) . . . . ?
F7 C29 C30 F8 -0.8(2) . . . . ?
F7 C29 C30 C31 179.71(15) . . . . ?
F8 C30 C31 F9 -0.7(2) . . . . ?
F8 C30 C31 C32 -179.57(15) . . . . ?
F9 C31 C32 F10 1.2(2) . . . . ?
F9 C31 C32 C27 -176.60(14) . . . . ?
O1 C7 C8 C9 168.87(14) . . . . ?
O1 C7 C8 C18 -10.2(2) . . . 2 ?
O1 C7 C16 C15 -170.78(15) . . . . ?
O2 C17 C18 C8 0.8(2) . . . 2 ?
O2 C17 C18 C19 179.34(14) . . . . ?
O2 C17 C26 C25 -178.45(14) . . . . ?
O3 C33 C34 C35 178.65(13) . . . . ?
O3 C33 C34 C44 -2.3(2) . . . 2_566 ?
O3 C33 C42 C41 -177.29(13) . . . . ?
O4 C43 C44 C34 -7.4(2) . . . 2_566 ?
O4 C43 C44 C45 172.38(13) . . . . ?
O4 C43 C52 C51 -176.39(14) . . . . ?
C1 C2 C3 F2 179.61(15) . . . . ?
C1 C2 C3 C4 0.6(3) . . . . ?
C2 C1 C6 F5 179.86(14) . . . . ?
C2 C1 C6 C5 -1.9(2) . . . . ?
C2 C1 B1 O1 47.0(2) . . . . ?
C2 C1 B1 O2 -131.02(17) . . . . ?
C2 C3 C4 F3 177.99(16) . . . . ?
C2 C3 C4 C5 -0.8(3) . . . . ?
C3 C4 C5 F4 178.87(16) . . . . ?
C3 C4 C5 C6 -0.4(3) . . . . ?
C4 C5 C6 F5 -179.93(15) . . . . ?
C4 C5 C6 C1 1.7(3) . . . . ?
C6 C1 C2 F1 -179.65(14) . . . . ?
C6 C1 C2 C3 0.7(2) . . . . ?
C6 C1 B1 O1 -134.46(18) . . . . ?
C6 C1 B1 O2 47.6(2) . . . . ?
C7 O1 B1 O2 -174.95(16) . . . . ?
C7 O1 B1 C1 7.1(3) . . . . ?
C7 C8 C9 C10 -176.04(15) . . . . ?
C7 C8 C9 C14 1.4(2) . . . . ?
C8 C7 C16 C15 1.9(3) . . . . ?
C8 C9 C10 C11 177.32(15) . . . . ?
C8 C9 C14 C13 -176.89(14) . . . . ?
C8 C9 C14 C15 1.7(2) . . . . ?
C8 C18 C19 C20 -5.0(2) 2 . . . ?
C8 C18 C19 C24 177.43(14) 2 . . . ?
C9 C10 C11 C12 -0.3(2) . . . . ?
C9 C14 C15 C16 -3.0(3) . . . . ?
C10 C9 C14 C13 0.6(2) . . . . ?
C10 C9 C14 C15 179.16(15) . . . . ?
C10 C11 C12 C13 0.3(2) . . . . ?
C11 C12 C13 C14 0.2(2) . . . . ?
C12 C13 C14 C9 -0.7(2) . . . . ?
C12 C13 C14 C15 -179.16(16) . . . . ?
C13 C14 C15 C16 175.47(16) . . . . ?
C14 C9 C10 C11 -0.1(2) . . . . ?
C14 C15 C16 C7 1.3(3) . . . . ?
C16 C7 C8 C9 -3.2(2) . . . . ?
C16 C7 C8 C18 177.71(15) . . . 2 ?
C17 O2 B1 O1 1.4(2) . . . . ?
C17 O2 B1 C1 179.56(14) . . . . ?
C17 C18 C19 C20 176.49(15) . . . . ?
C17 C18 C19 C24 -1.1(2) . . . . ?
C18 C8 C9 C10 3.1(2) 2 . . . ?
C18 C8 C9 C14 -179.50(14) 2 . . . ?
C18 C17 C26 C25 -1.6(2) . . . . ?
C18 C19 C20 C21 -176.71(16) . . . . ?
C18 C19 C24 C23 178.30(15) . . . . ?
C18 C19 C24 C25 -1.0(2) . . . . ?
C19 C20 C21 C22 -1.1(3) . . . . ?
C19 C24 C25 C26 1.9(2) . . . . ?
C20 C19 C24 C23 0.6(2) . . . . ?
C20 C19 C24 C25 -178.68(14) . . . . ?
C20 C21 C22 C23 -0.3(3) . . . . ?
C21 C22 C23 C24 1.9(3) . . . . ?
C22 C23 C24 C19 -2.0(2) . . . . ?
C22 C23 C24 C25 177.26(16) . . . . ?
C23 C24 C25 C26 -177.41(16) . . . . ?
C24 C19 C20 C21 0.9(2) . . . . ?
C24 C25 C26 C17 -0.6(2) . . . . ?
C26 C17 C18 C8 -176.06(14) . . . 2 ?
C26 C17 C18 C19 2.5(2) . . . . ?
C27 C28 C29 F7 -179.94(15) . . . . ?
C27 C28 C29 C30 1.5(3) . . . . ?
C28 C27 C32 F10 179.88(14) . . . . ?
C28 C27 C32 C31 -2.4(2) . . . . ?
C28 C27 B2 O3 -129.42(16) . . . . ?
C28 C27 B2 O4 50.2(2) . . . . ?
C28 C29 C30 F8 177.80(15) . . . . ?
C28 C29 C30 C31 -1.7(3) . . . . ?
C29 C30 C31 F9 178.76(15) . . . . ?
C29 C30 C31 C32 -0.1(3) . . . . ?
C30 C31 C32 F10 180.00(14) . . . . ?
C30 C31 C32 C27 2.2(3) . . . . ?
C32 C27 C28 F6 -179.40(13) . . . . ?
C32 C27 C28 C29 0.5(2) . . . . ?
C32 C27 B2 O3 53.9(2) . . . . ?
C32 C27 B2 O4 -126.51(18) . . . . ?
C33 O3 B2 O4 -3.4(2) . . . . ?
C33 O3 B2 C27 176.27(13) . . . . ?
C33 C34 C35 C36 176.29(14) . . . . ?
C33 C34 C35 C40 -2.5(2) . . . . ?
C34 C33 C42 C41 -1.3(2) . . . . ?
C34 C35 C36 C37 179.78(15) . . . . ?
C34 C35 C40 C39 -179.31(14) . . . . ?
C34 C35 C40 C41 1.2(2) . . . . ?
C34 C44 C45 C46 5.6(2) 2_566 . . . ?
C34 C44 C45 C50 -175.94(13) 2_566 . . . ?
C35 C36 C37 C38 0.0(2) . . . . ?
C35 C40 C41 C42 0.2(2) . . . . ?
C36 C35 C40 C39 1.8(2) . . . . ?
C36 C35 C40 C41 -177.72(14) . . . . ?
C36 C37 C38 C39 0.9(3) . . . . ?
C37 C38 C39 C40 -0.4(3) . . . . ?
C38 C39 C40 C35 -0.9(2) . . . . ?
C38 C39 C40 C41 178.58(16) . . . . ?
C39 C40 C41 C42 -179.32(15) . . . . ?
C40 C35 C36 C37 -1.4(2) . . . . ?
C40 C41 C42 C33 -0.2(2) . . . . ?
C42 C33 C34 C35 2.7(2) . . . . ?
C42 C33 C34 C44 -178.34(14) . . . 2_566 ?
C43 O4 B2 O3 176.07(15) . . . . ?
C43 O4 B2 C27 -3.5(3) . . . . ?
C43 C44 C45 C46 -174.13(14) . . . . ?
C43 C44 C45 C50 4.3(2) . . . . ?
C44 C34 C35 C36 -2.7(2) 2_566 . . . ?
C44 C34 C35 C40 178.44(14) 2_566 . . . ?
C44 C43 C52 C51 -1.0(2) . . . . ?
C44 C45 C46 C47 -179.55(14) . . . . ?
C44 C45 C50 C49 179.30(14) . . . . ?
C44 C45 C50 C51 -2.6(2) . . . . ?
C45 C46 C47 C48 -0.9(2) . . . . ?
C45 C50 C51 C52 -1.1(2) . . . . ?
C46 C45 C50 C49 -2.2(2) . . . . ?
C46 C45 C50 C51 175.93(14) . . . . ?
C46 C47 C48 C49 0.1(2) . . . . ?
C47 C48 C49 C50 -0.3(2) . . . . ?
C48 C49 C50 C45 1.4(2) . . . . ?
C48 C49 C50 C51 -176.68(15) . . . . ?
C49 C50 C51 C52 177.07(15) . . . . ?
C50 C45 C46 C47 2.0(2) . . . . ?
C50 C51 C52 C43 2.9(2) . . . . ?
C52 C43 C44 C34 177.68(14) . . . 2_566 ?
C52 C43 C44 C45 -2.5(2) . . . . ?
B1 O1 C7 C8 53.2(3) . . . . ?
B1 O1 C7 C16 -134.1(2) . . . . ?
B1 O2 C17 C18 127.77(16) . . . . ?
B1 O2 C17 C26 -55.3(2) . . . . ?
B1 C1 C2 F1 -1.0(2) . . . . ?
B1 C1 C2 C3 179.35(16) . . . . ?
B1 C1 C6 F5 1.2(2) . . . . ?
B1 C1 C6 C5 179.47(16) . . . . ?
B2 O3 C33 C34 129.28(16) . . . . ?
B2 O3 C33 C42 -54.6(2) . . . . ?
B2 O4 C43 C44 60.8(2) . . . . ?
B2 O4 C43 C52 -123.91(19) . . . . ?
B2 C27 C28 F6 3.7(2) . . . . ?
B2 C27 C28 C29 -176.39(15) . . . . ?
B2 C27 C32 F10 -3.2(2) . . . . ?
B2 C27 C32 C31 174.50(15) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.121 0.500 0.000 273.0 62.5 '2 C4H10O'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_exptl_crystal_mounting_method 'MiTeGen 50 micron MicroLoop'
_olex2_submission_original_sample_id kre19_42
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Diethyl ether'
