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

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

data_wa1940
_audit_block_doi                 10.5517/ccdc.csd.cc216r23
_database_code_depnum_ccdc_archive 'CCDC 1883314'
_audit_update_record             
;
2018-12-05 deposited with the CCDC.
2018-12-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
; 
 ; 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H26 Si2'
_chemical_formula_sum            'C20 H26 Si2'
_chemical_formula_weight         322.59

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   9.1691(3)
_cell_length_b                   12.4660(4)
_cell_length_c                   16.2294(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1855.05(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    41378
_cell_measurement_theta_min      2.1
_cell_measurement_theta_max      30.8

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_F_000             696
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    0.187
_shelx_estimated_absorpt_T_min   0.936
_shelx_estimated_absorpt_T_max   0.960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.915
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'

_exptl_special_details           
; 
 ; 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29132
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.060
_diffrn_reflns_theta_max         30.380
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             5529
_reflns_number_gt                5372
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.773
_reflns_Friedel_fraction_max     0.991
_reflns_Friedel_fraction_full    0.997

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  ?

_refine_special_details          
; 
 ; 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0578P)²+0.3532P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.041(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
; 
 Flack x determined using 2294 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.03(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5529
_refine_ls_number_parameters     200
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0353
_refine_ls_wR_factor_ref         0.0975
_refine_ls_wR_factor_gt          0.0965
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.13529(5) 0.51878(4) 0.66725(3) 0.02572(12) Uani 1 1 d . . . . .
Si2 Si 0.46052(6) 0.64374(4) 0.76023(3) 0.03017(13) Uani 1 1 d . . . . .
C1 C 0.33269(18) 0.51720(14) 0.62872(10) 0.0244(3) Uani 1 1 d . . . . .
C2 C 0.43448(19) 0.59447(14) 0.64959(11) 0.0266(3) Uani 1 1 d . . . . .
C3 C 0.5479(2) 0.62216(15) 0.58992(11) 0.0289(3) Uani 1 1 d . . . . .
C4 C 0.6327(2) 0.71653(17) 0.60002(15) 0.0388(4) Uani 1 1 d . . . . .
H4 H 0.6205 0.7584 0.6484 0.047 Uiso 1 1 calc R U . . .
C5 C 0.7323(3) 0.7491(2) 0.54165(17) 0.0452(5) Uani 1 1 d . . . . .
H5 H 0.7883 0.8123 0.5502 0.054 Uiso 1 1 calc R U . . .
C6 C 0.7505(2) 0.6889(2) 0.46966(15) 0.0444(5) Uani 1 1 d . . . . .
H6 H 0.8193 0.7109 0.4293 0.053 Uiso 1 1 calc R U . . .
C7 C 0.6688(2) 0.5977(2) 0.45737(13) 0.0386(4) Uani 1 1 d . . . . .
H7 H 0.6814 0.5576 0.4081 0.046 Uiso 1 1 calc R U . . .
C8 C 0.56683(19) 0.56250(15) 0.51638(11) 0.0294(3) Uani 1 1 d . . . . .
C9 C 0.48134(19) 0.46558(15) 0.50514(10) 0.0276(3) Uani 1 1 d . . . . .
C10 C 0.5111(2) 0.39034(17) 0.44254(12) 0.0338(4) Uani 1 1 d . . . . .
H10 H 0.5871 0.4048 0.4043 0.041 Uiso 1 1 calc R U . . .
C11 C 0.4335(2) 0.29686(17) 0.43533(12) 0.0353(4) Uani 1 1 d . . . . .
H11 H 0.4559 0.2475 0.3925 0.042 Uiso 1 1 calc R U . . .
C12 C 0.3211(2) 0.27406(16) 0.49109(12) 0.0339(4) Uani 1 1 d . . . . .
H12 H 0.2687 0.2085 0.4873 0.041 Uiso 1 1 calc R U . . .
C13 C 0.2871(2) 0.34765(15) 0.55135(11) 0.0297(3) Uani 1 1 d . . . . .
H13 H 0.2094 0.3324 0.5883 0.036 Uiso 1 1 calc R U . . .
C14 C 0.3643(2) 0.44509(13) 0.55999(10) 0.0250(3) Uani 1 1 d . . . . .
C15 C 0.0150(2) 0.50885(18) 0.57389(13) 0.0369(4) Uani 1 1 d . . . . .
H15A H 0.0322 0.4402 0.5461 0.055 Uiso 1 1 calc R U . . .
H15B H 0.0374 0.5678 0.5360 0.055 Uiso 1 1 calc R U . . .
H15C H -0.0875 0.5134 0.5908 0.055 Uiso 1 1 calc R U . . .
C16 C 0.0867(2) 0.65319(16) 0.71047(13) 0.0345(4) Uani 1 1 d . . . . .
H16A H 0.1143 0.7093 0.6711 0.052 Uiso 1 1 calc R U . . .
H16B H 0.1390 0.6643 0.7624 0.052 Uiso 1 1 calc R U . . .
H16C H -0.0186 0.6564 0.7205 0.052 Uiso 1 1 calc R U . . .
C17 C 0.0832(3) 0.41000(17) 0.74201(13) 0.0389(4) Uani 1 1 d . . . . .
H17A H 0.1094 0.3400 0.7189 0.058 Uiso 1 1 calc R U . . .
H17B H -0.0222 0.4125 0.7519 0.058 Uiso 1 1 calc R U . . .
H17C H 0.1352 0.4209 0.7941 0.058 Uiso 1 1 calc R U . . .
C18 C 0.3670(3) 0.55448(18) 0.83644(12) 0.0382(4) Uani 1 1 d . . . . .
H18A H 0.3932 0.4796 0.8255 0.057 Uiso 1 1 calc R U . . .
H18B H 0.2611 0.5632 0.8314 0.057 Uiso 1 1 calc R U . . .
H18C H 0.3976 0.5739 0.8923 0.057 Uiso 1 1 calc R U . . .
C19 C 0.6590(3) 0.6212(2) 0.78471(16) 0.0473(5) Uani 1 1 d . . . . .
H19A H 0.6842 0.5460 0.7741 0.071 Uiso 1 1 calc R U . . .
H19B H 0.6770 0.6380 0.8428 0.071 Uiso 1 1 calc R U . . .
H19C H 0.7191 0.6678 0.7499 0.071 Uiso 1 1 calc R U . . .
C20 C 0.4130(3) 0.78831(17) 0.77995(16) 0.0448(5) Uani 1 1 d . . . . .
H20A H 0.4626 0.8338 0.7394 0.067 Uiso 1 1 calc R U . . .
H20B H 0.4445 0.8084 0.8356 0.067 Uiso 1 1 calc R U . . .
H20C H 0.3073 0.7980 0.7751 0.067 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 C16 1.870(2) . ?
Si1 C15 1.878(2) . ?
Si1 C17 1.881(2) . ?
Si1 C1 1.9150(17) . ?
Si2 C18 1.872(2) . ?
Si2 C20 1.881(2) . ?
Si2 C19 1.884(2) . ?
Si2 C2 1.9129(18) . ?
C1 C2 1.383(2) . ?
C1 C14 1.462(2) . ?
C2 C3 1.462(2) . ?
C3 C8 1.417(3) . ?
C3 C4 1.420(3) . ?
C4 C5 1.377(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.399(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.376(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.408(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.452(3) . ?
C9 C10 1.409(3) . ?
C9 C14 1.417(2) . ?
C10 C11 1.371(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.401(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.376(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.413(2) . ?
C13 H13 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 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
C16 Si1 C15 102.81(10) . . ?
C16 Si1 C17 110.09(10) . . ?
C15 Si1 C17 108.88(10) . . ?
C16 Si1 C1 110.89(9) . . ?
C15 Si1 C1 106.92(8) . . ?
C17 Si1 C1 116.31(9) . . ?
C18 Si2 C20 110.55(11) . . ?
C18 Si2 C19 102.40(11) . . ?
C20 Si2 C19 109.31(12) . . ?
C18 Si2 C2 111.85(9) . . ?
C20 Si2 C2 116.00(10) . . ?
C19 Si2 C2 105.70(10) . . ?
C2 C1 C14 118.76(15) . . ?
C2 C1 Si1 123.41(13) . . ?
C14 C1 Si1 116.30(12) . . ?
C1 C2 C3 118.82(16) . . ?
C1 C2 Si2 122.52(13) . . ?
C3 C2 Si2 117.20(13) . . ?
C8 C3 C4 117.71(17) . . ?
C8 C3 C2 121.41(16) . . ?
C4 C3 C2 120.58(18) . . ?
C5 C4 C3 121.9(2) . . ?
C5 C4 H4 119.1 . . ?
C3 C4 H4 119.1 . . ?
C4 C5 C6 119.7(2) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C7 C6 C5 120.0(2) . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C8 121.3(2) . . ?
C6 C7 H7 119.3 . . ?
C8 C7 H7 119.3 . . ?
C7 C8 C3 119.39(18) . . ?
C7 C8 C9 122.15(18) . . ?
C3 C8 C9 118.46(15) . . ?
C10 C9 C14 118.66(17) . . ?
C10 C9 C8 122.66(16) . . ?
C14 C9 C8 118.68(16) . . ?
C11 C10 C9 121.77(18) . . ?
C11 C10 H10 119.1 . . ?
C9 C10 H10 119.1 . . ?
C10 C11 C12 119.98(17) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C13 C12 C11 119.34(19) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C12 C13 C14 122.03(18) . . ?
C12 C13 H13 119.0 . . ?
C14 C13 H13 119.0 . . ?
C13 C14 C9 118.15(16) . . ?
C13 C14 C1 120.34(15) . . ?
C9 C14 C1 121.24(16) . . ?
Si1 C15 H15A 109.5 . . ?
Si1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si1 C16 H16A 109.5 . . ?
Si1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Si1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si1 C17 H17A 109.5 . . ?
Si1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si2 C18 H18A 109.5 . . ?
Si2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Si2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si2 C19 H19A 109.5 . . ?
Si2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Si2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si2 C20 H20A 109.5 . . ?
Si2 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
Si2 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C14 C1 C2 C3 17.3(2) . . . . ?
Si1 C1 C2 C3 -148.04(14) . . . . ?
C14 C1 C2 Si2 -148.54(13) . . . . ?
Si1 C1 C2 Si2 46.1(2) . . . . ?
C1 C2 C3 C8 -8.2(3) . . . . ?
Si2 C2 C3 C8 158.39(14) . . . . ?
C1 C2 C3 C4 165.31(18) . . . . ?
Si2 C2 C3 C4 -28.1(2) . . . . ?
C8 C3 C4 C5 -1.1(3) . . . . ?
C2 C3 C4 C5 -174.8(2) . . . . ?
C3 C4 C5 C6 0.6(4) . . . . ?
C4 C5 C6 C7 0.2(4) . . . . ?
C5 C6 C7 C8 -0.5(3) . . . . ?
C6 C7 C8 C3 0.0(3) . . . . ?
C6 C7 C8 C9 -178.97(19) . . . . ?
C4 C3 C8 C7 0.8(3) . . . . ?
C2 C3 C8 C7 174.44(17) . . . . ?
C4 C3 C8 C9 179.79(17) . . . . ?
C2 C3 C8 C9 -6.5(2) . . . . ?
C7 C8 C9 C10 11.3(3) . . . . ?
C3 C8 C9 C10 -167.66(17) . . . . ?
C7 C8 C9 C14 -169.48(17) . . . . ?
C3 C8 C9 C14 11.5(2) . . . . ?
C14 C9 C10 C11 -2.3(3) . . . . ?
C8 C9 C10 C11 176.87(17) . . . . ?
C9 C10 C11 C12 0.0(3) . . . . ?
C10 C11 C12 C13 1.8(3) . . . . ?
C11 C12 C13 C14 -1.3(3) . . . . ?
C12 C13 C14 C9 -1.0(3) . . . . ?
C12 C13 C14 C1 -175.11(18) . . . . ?
C10 C9 C14 C13 2.7(2) . . . . ?
C8 C9 C14 C13 -176.49(16) . . . . ?
C10 C9 C14 C1 176.81(16) . . . . ?
C8 C9 C14 C1 -2.4(2) . . . . ?
C2 C1 C14 C13 161.60(17) . . . . ?
Si1 C1 C14 C13 -32.0(2) . . . . ?
C2 C1 C14 C9 -12.4(2) . . . . ?
Si1 C1 C14 C9 154.01(13) . . . . ?

_refine_diff_density_max         0.280
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.043

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_wa1856
_database_code_depnum_ccdc_archive 'CCDC 1883327'
_audit_update_record             
;
2018-12-18 deposited with the CCDC.
2018-12-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H26'
_chemical_formula_weight         290.43

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.4961(18)
_cell_length_b                   9.9907(14)
_cell_length_c                   15.608(3)
_cell_angle_alpha                90
_cell_angle_beta                 96.664(13)
_cell_angle_gamma                90
_cell_volume                     1780.5(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    10318
_cell_measurement_theta_min      3.4
_cell_measurement_theta_max      25.8

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.083
_exptl_crystal_F_000             632
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.060
_shelx_estimated_absorpt_T_min   0.976
_shelx_estimated_absorpt_T_max   0.997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  .486
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13210
_diffrn_reflns_av_unetI/netI     0.0680
_diffrn_reflns_av_R_equivalents  0.1093
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.327
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             3126
_reflns_number_gt                1686
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  ?
_refine_special_details          ;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0944P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3126
_refine_ls_number_parameters     212
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1256
_refine_ls_R_factor_gt           0.0651
_refine_ls_wR_factor_ref         0.1925
_refine_ls_wR_factor_gt          0.1598
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_restrained_S_all      0.966
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4767(3) 0.6281(3) 0.70017(16) 0.0552(8) Uani 1 1 d . . . . .
C2 C 0.4178(3) 0.6251(3) 0.63186(15) 0.0542(8) Uani 1 1 d . . . . .
C11 C 0.5487(3) 0.6281(3) 0.78199(14) 0.0516(7) Uani 1 1 d . . . . .
C12 C 0.5593(3) 0.5142(3) 0.83333(17) 0.0777(11) Uani 1 1 d . . . . .
H12 H 0.517771 0.435402 0.814272 0.093 Uiso 1 1 calc R U . . .
C13 C 0.6289(3) 0.5133(3) 0.91149(16) 0.0716(10) Uani 1 1 d . . . . .
H13 H 0.633533 0.433923 0.945182 0.086 Uiso 1 1 calc R U . . .
C14 C 0.6918(3) 0.6236(3) 0.94214(14) 0.0479(7) Uani 1 1 d . . . . .
C15 C 0.6815(3) 0.7361(3) 0.89044(15) 0.0541(7) Uani 1 1 d . . . . .
H15 H 0.723700 0.814400 0.909533 0.065 Uiso 1 1 calc R U . . .
C16 C 0.6124(3) 0.7390(3) 0.81222(15) 0.0562(8) Uani 1 1 d . . . . .
H16 H 0.608576 0.818509 0.778582 0.067 Uiso 1 1 calc R U . . .
C17 C 0.7686(3) 0.6231(3) 1.02853(14) 0.0541(8) Uani 1 1 d . . . . .
C18 C 0.8860(4) 0.6865(6) 1.0207(3) 0.0813(16) Uani 0.798(6) 1 d . . P A 1
H18A H 0.874293 0.775319 0.994367 0.122 Uiso 0.798(6) 1 calc R U P A 1
H18B H 0.929880 0.695300 1.078085 0.122 Uiso 0.798(6) 1 calc R U P A 1
H18C H 0.930105 0.630195 0.984422 0.122 Uiso 0.798(6) 1 calc R U P A 1
C19 C 0.7087(4) 0.7159(5) 1.0907(2) 0.0822(16) Uani 0.798(6) 1 d . . P A 1
H19A H 0.699308 0.805771 1.065707 0.123 Uiso 0.798(6) 1 calc R U P A 1
H19B H 0.631688 0.679484 1.099057 0.123 Uiso 0.798(6) 1 calc R U P A 1
H19C H 0.757521 0.720752 1.146430 0.123 Uiso 0.798(6) 1 calc R U P A 1
C20 C 0.7817(6) 0.4867(5) 1.0685(3) 0.113(3) Uani 0.798(6) 1 d . . P A 1
H20A H 0.704066 0.448478 1.072664 0.170 Uiso 0.798(6) 1 calc R U P A 1
H20B H 0.824947 0.428682 1.032678 0.170 Uiso 0.798(6) 1 calc R U P A 1
H20C H 0.824722 0.493786 1.126341 0.170 Uiso 0.798(6) 1 calc R U P A 1
C18' C 0.8569(16) 0.5005(18) 1.0213(11) 0.068(5) Uiso 0.202(6) 1 d . . P A 2
H18D H 0.811952 0.418567 1.006910 0.082 Uiso 0.202(6) 1 calc R U P A 2
H18E H 0.906992 0.519360 0.976095 0.082 Uiso 0.202(6) 1 calc R U P A 2
H18F H 0.905661 0.488587 1.076599 0.082 Uiso 0.202(6) 1 calc R U P A 2
C19' C 0.828(2) 0.745(2) 1.0493(14) 0.092(7) Uiso 0.202(6) 1 d . . P A 2
H19D H 0.875940 0.767896 1.003502 0.110 Uiso 0.202(6) 1 calc R U P A 2
H19E H 0.770559 0.816039 1.054660 0.110 Uiso 0.202(6) 1 calc R U P A 2
H19F H 0.878225 0.734915 1.104019 0.110 Uiso 0.202(6) 1 calc R U P A 2
C20' C 0.6935(14) 0.5866(16) 1.0996(8) 0.057(4) Uiso 0.202(6) 1 d . . P A 2
H20D H 0.652537 0.502115 1.084986 0.068 Uiso 0.202(6) 1 calc R U P A 2
H20E H 0.743686 0.576472 1.154430 0.068 Uiso 0.202(6) 1 calc R U P A 2
H20F H 0.636020 0.657596 1.105071 0.068 Uiso 0.202(6) 1 calc R U P A 2
C21 C 0.3442(3) 0.6217(3) 0.55087(14) 0.0489(7) Uani 1 1 d . . . . .
C22 C 0.3916(3) 0.6347(3) 0.47247(15) 0.0574(8) Uani 1 1 d . . . . .
H22 H 0.473682 0.645762 0.472382 0.069 Uiso 1 1 calc R U . . .
C23 C 0.3192(3) 0.6315(3) 0.39527(15) 0.0553(8) Uani 1 1 d . . . . .
H23 H 0.353306 0.639431 0.342883 0.066 Uiso 1 1 calc R U . . .
C24 C 0.1999(3) 0.6173(2) 0.39157(14) 0.0452(7) Uani 1 1 d . . . . .
C25 C 0.1541(3) 0.6040(3) 0.47002(14) 0.0508(7) Uani 1 1 d . . . . .
H25 H 0.072025 0.593699 0.470220 0.061 Uiso 1 1 calc R U . . .
C26 C 0.2258(3) 0.6057(3) 0.54748(15) 0.0516(7) Uani 1 1 d . . . . .
H26 H 0.191796 0.595354 0.599731 0.062 Uiso 1 1 calc R U . . .
C27 C 0.1218(3) 0.6141(3) 0.30466(14) 0.0497(7) Uani 1 1 d . . . . .
C28 C 0.1562(3) 0.7264(4) 0.24642(19) 0.0891(13) Uani 1 1 d . . . . .
H28A H 0.239414 0.718414 0.239095 0.134 Uiso 1 1 calc R U . . .
H28B H 0.109222 0.720021 0.190014 0.134 Uiso 1 1 calc R U . . .
H28C H 0.142011 0.813110 0.272736 0.134 Uiso 1 1 calc R U . . .
C29 C -0.0059(3) 0.6279(4) 0.31519(19) 0.0902(12) Uani 1 1 d . . . . .
H29A H -0.029011 0.556130 0.352541 0.135 Uiso 1 1 calc R U . . .
H29B H -0.019637 0.714845 0.341311 0.135 Uiso 1 1 calc R U . . .
H29C H -0.052426 0.621756 0.258589 0.135 Uiso 1 1 calc R U . . .
C30 C 0.1389(4) 0.4802(4) 0.26009(19) 0.0930(13) Uani 1 1 d . . . . .
H30A H 0.221721 0.468843 0.252491 0.139 Uiso 1 1 calc R U . . .
H30B H 0.114059 0.407001 0.295658 0.139 Uiso 1 1 calc R U . . .
H30C H 0.091728 0.478905 0.203595 0.139 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.196(3) . ?
C1 C11 1.439(3) . ?
C2 C21 1.437(3) . ?
C11 C16 1.382(4) . ?
C11 C12 1.389(4) . ?
C12 C13 1.379(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.372(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.381(4) . ?
C14 C17 1.524(3) . ?
C15 C16 1.377(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C19' 1.41(2) . ?
C17 C20 1.499(5) . ?
C17 C18 1.509(5) . ?
C17 C20' 1.527(14) . ?
C17 C19 1.559(5) . ?
C17 C18' 1.603(17) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C18' H18D 0.9800 . ?
C18' H18E 0.9800 . ?
C18' H18F 0.9800 . ?
C19' H19D 0.9800 . ?
C19' H19E 0.9800 . ?
C19' H19F 0.9800 . ?
C20' H20D 0.9800 . ?
C20' H20E 0.9800 . ?
C20' H20F 0.9800 . ?
C21 C26 1.366(4) . ?
C21 C22 1.402(4) . ?
C22 C23 1.383(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.373(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.394(3) . ?
C24 C27 1.538(3) . ?
C25 C26 1.382(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C29 1.503(5) . ?
C27 C28 1.525(4) . ?
C27 C30 1.531(4) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C11 178.4(3) . . ?
C1 C2 C21 178.5(3) . . ?
C16 C11 C12 116.9(2) . . ?
C16 C11 C1 122.0(2) . . ?
C12 C11 C1 121.0(3) . . ?
C13 C12 C11 121.2(3) . . ?
C13 C12 H12 119.4 . . ?
C11 C12 H12 119.4 . . ?
C14 C13 C12 122.1(3) . . ?
C14 C13 H13 118.9 . . ?
C12 C13 H13 118.9 . . ?
C13 C14 C15 116.3(2) . . ?
C13 C14 C17 122.3(2) . . ?
C15 C14 C17 121.4(3) . . ?
C16 C15 C14 122.5(3) . . ?
C16 C15 H15 118.8 . . ?
C14 C15 H15 118.8 . . ?
C15 C16 C11 120.9(2) . . ?
C15 C16 H16 119.5 . . ?
C11 C16 H16 119.5 . . ?
C20 C17 C18 111.6(4) . . ?
C19' C17 C20' 109.7(11) . . ?
C19' C17 C14 114.5(9) . . ?
C20 C17 C14 113.0(3) . . ?
C18 C17 C14 111.0(2) . . ?
C20' C17 C14 109.0(6) . . ?
C20 C17 C19 108.2(4) . . ?
C18 C17 C19 105.4(3) . . ?
C14 C17 C19 107.3(3) . . ?
C19' C17 C18' 112.4(12) . . ?
C20' C17 C18' 106.5(9) . . ?
C14 C17 C18' 104.3(6) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C17 C18' H18D 109.5 . . ?
C17 C18' H18E 109.5 . . ?
H18D C18' H18E 109.5 . . ?
C17 C18' H18F 109.5 . . ?
H18D C18' H18F 109.5 . . ?
H18E C18' H18F 109.5 . . ?
C17 C19' H19D 109.5 . . ?
C17 C19' H19E 109.5 . . ?
H19D C19' H19E 109.5 . . ?
C17 C19' H19F 109.5 . . ?
H19D C19' H19F 109.5 . . ?
H19E C19' H19F 109.5 . . ?
C17 C20' H20D 109.5 . . ?
C17 C20' H20E 109.5 . . ?
H20D C20' H20E 109.5 . . ?
C17 C20' H20F 109.5 . . ?
H20D C20' H20F 109.5 . . ?
H20E C20' H20F 109.5 . . ?
C26 C21 C22 117.6(2) . . ?
C26 C21 C2 121.3(2) . . ?
C22 C21 C2 121.1(3) . . ?
C23 C22 C21 120.2(3) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C24 C23 C22 122.4(2) . . ?
C24 C23 H23 118.8 . . ?
C22 C23 H23 118.8 . . ?
C23 C24 C25 116.7(2) . . ?
C23 C24 C27 121.2(2) . . ?
C25 C24 C27 122.1(3) . . ?
C26 C25 C24 121.3(3) . . ?
C26 C25 H25 119.3 . . ?
C24 C25 H25 119.3 . . ?
C21 C26 C25 121.7(2) . . ?
C21 C26 H26 119.1 . . ?
C25 C26 H26 119.1 . . ?
C29 C27 C28 108.8(3) . . ?
C29 C27 C30 108.0(3) . . ?
C28 C27 C30 108.5(3) . . ?
C29 C27 C24 112.3(2) . . ?
C28 C27 C24 110.2(2) . . ?
C30 C27 C24 109.1(2) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C16 C11 C12 C13 1.0(5) . . . . ?
C1 C11 C12 C13 179.5(3) . . . . ?
C11 C12 C13 C14 -0.6(6) . . . . ?
C12 C13 C14 C15 0.1(5) . . . . ?
C12 C13 C14 C17 179.9(3) . . . . ?
C13 C14 C15 C16 -0.1(4) . . . . ?
C17 C14 C15 C16 -179.8(3) . . . . ?
C14 C15 C16 C11 0.5(4) . . . . ?
C12 C11 C16 C15 -1.0(4) . . . . ?
C1 C11 C16 C15 -179.4(3) . . . . ?
C13 C14 C17 C19' 179.3(12) . . . . ?
C15 C14 C17 C19' -0.9(12) . . . . ?
C13 C14 C17 C20 8.6(5) . . . . ?
C15 C14 C17 C20 -171.6(4) . . . . ?
C13 C14 C17 C18 134.9(4) . . . . ?
C15 C14 C17 C18 -45.4(4) . . . . ?
C13 C14 C17 C20' -57.3(7) . . . . ?
C15 C14 C17 C20' 122.4(7) . . . . ?
C13 C14 C17 C19 -110.5(4) . . . . ?
C15 C14 C17 C19 69.3(4) . . . . ?
C13 C14 C17 C18' 56.1(8) . . . . ?
C15 C14 C17 C18' -124.2(8) . . . . ?
C26 C21 C22 C23 0.2(4) . . . . ?
C2 C21 C22 C23 -179.9(3) . . . . ?
C21 C22 C23 C24 0.7(4) . . . . ?
C22 C23 C24 C25 -0.9(4) . . . . ?
C22 C23 C24 C27 180.0(3) . . . . ?
C23 C24 C25 C26 0.2(4) . . . . ?
C27 C24 C25 C26 179.3(3) . . . . ?
C22 C21 C26 C25 -0.9(4) . . . . ?
C2 C21 C26 C25 179.2(3) . . . . ?
C24 C25 C26 C21 0.7(4) . . . . ?
C23 C24 C27 C29 -167.6(3) . . . . ?
C25 C24 C27 C29 13.4(4) . . . . ?
C23 C24 C27 C28 -46.2(4) . . . . ?
C25 C24 C27 C28 134.8(3) . . . . ?
C23 C24 C27 C30 72.8(4) . . . . ?
C25 C24 C27 C30 -106.2(3) . . . . ?

_refine_diff_density_max         0.165
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.043

####################################################################### 
# 
# 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_wa1973
_audit_block_doi                 10.5517/ccdc.csd.cc216r45
_database_code_depnum_ccdc_archive 'CCDC 1883316'
_audit_update_record             
;
2018-12-05 deposited with the CCDC.
2018-12-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
; 
 ; 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H8 Br2'
_chemical_formula_sum            'C14 H8 Br2'
_chemical_formula_weight         336.02

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   18.001(2)
_cell_length_b                   9.0764(6)
_cell_length_c                   7.2612(9)
_cell_angle_alpha                90
_cell_angle_beta                 112.754(9)
_cell_angle_gamma                90
_cell_volume                     1094.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8701
_cell_measurement_theta_min      3.6
_cell_measurement_theta_max      27.4

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.040
_exptl_crystal_F_000             648
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    7.373
_shelx_estimated_absorpt_T_min   0.208
_shelx_estimated_absorpt_T_max   0.557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.179
_exptl_absorpt_correction_T_max  0.761
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'

_exptl_special_details           
; 
 ; 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7041
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_av_R_equivalents  0.1127
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.594
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             1198
_reflns_number_gt                1076
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  SHELXL97

_refine_special_details          
; 
 ; 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0360P)²+0.8623P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1198
_refine_ls_number_parameters     73
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_ref         0.0827
_refine_ls_wR_factor_gt          0.0800
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.09367(2) 0.11024(3) 0.40995(5) 0.03540(15) Uani 1 1 d . . . . .
C1 C 0.08254(15) 0.4250(3) 0.3898(4) 0.0172(5) Uani 1 1 d . . . . .
C2 C 0.04155(14) 0.5599(3) 0.3208(3) 0.0175(5) Uani 1 1 d . . . . .
C3 C 0.08351(17) 0.6928(3) 0.3953(4) 0.0257(6) Uani 1 1 d . . . . .
H3 H 0.0569 0.7844 0.3527 0.031 Uiso 1 1 calc R U . . .
C4 C 0.16255(17) 0.6907(4) 0.5289(4) 0.0284(6) Uani 1 1 d . . . . .
H4 H 0.1900 0.7810 0.5766 0.034 Uiso 1 1 calc R U . . .
C5 C 0.20283(17) 0.5574(4) 0.5950(4) 0.0285(6) Uani 1 1 d . . . . .
H5 H 0.2572 0.5572 0.6878 0.034 Uiso 1 1 calc R U . . .
C6 C 0.16372(16) 0.4268(3) 0.5259(4) 0.0232(5) Uani 1 1 d . . . . .
H6 H 0.1915 0.3365 0.5701 0.028 Uiso 1 1 calc R U . . .
C7 C 0.03900(15) 0.2900(3) 0.3160(3) 0.0183(5) 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
Br1 C7 1.892(2) . ?
C1 C6 1.413(3) . ?
C1 C2 1.417(4) . ?
C1 C7 1.441(4) . ?
C2 C3 1.415(4) . ?
C2 C2 1.451(5) 2 ?
C3 C4 1.378(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.397(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.370(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C7 1.360(5) 2 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 C1 C2 119.5(2) . . ?
C6 C1 C7 122.5(3) . . ?
C2 C1 C7 118.0(2) . . ?
C3 C2 C1 118.3(2) . . ?
C3 C2 C2 121.50(16) . 2 ?
C1 C2 C2 120.24(15) . 2 ?
C4 C3 C2 120.7(3) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C3 C4 C5 120.7(3) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C6 C5 C4 119.9(3) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C1 120.8(3) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 119.6 . . ?
C7 C7 C1 121.80(15) 2 . ?
C7 C7 Br1 120.37(8) 2 . ?
C1 C7 Br1 117.83(19) . . ?

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
C6 C1 C2 C3 -1.4(3) . . . . ?
C7 C1 C2 C3 178.9(2) . . . . ?
C6 C1 C2 C2 179.3(3) . . . 2 ?
C7 C1 C2 C2 -0.4(4) . . . 2 ?
C1 C2 C3 C4 1.0(4) . . . . ?
C2 C2 C3 C4 -179.6(3) 2 . . . ?
C2 C3 C4 C5 -0.5(4) . . . . ?
C3 C4 C5 C6 0.4(4) . . . . ?
C4 C5 C6 C1 -0.7(4) . . . . ?
C2 C1 C6 C5 1.2(4) . . . . ?
C7 C1 C6 C5 -179.1(2) . . . . ?
C6 C1 C7 C7 -179.6(3) . . . 2 ?
C2 C1 C7 C7 0.1(4) . . . 2 ?
C6 C1 C7 Br1 0.8(3) . . . . ?
C2 C1 C7 Br1 -179.52(17) . . . . ?

_refine_diff_density_max         0.588
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.112

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_wa2050
_audit_block_doi                 10.5517/ccdc.csd.cc216r56
_database_code_depnum_ccdc_archive 'CCDC 1883317'
_audit_update_record             
;
2018-12-05 deposited with the CCDC.
2018-12-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H39 B O2'
_chemical_formula_sum            'C28 H39 B O2'
_chemical_formula_weight         418.40

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   6.1626(5)
_cell_length_b                   12.0463(10)
_cell_length_c                   18.6987(15)
_cell_angle_alpha                107.075(6)
_cell_angle_beta                 94.331(6)
_cell_angle_gamma                101.872(6)
_cell_volume                     1284.77(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    16019
_cell_measurement_theta_min      3.4
_cell_measurement_theta_max      26.8

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.082
_exptl_crystal_F_000             456
_exptl_transmission_factor_min   0.327
_exptl_transmission_factor_max   1.000
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    0.065
_shelx_estimated_absorpt_T_min   0.973
_shelx_estimated_absorpt_T_max   0.994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17245
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.358
_diffrn_reflns_theta_max         26.418
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             5224
_reflns_number_gt                4066
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  SHELXL97
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0629P)²+0.1884P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5224
_refine_ls_number_parameters     280
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0485
_refine_ls_wR_factor_ref         0.1328
_refine_ls_wR_factor_gt          0.1264
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6859(2) 0.66699(13) 0.36484(8) 0.0275(3) Uani 1 1 d . . . . .
C2 C 0.5708(3) 0.74328(13) 0.35039(8) 0.0285(3) Uani 1 1 d . . . . .
H2 H 0.6002 0.8184 0.3890 0.034 Uiso 1 1 calc R U . . .
C11 C 0.6574(2) 0.54168(13) 0.31477(8) 0.0266(3) Uani 1 1 d . . . . .
C12 C 0.8287(3) 0.50550(14) 0.27715(9) 0.0334(3) Uani 1 1 d . . . . .
H12 H 0.9683 0.5612 0.2841 0.040 Uiso 1 1 calc R U . . .
C13 C 0.7997(3) 0.38923(14) 0.22951(9) 0.0349(4) Uani 1 1 d . . . . .
H13 H 0.9194 0.3675 0.2038 0.042 Uiso 1 1 calc R U . . .
C14 C 0.5999(3) 0.30383(13) 0.21843(8) 0.0289(3) Uani 1 1 d . . . . .
C15 C 0.4307(3) 0.34074(14) 0.25721(9) 0.0336(3) Uani 1 1 d . . . . .
H15 H 0.2922 0.2846 0.2512 0.040 Uiso 1 1 calc R U . . .
C16 C 0.4573(3) 0.45667(14) 0.30432(9) 0.0329(3) Uani 1 1 d . . . . .
H16 H 0.3373 0.4785 0.3298 0.039 Uiso 1 1 calc R U . . .
C17 C 0.5606(3) 0.17560(14) 0.16446(9) 0.0355(4) Uani 1 1 d . . . . .
C18 C 0.4108(4) 0.16473(19) 0.09232(11) 0.0584(6) Uani 1 1 d . . . . .
H18A H 0.2691 0.1843 0.1053 0.088 Uiso 1 1 calc R U . . .
H18B H 0.4869 0.2202 0.0678 0.088 Uiso 1 1 calc R U . . .
H18C H 0.3807 0.0827 0.0577 0.088 Uiso 1 1 calc R U . . .
C19 C 0.4452(4) 0.08529(16) 0.20072(12) 0.0535(5) Uani 1 1 d . . . . .
H19A H 0.3038 0.1037 0.2151 0.080 Uiso 1 1 calc R U . . .
H19B H 0.4148 0.0045 0.1645 0.080 Uiso 1 1 calc R U . . .
H19C H 0.5430 0.0899 0.2458 0.080 Uiso 1 1 calc R U . . .
C20 C 0.7800(3) 0.14466(17) 0.14274(12) 0.0525(5) Uani 1 1 d . . . . .
H20A H 0.8567 0.2017 0.1193 0.079 Uiso 1 1 calc R U . . .
H20B H 0.8761 0.1489 0.1881 0.079 Uiso 1 1 calc R U . . .
H20C H 0.7479 0.0635 0.1068 0.079 Uiso 1 1 calc R U . . .
C21 C 0.4069(3) 0.73130(13) 0.28527(8) 0.0280(3) Uani 1 1 d . . . . .
C22 C 0.2756(3) 0.81385(14) 0.29320(9) 0.0356(4) Uani 1 1 d . . . . .
H22 H 0.2919 0.8743 0.3406 0.043 Uiso 1 1 calc R U . . .
C23 C 0.1209(3) 0.81089(14) 0.23409(9) 0.0360(4) Uani 1 1 d . . . . .
H23 H 0.0325 0.8682 0.2422 0.043 Uiso 1 1 calc R U . . .
C24 C 0.0939(3) 0.72550(13) 0.16348(8) 0.0286(3) Uani 1 1 d . . . . .
C25 C 0.2258(3) 0.64261(14) 0.15561(8) 0.0340(4) Uani 1 1 d . . . . .
H25 H 0.2109 0.5829 0.1080 0.041 Uiso 1 1 calc R U . . .
C26 C 0.3773(3) 0.64427(14) 0.21454(8) 0.0325(3) Uani 1 1 d . . . . .
H26 H 0.4624 0.5854 0.2068 0.039 Uiso 1 1 calc R U . . .
C27 C -0.0666(3) 0.72227(14) 0.09566(9) 0.0347(4) Uani 1 1 d . . . . .
C28 C -0.2276(3) 0.59823(16) 0.06329(10) 0.0435(4) Uani 1 1 d . . . . .
H28A H -0.1412 0.5373 0.0492 0.065 Uiso 1 1 calc R U . . .
H28B H -0.3194 0.5830 0.1015 0.065 Uiso 1 1 calc R U . . .
H28C H -0.3250 0.5952 0.0185 0.065 Uiso 1 1 calc R U . . .
C29 C 0.0712(3) 0.74639(19) 0.03448(10) 0.0504(5) Uani 1 1 d . . . . .
H29A H 0.1605 0.6868 0.0203 0.076 Uiso 1 1 calc R U . . .
H29B H -0.0300 0.7411 -0.0100 0.076 Uiso 1 1 calc R U . . .
H29C H 0.1712 0.8266 0.0541 0.076 Uiso 1 1 calc R U . . .
C30 C -0.2047(3) 0.81565(17) 0.11721(11) 0.0491(5) Uani 1 1 d . . . . .
H30A H -0.1039 0.8955 0.1380 0.074 Uiso 1 1 calc R U . . .
H30B H -0.3022 0.8118 0.0722 0.074 Uiso 1 1 calc R U . . .
H30C H -0.2966 0.7996 0.1552 0.074 Uiso 1 1 calc R U . . .
B31 B 0.8528(3) 0.71163(14) 0.44003(9) 0.0273(3) Uani 1 1 d . . . . .
O32 O 0.98156(18) 0.64448(9) 0.46205(6) 0.0302(2) Uani 1 1 d . . . . .
C33 C 1.0828(3) 0.70946(13) 0.54070(8) 0.0287(3) Uani 1 1 d . . . . .
C34 C 1.0741(3) 0.84083(13) 0.54701(8) 0.0293(3) Uani 1 1 d . . . . .
O35 O 0.88085(18) 0.82327(9) 0.49114(6) 0.0318(3) Uani 1 1 d . . . . .
C36 C 0.9365(3) 0.65672(16) 0.58973(10) 0.0402(4) Uani 1 1 d . . . . .
H36A H 0.9983 0.6977 0.6431 0.060 Uiso 1 1 calc R U . . .
H36B H 0.7844 0.6669 0.5804 0.060 Uiso 1 1 calc R U . . .
H36C H 0.9322 0.5713 0.5775 0.060 Uiso 1 1 calc R U . . .
C37 C 1.3165(3) 0.68942(15) 0.55213(10) 0.0376(4) Uani 1 1 d . . . . .
H37A H 1.3864 0.7324 0.6045 0.056 Uiso 1 1 calc R U . . .
H37B H 1.3068 0.6037 0.5414 0.056 Uiso 1 1 calc R U . . .
H37C H 1.4073 0.7192 0.5178 0.056 Uiso 1 1 calc R U . . .
C38 C 1.2754(3) 0.90726(15) 0.52178(10) 0.0400(4) Uani 1 1 d . . . . .
H38A H 1.4098 0.9211 0.5578 0.060 Uiso 1 1 calc R U . . .
H38B H 1.2955 0.8594 0.4715 0.060 Uiso 1 1 calc R U . . .
H38C H 1.2509 0.9842 0.5198 0.060 Uiso 1 1 calc R U . . .
C39 C 1.0322(3) 0.91589(16) 0.62285(9) 0.0432(4) Uani 1 1 d . . . . .
H39A H 1.1600 0.9289 0.6614 0.065 Uiso 1 1 calc R U . . .
H39B H 1.0135 0.9932 0.6195 0.065 Uiso 1 1 calc R U . . .
H39C H 0.8960 0.8742 0.6367 0.065 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.344(2) . ?
C1 C11 1.491(2) . ?
C1 B31 1.560(2) . ?
C2 C21 1.474(2) . ?
C2 H2 0.9500 . ?
C11 C12 1.386(2) . ?
C11 C16 1.391(2) . ?
C12 C13 1.388(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.390(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.388(2) . ?
C14 C17 1.535(2) . ?
C15 C16 1.384(2) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C20 1.527(3) . ?
C17 C19 1.529(3) . ?
C17 C18 1.532(2) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
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 C22 1.389(2) . ?
C21 C26 1.397(2) . ?
C22 C23 1.391(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.388(2) . ?
C23 H23 0.9500 . ?
C24 C25 1.395(2) . ?
C24 C27 1.534(2) . ?
C25 C26 1.382(2) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C30 1.527(2) . ?
C27 C28 1.534(2) . ?
C27 C29 1.534(3) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
B31 O32 1.365(2) . ?
B31 O35 1.3700(19) . ?
O32 C33 1.4660(17) . ?
C33 C36 1.513(2) . ?
C33 C37 1.518(2) . ?
C33 C34 1.564(2) . ?
C34 O35 1.4607(17) . ?
C34 C39 1.514(2) . ?
C34 C38 1.517(2) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C11 123.91(13) . . ?
C2 C1 B31 117.62(13) . . ?
C11 C1 B31 118.43(13) . . ?
C1 C2 C21 131.54(14) . . ?
C1 C2 H2 114.2 . . ?
C21 C2 H2 114.2 . . ?
C12 C11 C16 117.59(14) . . ?
C12 C11 C1 121.43(13) . . ?
C16 C11 C1 120.98(14) . . ?
C11 C12 C13 121.14(14) . . ?
C11 C12 H12 119.4 . . ?
C13 C12 H12 119.4 . . ?
C12 C13 C14 121.67(15) . . ?
C12 C13 H13 119.2 . . ?
C14 C13 H13 119.2 . . ?
C15 C14 C13 116.64(14) . . ?
C15 C14 C17 120.47(14) . . ?
C13 C14 C17 122.86(14) . . ?
C16 C15 C14 122.13(14) . . ?
C16 C15 H15 118.9 . . ?
C14 C15 H15 118.9 . . ?
C15 C16 C11 120.82(15) . . ?
C15 C16 H16 119.6 . . ?
C11 C16 H16 119.6 . . ?
C20 C17 C19 108.22(16) . . ?
C20 C17 C18 108.42(16) . . ?
C19 C17 C18 109.23(16) . . ?
C20 C17 C14 111.77(14) . . ?
C19 C17 C14 110.76(14) . . ?
C18 C17 C14 108.38(13) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C26 116.81(13) . . ?
C22 C21 C2 118.41(13) . . ?
C26 C21 C2 124.75(14) . . ?
C21 C22 C23 122.16(14) . . ?
C21 C22 H22 118.9 . . ?
C23 C22 H22 118.9 . . ?
C24 C23 C22 121.03(15) . . ?
C24 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?
C23 C24 C25 116.73(13) . . ?
C23 C24 C27 122.88(14) . . ?
C25 C24 C27 120.37(13) . . ?
C26 C25 C24 122.37(13) . . ?
C26 C25 H25 118.8 . . ?
C24 C25 H25 118.8 . . ?
C25 C26 C21 120.88(14) . . ?
C25 C26 H26 119.6 . . ?
C21 C26 H26 119.6 . . ?
C30 C27 C28 108.53(15) . . ?
C30 C27 C24 112.09(13) . . ?
C28 C27 C24 109.66(13) . . ?
C30 C27 C29 108.89(15) . . ?
C28 C27 C29 108.86(14) . . ?
C24 C27 C29 108.76(14) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O32 B31 O35 113.51(13) . . ?
O32 B31 C1 124.17(13) . . ?
O35 B31 C1 122.31(13) . . ?
B31 O32 C33 107.17(11) . . ?
O32 C33 C36 106.66(13) . . ?
O32 C33 C37 108.55(12) . . ?
C36 C33 C37 110.01(13) . . ?
O32 C33 C34 101.94(11) . . ?
C36 C33 C34 113.80(13) . . ?
C37 C33 C34 115.12(13) . . ?
O35 C34 C39 107.95(13) . . ?
O35 C34 C38 106.57(12) . . ?
C39 C34 C38 110.48(14) . . ?
O35 C34 C33 102.39(11) . . ?
C39 C34 C33 115.61(13) . . ?
C38 C34 C33 113.01(13) . . ?
B31 O35 C34 106.85(11) . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C33 C37 H37A 109.5 . . ?
C33 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C33 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C34 C38 H38A 109.5 . . ?
C34 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C34 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C34 C39 H39A 109.5 . . ?
C34 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C34 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C11 C1 C2 C21 -3.8(3) . . . . ?
B31 C1 C2 C21 178.43(15) . . . . ?
C2 C1 C11 C12 114.24(18) . . . . ?
B31 C1 C11 C12 -67.99(19) . . . . ?
C2 C1 C11 C16 -65.9(2) . . . . ?
B31 C1 C11 C16 111.88(17) . . . . ?
C16 C11 C12 C13 1.3(2) . . . . ?
C1 C11 C12 C13 -178.80(14) . . . . ?
C11 C12 C13 C14 -1.1(3) . . . . ?
C12 C13 C14 C15 0.2(2) . . . . ?
C12 C13 C14 C17 178.26(15) . . . . ?
C13 C14 C15 C16 0.4(2) . . . . ?
C17 C14 C15 C16 -177.75(14) . . . . ?
C14 C15 C16 C11 -0.1(2) . . . . ?
C12 C11 C16 C15 -0.8(2) . . . . ?
C1 C11 C16 C15 179.35(14) . . . . ?
C15 C14 C17 C20 -166.28(16) . . . . ?
C13 C14 C17 C20 15.7(2) . . . . ?
C15 C14 C17 C19 -45.5(2) . . . . ?
C13 C14 C17 C19 136.47(17) . . . . ?
C15 C14 C17 C18 74.3(2) . . . . ?
C13 C14 C17 C18 -103.71(19) . . . . ?
C1 C2 C21 C22 165.13(17) . . . . ?
C1 C2 C21 C26 -16.8(3) . . . . ?
C26 C21 C22 C23 0.2(2) . . . . ?
C2 C21 C22 C23 178.38(15) . . . . ?
C21 C22 C23 C24 -1.1(3) . . . . ?
C22 C23 C24 C25 1.1(2) . . . . ?
C22 C23 C24 C27 -177.10(15) . . . . ?
C23 C24 C25 C26 -0.2(2) . . . . ?
C27 C24 C25 C26 178.08(15) . . . . ?
C24 C25 C26 C21 -0.8(3) . . . . ?
C22 C21 C26 C25 0.8(2) . . . . ?
C2 C21 C26 C25 -177.33(15) . . . . ?
C23 C24 C27 C30 -5.1(2) . . . . ?
C25 C24 C27 C30 176.74(16) . . . . ?
C23 C24 C27 C28 -125.72(17) . . . . ?
C25 C24 C27 C28 56.1(2) . . . . ?
C23 C24 C27 C29 115.34(18) . . . . ?
C25 C24 C27 C29 -62.8(2) . . . . ?
C2 C1 B31 O32 -179.69(15) . . . . ?
C11 C1 B31 O32 2.4(2) . . . . ?
C2 C1 B31 O35 1.3(2) . . . . ?
C11 C1 B31 O35 -176.62(14) . . . . ?
O35 B31 O32 C33 9.07(17) . . . . ?
C1 B31 O32 C33 -170.03(14) . . . . ?
B31 O32 C33 C36 96.77(14) . . . . ?
B31 O32 C33 C37 -144.73(13) . . . . ?
B31 O32 C33 C34 -22.82(15) . . . . ?
O32 C33 C34 O35 27.91(14) . . . . ?
C36 C33 C34 O35 -86.51(14) . . . . ?
C37 C33 C34 O35 145.19(13) . . . . ?
O32 C33 C34 C39 145.00(13) . . . . ?
C36 C33 C34 C39 30.57(19) . . . . ?
C37 C33 C34 C39 -97.73(17) . . . . ?
O32 C33 C34 C38 -86.32(14) . . . . ?
C36 C33 C34 C38 159.25(14) . . . . ?
C37 C33 C34 C38 30.95(17) . . . . ?
O32 B31 O35 C34 10.35(17) . . . . ?
C1 B31 O35 C34 -170.54(14) . . . . ?
C39 C34 O35 B31 -146.06(14) . . . . ?
C38 C34 O35 B31 95.25(14) . . . . ?
C33 C34 O35 B31 -23.63(15) . . . . ?

_refine_diff_density_max         0.252
_refine_diff_density_min         -0.180
_refine_diff_density_rms         0.038

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_wa1968
_audit_block_doi                 10.5517/ccdc.csd.cc216r34
_database_code_depnum_ccdc_archive 'CCDC 1883315'
_audit_update_record             
;
2018-12-05 deposited with the CCDC.
2018-12-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
; 
 ; 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H32 B2 O4'
_chemical_formula_sum            'C26 H32 B2 O4'
_chemical_formula_weight         430.13

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   10.4796(8)
_cell_length_b                   10.8034(11)
_cell_length_c                   21.3385(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2415.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    13620
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      26.48

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_F_000             920
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.340
_exptl_absorpt_coefficient_mu    0.077
_shelx_estimated_absorpt_T_min   0.972
_shelx_estimated_absorpt_T_max   0.974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_T_max  0.886
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'

_exptl_special_details           
; 
 ; 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8005
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.683
_diffrn_reflns_theta_max         25.927
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             4662
_reflns_number_gt                4274
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.757
_reflns_Friedel_fraction_max     0.988
_reflns_Friedel_fraction_full    0.995

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  SHELXL97

_refine_special_details          
; 
 ; 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0749P)²+0.0787P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Flack x determined using 1732 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.4(10)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4662
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0417
_refine_ls_wR_factor_ref         0.1134
_refine_ls_wR_factor_gt          0.1107
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6392(2) 0.52220(18) 0.47912(10) 0.0355(4) Uani 1 1 d . . . . .
C2 C 0.6481(2) 0.51082(18) 0.41519(11) 0.0356(4) Uani 1 1 d . . . . .
C3 C 0.7589(2) 0.55677(19) 0.38203(11) 0.0387(5) Uani 1 1 d . . . . .
C4 C 0.7720(2) 0.5423(2) 0.31655(12) 0.0481(6) Uani 1 1 d . . . . .
H4 H 0.7046 0.5049 0.2936 0.058 Uiso 1 1 calc R U . . .
C5 C 0.8787(3) 0.5803(3) 0.28523(14) 0.0578(7) Uani 1 1 d . . . . .
H5 H 0.8852 0.5690 0.2412 0.069 Uiso 1 1 calc R U . . .
C6 C 0.9769(3) 0.6354(3) 0.31823(15) 0.0610(7) Uani 1 1 d . . . . .
H6 H 1.0510 0.6626 0.2966 0.073 Uiso 1 1 calc R U . . .
C7 C 0.9689(3) 0.6513(2) 0.38174(14) 0.0530(6) Uani 1 1 d . . . . .
H7 H 1.0380 0.6887 0.4034 0.064 Uiso 1 1 calc R U . . .
C8 C 0.8601(2) 0.6133(2) 0.41574(12) 0.0411(5) Uani 1 1 d . . . . .
C9 C 0.8478(2) 0.63089(19) 0.48292(12) 0.0409(5) Uani 1 1 d . . . . .
C10 C 0.9406(2) 0.6941(2) 0.51871(14) 0.0513(6) Uani 1 1 d . . . . .
H10 H 1.0154 0.7235 0.4985 0.062 Uiso 1 1 calc R U . . .
C11 C 0.9259(3) 0.7141(2) 0.58135(15) 0.0575(7) Uani 1 1 d . . . . .
H11 H 0.9901 0.7570 0.6041 0.069 Uiso 1 1 calc R U . . .
C12 C 0.8176(3) 0.6721(2) 0.61196(13) 0.0522(6) Uani 1 1 d . . . . .
H12 H 0.8069 0.6871 0.6555 0.063 Uiso 1 1 calc R U . . .
C13 C 0.7254(2) 0.6083(2) 0.57904(12) 0.0437(5) Uani 1 1 d . . . . .
H13 H 0.6519 0.5787 0.6004 0.052 Uiso 1 1 calc R U . . .
C14 C 0.7382(2) 0.58631(18) 0.51409(11) 0.0371(5) Uani 1 1 d . . . . .
B21 B 0.5220(2) 0.4664(2) 0.51463(11) 0.0357(5) Uani 1 1 d . . . . .
O22 O 0.39943(14) 0.48401(14) 0.49587(7) 0.0384(4) Uani 1 1 d . . . . .
C23 C 0.3174(2) 0.4400(2) 0.54677(10) 0.0392(5) Uani 1 1 d . . . . .
C24 C 0.4059(2) 0.3455(2) 0.58040(11) 0.0414(5) Uani 1 1 d . . . . .
O25 O 0.53197(15) 0.39708(16) 0.56853(8) 0.0445(4) Uani 1 1 d . . . . .
C26 C 0.2859(3) 0.5534(3) 0.58610(14) 0.0559(6) Uani 1 1 d . . . . .
H26A H 0.3646 0.5876 0.6038 0.084 Uiso 1 1 calc R U . . .
H26B H 0.2280 0.5298 0.6201 0.084 Uiso 1 1 calc R U . . .
H26C H 0.2447 0.6159 0.5597 0.084 Uiso 1 1 calc R U . . .
C27 C 0.1969(2) 0.3859(3) 0.51968(12) 0.0516(6) Uani 1 1 d . . . . .
H27A H 0.2180 0.3127 0.4947 0.077 Uiso 1 1 calc R U . . .
H27B H 0.1552 0.4476 0.4930 0.077 Uiso 1 1 calc R U . . .
H27C H 0.1392 0.3623 0.5538 0.077 Uiso 1 1 calc R U . . .
C28 C 0.3867(3) 0.3358(3) 0.65073(12) 0.0605(7) Uani 1 1 d . . . . .
H28A H 0.3884 0.4188 0.6693 0.091 Uiso 1 1 calc R U . . .
H28B H 0.4552 0.2856 0.6689 0.091 Uiso 1 1 calc R U . . .
H28C H 0.3042 0.2968 0.6594 0.091 Uiso 1 1 calc R U . . .
C29 C 0.4037(3) 0.2181(2) 0.55041(15) 0.0550(6) Uani 1 1 d . . . . .
H29A H 0.4162 0.2262 0.5051 0.082 Uiso 1 1 calc R U . . .
H29B H 0.3212 0.1786 0.5586 0.082 Uiso 1 1 calc R U . . .
H29C H 0.4722 0.1674 0.5682 0.082 Uiso 1 1 calc R U . . .
B31 B 0.5430(2) 0.4382(2) 0.37718(12) 0.0365(5) Uani 1 1 d . . . . .
O32 O 0.47666(18) 0.48506(15) 0.32803(8) 0.0483(4) Uani 1 1 d . . . . .
C33 C 0.3786(2) 0.3939(2) 0.31142(12) 0.0460(6) Uani 1 1 d . . . . .
C34 C 0.4359(3) 0.2733(2) 0.33790(11) 0.0461(6) Uani 1 1 d . . . . .
O35 O 0.51561(17) 0.31817(14) 0.38962(8) 0.0434(4) Uani 1 1 d . . . . .
C36 C 0.3566(3) 0.3956(3) 0.24204(13) 0.0681(8) Uani 1 1 d . . . . .
H36A H 0.4343 0.3686 0.2204 0.102 Uiso 1 1 calc R U . . .
H36B H 0.3348 0.4798 0.2287 0.102 Uiso 1 1 calc R U . . .
H36C H 0.2863 0.3395 0.2316 0.102 Uiso 1 1 calc R U . . .
C37 C 0.2593(3) 0.4349(4) 0.34635(18) 0.0732(9) Uani 1 1 d . . . . .
H37A H 0.2755 0.4328 0.3916 0.110 Uiso 1 1 calc R U . . .
H37B H 0.1886 0.3790 0.3362 0.110 Uiso 1 1 calc R U . . .
H37C H 0.2369 0.5194 0.3337 0.110 Uiso 1 1 calc R U . . .
C38 C 0.5262(4) 0.2109(3) 0.29218(17) 0.0765(10) Uani 1 1 d . . . . .
H38A H 0.5873 0.2719 0.2761 0.115 Uiso 1 1 calc R U . . .
H38B H 0.4773 0.1761 0.2572 0.115 Uiso 1 1 calc R U . . .
H38C H 0.5725 0.1445 0.3137 0.115 Uiso 1 1 calc R U . . .
C39 C 0.3411(4) 0.1813(3) 0.36379(16) 0.0752(10) Uani 1 1 d . . . . .
H39A H 0.3867 0.1085 0.3796 0.113 Uiso 1 1 calc R U . . .
H39B H 0.2821 0.1560 0.3305 0.113 Uiso 1 1 calc R U . . .
H39C H 0.2930 0.2196 0.3981 0.113 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.373(3) . ?
C1 C14 1.454(3) . ?
C1 B21 1.564(3) . ?
C2 C3 1.448(3) . ?
C2 B31 1.577(3) . ?
C3 C4 1.413(3) . ?
C3 C8 1.419(3) . ?
C4 C5 1.365(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.382(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.369(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.413(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.452(3) . ?
C9 C10 1.412(3) . ?
C9 C14 1.412(3) . ?
C10 C11 1.363(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.386(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.379(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.413(3) . ?
C13 H13 0.9500 . ?
B21 O22 1.359(3) . ?
B21 O25 1.377(3) . ?
O22 C23 1.464(3) . ?
C23 C27 1.506(3) . ?
C23 C26 1.521(3) . ?
C23 C24 1.555(3) . ?
C24 O25 1.456(3) . ?
C24 C29 1.518(4) . ?
C24 C28 1.518(3) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
B31 O32 1.356(3) . ?
B31 O35 1.355(3) . ?
O32 C33 1.467(3) . ?
C33 C36 1.498(4) . ?
C33 C37 1.522(4) . ?
C33 C34 1.542(3) . ?
C34 O35 1.466(3) . ?
C34 C39 1.510(4) . ?
C34 C38 1.517(4) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C14 120.3(2) . . ?
C2 C1 B21 120.03(19) . . ?
C14 C1 B21 119.71(19) . . ?
C1 C2 C3 120.6(2) . . ?
C1 C2 B31 120.54(19) . . ?
C3 C2 B31 118.65(19) . . ?
C4 C3 C8 118.5(2) . . ?
C4 C3 C2 121.6(2) . . ?
C8 C3 C2 119.9(2) . . ?
C5 C4 C3 122.0(3) . . ?
C5 C4 H4 119.0 . . ?
C3 C4 H4 119.0 . . ?
C4 C5 C6 119.3(3) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
C7 C6 C5 120.8(2) . . ?
C7 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C6 C7 C8 121.4(3) . . ?
C6 C7 H7 119.3 . . ?
C8 C7 H7 119.3 . . ?
C7 C8 C3 117.9(2) . . ?
C7 C8 C9 122.7(2) . . ?
C3 C8 C9 119.4(2) . . ?
C10 C9 C14 118.0(2) . . ?
C10 C9 C8 122.5(2) . . ?
C14 C9 C8 119.5(2) . . ?
C11 C10 C9 122.0(2) . . ?
C11 C10 H10 119.0 . . ?
C9 C10 H10 119.0 . . ?
C10 C11 C12 120.2(2) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C13 C12 C11 119.8(3) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C12 C13 C14 121.1(2) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
C9 C14 C13 118.8(2) . . ?
C9 C14 C1 120.1(2) . . ?
C13 C14 C1 121.0(2) . . ?
O22 B21 O25 113.20(19) . . ?
O22 B21 C1 123.07(19) . . ?
O25 B21 C1 123.7(2) . . ?
B21 O22 C23 106.92(16) . . ?
O22 C23 C27 109.46(18) . . ?
O22 C23 C26 106.00(19) . . ?
C27 C23 C26 110.0(2) . . ?
O22 C23 C24 101.85(17) . . ?
C27 C23 C24 115.0(2) . . ?
C26 C23 C24 113.8(2) . . ?
O25 C24 C29 106.7(2) . . ?
O25 C24 C28 108.6(2) . . ?
C29 C24 C28 110.6(2) . . ?
O25 C24 C23 102.11(16) . . ?
C29 C24 C23 113.1(2) . . ?
C28 C24 C23 115.0(2) . . ?
B21 O25 C24 106.53(17) . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 C27 H27A 109.5 . . ?
C23 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C23 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C24 C28 H28A 109.5 . . ?
C24 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C24 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C24 C29 H29A 109.5 . . ?
C24 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C24 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O32 B31 O35 113.6(2) . . ?
O32 B31 C2 124.78(19) . . ?
O35 B31 C2 121.6(2) . . ?
B31 O32 C33 107.19(17) . . ?
O32 C33 C36 109.8(2) . . ?
O32 C33 C37 105.2(2) . . ?
C36 C33 C37 110.7(3) . . ?
O32 C33 C34 101.88(18) . . ?
C36 C33 C34 115.6(2) . . ?
C37 C33 C34 112.7(2) . . ?
O35 C34 C39 108.5(2) . . ?
O35 C34 C38 106.0(2) . . ?
C39 C34 C38 110.7(3) . . ?
O35 C34 C33 102.63(18) . . ?
C39 C34 C33 115.7(3) . . ?
C38 C34 C33 112.5(2) . . ?
B31 O35 C34 106.83(18) . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C33 C37 H37A 109.5 . . ?
C33 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C33 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C34 C38 H38A 109.5 . . ?
C34 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C34 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C34 C39 H39A 109.5 . . ?
C34 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C34 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C14 C1 C2 C3 3.1(3) . . . . ?
B21 C1 C2 C3 -177.03(18) . . . . ?
C14 C1 C2 B31 178.31(18) . . . . ?
B21 C1 C2 B31 -1.8(3) . . . . ?
C1 C2 C3 C4 177.8(2) . . . . ?
B31 C2 C3 C4 2.5(3) . . . . ?
C1 C2 C3 C8 0.5(3) . . . . ?
B31 C2 C3 C8 -174.75(19) . . . . ?
C8 C3 C4 C5 0.3(4) . . . . ?
C2 C3 C4 C5 -177.0(2) . . . . ?
C3 C4 C5 C6 -0.4(4) . . . . ?
C4 C5 C6 C7 0.5(5) . . . . ?
C5 C6 C7 C8 -0.6(4) . . . . ?
C6 C7 C8 C3 0.5(4) . . . . ?
C6 C7 C8 C9 -178.9(2) . . . . ?
C4 C3 C8 C7 -0.4(3) . . . . ?
C2 C3 C8 C7 177.0(2) . . . . ?
C4 C3 C8 C9 179.0(2) . . . . ?
C2 C3 C8 C9 -3.6(3) . . . . ?
C7 C8 C9 C10 3.9(3) . . . . ?
C3 C8 C9 C10 -175.5(2) . . . . ?
C7 C8 C9 C14 -177.6(2) . . . . ?
C3 C8 C9 C14 3.0(3) . . . . ?
C14 C9 C10 C11 -1.0(4) . . . . ?
C8 C9 C10 C11 177.5(2) . . . . ?
C9 C10 C11 C12 0.0(4) . . . . ?
C10 C11 C12 C13 0.9(4) . . . . ?
C11 C12 C13 C14 -0.9(4) . . . . ?
C10 C9 C14 C13 0.9(3) . . . . ?
C8 C9 C14 C13 -177.59(19) . . . . ?
C10 C9 C14 C1 179.14(19) . . . . ?
C8 C9 C14 C1 0.6(3) . . . . ?
C12 C13 C14 C9 0.0(3) . . . . ?
C12 C13 C14 C1 -178.2(2) . . . . ?
C2 C1 C14 C9 -3.7(3) . . . . ?
B21 C1 C14 C9 176.44(18) . . . . ?
C2 C1 C14 C13 174.46(19) . . . . ?
B21 C1 C14 C13 -5.4(3) . . . . ?
C2 C1 B21 O22 -47.6(3) . . . . ?
C14 C1 B21 O22 132.2(2) . . . . ?
C2 C1 B21 O25 133.8(2) . . . . ?
C14 C1 B21 O25 -46.3(3) . . . . ?
O25 B21 O22 C23 9.8(2) . . . . ?
C1 B21 O22 C23 -168.84(19) . . . . ?
B21 O22 C23 C27 -146.7(2) . . . . ?
B21 O22 C23 C26 94.7(2) . . . . ?
B21 O22 C23 C24 -24.6(2) . . . . ?
O22 C23 C24 O25 30.0(2) . . . . ?
C27 C23 C24 O25 148.2(2) . . . . ?
C26 C23 C24 O25 -83.6(2) . . . . ?
O22 C23 C24 C29 -84.3(2) . . . . ?
C27 C23 C24 C29 34.0(3) . . . . ?
C26 C23 C24 C29 162.1(2) . . . . ?
O22 C23 C24 C28 147.3(2) . . . . ?
C27 C23 C24 C28 -94.4(3) . . . . ?
C26 C23 C24 C28 33.7(3) . . . . ?
O22 B21 O25 C24 10.9(3) . . . . ?
C1 B21 O25 C24 -170.4(2) . . . . ?
C29 C24 O25 B21 93.6(2) . . . . ?
C28 C24 O25 B21 -147.1(2) . . . . ?
C23 C24 O25 B21 -25.2(2) . . . . ?
C1 C2 B31 O32 125.4(2) . . . . ?
C3 C2 B31 O32 -59.3(3) . . . . ?
C1 C2 B31 O35 -58.0(3) . . . . ?
C3 C2 B31 O35 117.3(2) . . . . ?
O35 B31 O32 C33 10.0(3) . . . . ?
C2 B31 O32 C33 -173.2(2) . . . . ?
B31 O32 C33 C36 -146.3(2) . . . . ?
B31 O32 C33 C37 94.6(2) . . . . ?
B31 O32 C33 C34 -23.2(2) . . . . ?
O32 C33 C34 O35 27.4(2) . . . . ?
C36 C33 C34 O35 146.4(2) . . . . ?
C37 C33 C34 O35 -84.8(3) . . . . ?
O32 C33 C34 C39 145.3(2) . . . . ?
C36 C33 C34 C39 -95.7(3) . . . . ?
C37 C33 C34 C39 33.1(3) . . . . ?
O32 C33 C34 C38 -86.1(2) . . . . ?
C36 C33 C34 C38 32.9(3) . . . . ?
C37 C33 C34 C38 161.7(2) . . . . ?
O32 B31 O35 C34 8.9(3) . . . . ?
C2 B31 O35 C34 -168.0(2) . . . . ?
C39 C34 O35 B31 -145.7(3) . . . . ?
C38 C34 O35 B31 95.5(3) . . . . ?
C33 C34 O35 B31 -22.7(3) . . . . ?

_refine_diff_density_max         0.152
_refine_diff_density_min         -0.158
_refine_diff_density_rms         0.032

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_wa2631
_database_code_depnum_ccdc_archive 'CCDC 1883335'
_audit_update_record             
;
2018-12-18 deposited with the CCDC.
2018-12-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C50 H46 B2 S4'
_chemical_formula_sum            'C50 H46 B2 S4'
_chemical_formula_weight         796.73

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   7.965(2)
_cell_length_b                   10.844(3)
_cell_length_c                   13.205(4)
_cell_angle_alpha                96.17(2)
_cell_angle_beta                 107.48(2)
_cell_angle_gamma                100.62(2)
_cell_volume                     1053.0(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3631
_cell_measurement_theta_min      3.29
_cell_measurement_theta_max      25.65

_exptl_crystal_description       block
_exptl_crystal_colour            'light orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_F_000             420
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    0.261
_shelx_estimated_absorpt_T_min   0.947
_shelx_estimated_absorpt_T_max   0.972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.662
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8159
_diffrn_reflns_av_unetI/netI     0.1847
_diffrn_reflns_av_R_equivalents  0.0858
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.513
_diffrn_reflns_theta_max         25.638
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             3935
_reflns_number_gt                1723
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .


_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0482P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3935
_refine_ls_number_parameters     290
_refine_ls_number_restraints     52
_refine_ls_R_factor_all          0.1483
_refine_ls_R_factor_gt           0.0619
_refine_ls_wR_factor_ref         0.1446
_refine_ls_wR_factor_gt          0.1248
_refine_ls_goodness_of_fit_ref   0.808
_refine_ls_restrained_S_all      0.816
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
B1 B 0.3564(8) 0.0201(4) 0.4029(4) 0.0411(13) Uani 1 1 d . . . . .
C1 C 0.4318(6) 0.1210(3) 0.5088(3) 0.0359(10) Uani 1 1 d . . . . .
C11 C 0.5581(6) 0.0979(3) 0.6007(3) 0.0402(11) Uani 1 1 d . . . . .
C12 C 0.6092(6) 0.1857(4) 0.6955(3) 0.0420(11) Uani 1 1 d . . . . .
H12 H 0.694635 0.170932 0.758090 0.050 Uiso 1 1 calc R U . . .
C13 C 0.5409(6) 0.2938(4) 0.7028(3) 0.0395(11) Uani 1 1 d . . . . .
C3 C 0.4209(6) 0.3199(4) 0.6115(3) 0.0363(11) Uani 1 1 d . . . . .
C2 C 0.3684(6) 0.2316(3) 0.5162(3) 0.0374(11) Uani 1 1 d . . . . .
H2 H 0.285379 0.248041 0.453392 0.045 Uiso 1 1 calc R U . . .
C14 C 0.6058(6) 0.3754(4) 0.8119(3) 0.0421(12) Uani 1 1 d D . . . .
S2 S 0.74512(18) 0.52371(11) 0.84149(10) 0.0499(4) Uani 1 1 d D . . . .
C17 C 0.7699(6) 0.5364(4) 0.9757(3) 0.0460(12) Uani 1 1 d D . . . .
C16 C 0.6756(7) 0.4312(4) 0.9949(4) 0.0560(14) Uani 1 1 d D . . . .
H16 H 0.671153 0.420090 1.064536 0.067 Uiso 1 1 calc R U . . .
C15 C 0.5838(7) 0.3387(4) 0.9017(3) 0.0528(13) Uani 1 1 d D . . . .
H15 H 0.513112 0.258205 0.902364 0.063 Uiso 1 1 calc R U . . .
C41 C 0.8868(7) 0.6537(4) 1.0557(4) 0.0639(15) Uani 1 1 d D . . . .
H41A H 0.903225 0.637192 1.129144 0.096 Uiso 1 1 calc R U . . .
H41B H 0.827951 0.725258 1.044413 0.096 Uiso 1 1 calc R U . . .
H41C H 1.004828 0.674746 1.045278 0.096 Uiso 1 1 calc R U . . .
C4 C 0.3409(6) 0.4314(4) 0.6104(3) 0.0453(12) Uani 1 1 d D U . . .
S1 S 0.2671(3) 0.49169(17) 0.70620(14) 0.0437(6) Uani 0.767(5) 1 d D . P A 1
C5' C 0.276(5) 0.455(3) 0.693(2) 0.074(9) Uani 0.233(5) 1 d D U P A 2
H5' H 0.281349 0.403909 0.747131 0.089 Uiso 0.233(5) 1 calc R U P A 2
C7 C 0.1817(10) 0.6033(6) 0.6357(7) 0.0387(17) Uani 0.767(5) 1 d D . P A 1
C6 C 0.2109(8) 0.5976(5) 0.5409(5) 0.0421(17) Uani 0.767(5) 1 d D . P A 1
H6 H 0.175698 0.649988 0.488720 0.051 Uiso 0.767(5) 1 calc R U P A 1
C5 C 0.3030(19) 0.5000(11) 0.5321(8) 0.019(2) Uani 0.767(5) 1 d D U P A 1
H5 H 0.338144 0.483110 0.470262 0.023 Uiso 0.767(5) 1 calc R U P A 1
S1' S 0.293(2) 0.5174(13) 0.5228(10) 0.067(5) Uani 0.233(5) 1 d D . P A 2
C31 C 0.0973(9) 0.6957(6) 0.6842(5) 0.065(2) Uani 0.767(5) 1 d D . P A 1
H31A H 0.050216 0.748568 0.631583 0.097 Uiso 0.767(5) 1 calc R U P A 1
H31B H 0.188232 0.750240 0.748551 0.097 Uiso 0.767(5) 1 calc R U P A 1
H31C H -0.002013 0.648925 0.704335 0.097 Uiso 0.767(5) 1 calc R U P A 1
C7' C 0.212(5) 0.614(2) 0.602(2) 0.042(10) Uiso 0.233(5) 1 d D . P A 2
C6' C 0.199(3) 0.5634(18) 0.6889(14) 0.038(6) Uiso 0.233(5) 1 d D . P A 2
H6' H 0.147024 0.595000 0.739349 0.045 Uiso 0.233(5) 1 calc R U P A 2
C31' C 0.137(3) 0.7182(17) 0.5520(16) 0.061(6) Uiso 0.233(5) 1 d D . P A 2
H31D H 0.013886 0.682785 0.502243 0.091 Uiso 0.233(5) 1 calc R U P A 2
H31E H 0.213262 0.756708 0.512496 0.091 Uiso 0.233(5) 1 calc R U P A 2
H31F H 0.134436 0.783220 0.608784 0.091 Uiso 0.233(5) 1 calc R U P A 2
C21 C 0.1987(6) 0.0326(3) 0.3061(3) 0.0358(11) Uani 1 1 d . . . . .
C26 C 0.0199(7) -0.0288(4) 0.2943(4) 0.0519(13) Uani 1 1 d . . . . .
C25 C -0.1203(8) -0.0176(5) 0.2068(5) 0.0684(17) Uani 1 1 d . . . . .
H25 H -0.239985 -0.061047 0.198490 0.082 Uiso 1 1 calc R U . . .
C24 C -0.0928(7) 0.0537(6) 0.1318(5) 0.0659(16) Uani 1 1 d . . . . .
C23 C 0.0795(7) 0.1121(5) 0.1423(4) 0.0598(15) Uani 1 1 d . . . . .
H23 H 0.100497 0.159857 0.089237 0.072 Uiso 1 1 calc R U . . .
C22 C 0.2253(6) 0.1036(4) 0.2286(4) 0.0442(12) Uani 1 1 d . . . . .
C27 C -0.0137(9) -0.1103(6) 0.3740(5) 0.088(2) Uani 1 1 d . . . . .
H27A H -0.141980 -0.126183 0.367617 0.133 Uiso 1 1 calc R U . . .
H27B H 0.059812 -0.066569 0.447137 0.133 Uiso 1 1 calc R U . . .
H27C H 0.018947 -0.191635 0.359379 0.133 Uiso 1 1 calc R U . . .
C29 C -0.2507(9) 0.0694(7) 0.0390(5) 0.112(3) Uani 1 1 d . . . . .
H29A H -0.282783 0.150055 0.056943 0.168 Uiso 1 1 calc R U . . .
H29B H -0.354807 -0.001422 0.026518 0.168 Uiso 1 1 calc R U . . .
H29C H -0.216391 0.069684 -0.026313 0.168 Uiso 1 1 calc R U . . .
C28 C 0.4121(7) 0.1699(5) 0.2369(4) 0.0581(14) Uani 1 1 d . . . . .
H28A H 0.462830 0.235664 0.301767 0.087 Uiso 1 1 calc R U . . .
H28B H 0.407552 0.209610 0.173123 0.087 Uiso 1 1 calc R U . . .
H28C H 0.488287 0.108007 0.241142 0.087 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
B1 C21 1.538(7) . ?
B1 C11 1.560(6) 2_656 ?
B1 C1 1.561(6) . ?
C1 C2 1.390(5) . ?
C1 C11 1.404(6) . ?
C11 C12 1.391(5) . ?
C12 C13 1.385(5) . ?
C12 H12 0.9500 . ?
C13 C3 1.389(6) . ?
C13 C14 1.495(5) . ?
C3 C2 1.397(5) . ?
C3 C4 1.466(6) . ?
C2 H2 0.9500 . ?
C14 C15 1.340(6) . ?
C14 S2 1.708(4) . ?
S2 C17 1.710(4) . ?
C17 C16 1.338(6) . ?
C17 C41 1.511(6) . ?
C16 C15 1.407(6) . ?
C16 H16 0.9500 . ?
C15 H15 0.9500 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C4 S1' 1.565(11) . ?
C4 C5 1.333(10) . ?
C4 C5' 1.354(16) . ?
C4 S1 1.669(5) . ?
S1 C7 1.720(7) . ?
C5' C6' 1.423(16) . ?
C5' H5' 0.9500 . ?
C7 C6 1.338(10) . ?
C7 C31 1.495(7) . ?
C6 C5 1.408(10) . ?
C6 H6 0.9500 . ?
C5 H5 0.9500 . ?
S1' C7' 1.739(15) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C7' C6' 1.351(16) . ?
C7' C31' 1.495(15) . ?
C6' H6' 0.9500 . ?
C31' H31D 0.9800 . ?
C31' H31E 0.9800 . ?
C31' H31F 0.9800 . ?
C21 C22 1.387(6) . ?
C21 C26 1.411(6) . ?
C26 C25 1.379(7) . ?
C26 C27 1.498(7) . ?
C25 C24 1.364(8) . ?
C25 H25 0.9500 . ?
C24 C23 1.361(7) . ?
C24 C29 1.520(7) . ?
C23 C22 1.387(6) . ?
C23 H23 0.9500 . ?
C22 C28 1.494(6) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 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
C21 B1 C11 120.4(4) . 2_656 ?
C21 B1 C1 121.9(4) . . ?
C11 B1 C1 117.7(4) 2_656 . ?
C2 C1 C11 118.6(3) . . ?
C2 C1 B1 121.0(4) . . ?
C11 C1 B1 120.3(4) . . ?
C12 C11 C1 118.0(4) . . ?
C12 C11 B1 120.4(4) . 2_656 ?
C1 C11 B1 121.6(3) . 2_656 ?
C13 C12 C11 122.9(4) . . ?
C13 C12 H12 118.5 . . ?
C11 C12 H12 118.5 . . ?
C12 C13 C3 119.6(3) . . ?
C12 C13 C14 115.8(4) . . ?
C3 C13 C14 124.6(4) . . ?
C13 C3 C2 117.7(4) . . ?
C13 C3 C4 123.9(3) . . ?
C2 C3 C4 118.4(4) . . ?
C1 C2 C3 123.2(4) . . ?
C1 C2 H2 118.4 . . ?
C3 C2 H2 118.4 . . ?
C15 C14 C13 125.8(4) . . ?
C15 C14 S2 110.5(3) . . ?
C13 C14 S2 123.2(3) . . ?
C14 S2 C17 92.4(2) . . ?
C16 C17 C41 128.1(4) . . ?
C16 C17 S2 110.6(3) . . ?
C41 C17 S2 121.3(4) . . ?
C17 C16 C15 113.2(4) . . ?
C17 C16 H16 123.4 . . ?
C15 C16 H16 123.4 . . ?
C14 C15 C16 113.4(4) . . ?
C14 C15 H15 123.3 . . ?
C16 C15 H15 123.3 . . ?
C17 C41 H41A 109.5 . . ?
C17 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C17 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
S1' C4 C3 131.1(6) . . ?
C5 C4 C3 127.8(5) . . ?
S1' C4 C5' 113.6(10) . . ?
C3 C4 C5' 114.8(11) . . ?
C5 C4 S1 106.3(5) . . ?
C3 C4 S1 125.8(4) . . ?
C4 S1 C7 94.4(3) . . ?
C6' C5' C4 113.3(15) . . ?
C6' C5' H5' 123.4 . . ?
C4 C5' H5' 123.4 . . ?
C6 C7 C31 127.9(6) . . ?
C6 C7 S1 111.4(4) . . ?
C31 C7 S1 120.6(6) . . ?
C5 C6 C7 107.8(6) . . ?
C5 C6 H6 126.1 . . ?
C7 C6 H6 126.1 . . ?
C6 C5 C4 120.1(8) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C4 S1' C7' 92.6(8) . . ?
C7 C31 H31A 109.5 . . ?
C7 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C7 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C6' C7' C31' 131.7(17) . . ?
C6' C7' S1' 110.7(12) . . ?
C31' C7' S1' 116.2(14) . . ?
C5' C6' C7' 108.7(15) . . ?
C5' C6' H6' 125.6 . . ?
C7' C6' H6' 125.6 . . ?
C7' C31' H31D 109.5 . . ?
C7' C31' H31E 109.5 . . ?
H31D C31' H31E 109.5 . . ?
C7' C31' H31F 109.5 . . ?
H31D C31' H31F 109.5 . . ?
H31E C31' H31F 109.5 . . ?
C22 C21 C26 117.9(4) . . ?
C22 C21 B1 122.2(4) . . ?
C26 C21 B1 120.0(4) . . ?
C25 C26 C21 119.5(5) . . ?
C25 C26 C27 121.0(5) . . ?
C21 C26 C27 119.5(5) . . ?
C24 C25 C26 122.1(5) . . ?
C24 C25 H25 118.9 . . ?
C26 C25 H25 118.9 . . ?
C23 C24 C25 118.6(5) . . ?
C23 C24 C29 120.4(6) . . ?
C25 C24 C29 121.0(6) . . ?
C24 C23 C22 121.5(5) . . ?
C24 C23 H23 119.2 . . ?
C22 C23 H23 119.2 . . ?
C21 C22 C23 120.4(5) . . ?
C21 C22 C28 120.1(4) . . ?
C23 C22 C28 119.6(5) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C24 C29 H29A 109.5 . . ?
C24 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C24 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C22 C28 H28A 109.5 . . ?
C22 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C22 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C21 B1 C1 C2 -5.2(7) . . . . ?
C11 B1 C1 C2 176.9(4) 2_656 . . . ?
C21 B1 C1 C11 171.1(4) . . . . ?
C11 B1 C1 C11 -6.8(7) 2_656 . . . ?
C2 C1 C11 C12 1.8(6) . . . . ?
B1 C1 C11 C12 -174.5(4) . . . . ?
C2 C1 C11 B1 -176.5(4) . . . 2_656 ?
B1 C1 C11 B1 7.1(7) . . . 2_656 ?
C1 C11 C12 C13 0.1(7) . . . . ?
B1 C11 C12 C13 178.5(4) 2_656 . . . ?
C11 C12 C13 C3 -2.4(7) . . . . ?
C11 C12 C13 C14 178.0(4) . . . . ?
C12 C13 C3 C2 2.6(6) . . . . ?
C14 C13 C3 C2 -177.8(4) . . . . ?
C12 C13 C3 C4 180.0(4) . . . . ?
C14 C13 C3 C4 -0.4(7) . . . . ?
C11 C1 C2 C3 -1.6(6) . . . . ?
B1 C1 C2 C3 174.8(4) . . . . ?
C13 C3 C2 C1 -0.7(6) . . . . ?
C4 C3 C2 C1 -178.2(4) . . . . ?
C12 C13 C14 C15 -60.0(6) . . . . ?
C3 C13 C14 C15 120.4(5) . . . . ?
C12 C13 C14 S2 111.1(4) . . . . ?
C3 C13 C14 S2 -68.5(6) . . . . ?
C15 C14 S2 C17 -0.9(4) . . . . ?
C13 C14 S2 C17 -173.2(4) . . . . ?
C14 S2 C17 C16 0.2(4) . . . . ?
C14 S2 C17 C41 179.7(4) . . . . ?
C41 C17 C16 C15 -178.9(5) . . . . ?
S2 C17 C16 C15 0.6(5) . . . . ?
C13 C14 C15 C16 173.5(4) . . . . ?
S2 C14 C15 C16 1.5(5) . . . . ?
C17 C16 C15 C14 -1.4(6) . . . . ?
C13 C3 C4 S1' 143.6(10) . . . . ?
C2 C3 C4 S1' -39.0(11) . . . . ?
C13 C3 C4 C5 144.0(9) . . . . ?
C2 C3 C4 C5 -38.6(10) . . . . ?
C13 C3 C4 C5' -46(2) . . . . ?
C2 C3 C4 C5' 131.4(19) . . . . ?
C13 C3 C4 S1 -40.0(6) . . . . ?
C2 C3 C4 S1 137.3(4) . . . . ?
C5 C4 S1 C7 1.8(7) . . . . ?
C3 C4 S1 C7 -174.8(4) . . . . ?
S1' C4 C5' C6' -8(3) . . . . ?
C3 C4 C5' C6' -180(2) . . . . ?
C4 S1 C7 C6 -1.1(5) . . . . ?
C4 S1 C7 C31 -178.0(6) . . . . ?
C31 C7 C6 C5 176.6(9) . . . . ?
S1 C7 C6 C5 0.1(9) . . . . ?
C7 C6 C5 C4 1.5(14) . . . . ?
C3 C4 C5 C6 174.3(7) . . . . ?
S1 C4 C5 C6 -2.3(13) . . . . ?
C3 C4 S1' C7' -179.7(13) . . . . ?
C5' C4 S1' C7' 10(2) . . . . ?
C4 S1' C7' C6' -10(3) . . . . ?
C4 S1' C7' C31' -178(2) . . . . ?
C4 C5' C6' C7' 0(4) . . . . ?
C31' C7' C6' C5' 172(3) . . . . ?
S1' C7' C6' C5' 7(4) . . . . ?
C11 B1 C21 C22 -96.6(5) 2_656 . . . ?
C1 B1 C21 C22 85.6(5) . . . . ?
C11 B1 C21 C26 83.7(5) 2_656 . . . ?
C1 B1 C21 C26 -94.1(5) . . . . ?
C22 C21 C26 C25 0.7(6) . . . . ?
B1 C21 C26 C25 -179.6(4) . . . . ?
C22 C21 C26 C27 177.7(4) . . . . ?
B1 C21 C26 C27 -2.6(6) . . . . ?
C21 C26 C25 C24 -1.6(7) . . . . ?
C27 C26 C25 C24 -178.5(5) . . . . ?
C26 C25 C24 C23 2.2(7) . . . . ?
C26 C25 C24 C29 -177.1(5) . . . . ?
C25 C24 C23 C22 -2.0(7) . . . . ?
C29 C24 C23 C22 177.3(5) . . . . ?
C26 C21 C22 C23 -0.5(6) . . . . ?
B1 C21 C22 C23 179.8(4) . . . . ?
C26 C21 C22 C28 -179.6(4) . . . . ?
B1 C21 C22 C28 0.6(6) . . . . ?
C24 C23 C22 C21 1.2(7) . . . . ?
C24 C23 C22 C28 -179.7(4) . . . . ?

_refine_diff_density_max         0.224
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.054

####################################################################### 
# 
# 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_wa1847
_database_code_depnum_ccdc_archive 'CCDC 1883328'
_audit_update_record             
;
2018-12-18 deposited with the CCDC.
2018-12-20 downloaded from the CCDC.
;


# start Validation Reply Form
_vrf_PLAT213_wa1847              
;
PROBLEM: Atom C38             has ADP max/min Ratio .....        5.6 prolat
RESPONSE: This atom is one site of a disordered methyl group.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ; 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H50 B2 O4'
_chemical_formula_sum            'C34 H50 B2 O4'
_chemical_formula_weight         544.36

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   11.2074(3)
_cell_length_b                   22.0029(6)
_cell_length_c                   27.0385(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6667.6(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    45265
_cell_measurement_theta_min      1.8
_cell_measurement_theta_max      26.3

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_F_000             2368
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    0.068
_shelx_estimated_absorpt_T_min   0.971
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.971
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'

_exptl_special_details           
; 
 ; 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            74625
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_av_R_equivalents  0.1248
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.851
_diffrn_reflns_theta_max         25.727
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6348
_reflns_number_gt                4950
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .


_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  SHELXL
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1122P)²+8.3819P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6348
_refine_ls_number_parameters     426
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.1071
_refine_ls_R_factor_gt           0.0868
_refine_ls_wR_factor_ref         0.2391
_refine_ls_wR_factor_gt          0.2234
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_restrained_S_all      0.953
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8744(3) 0.11323(14) 0.54094(10) 0.0433(7) Uani 1 1 d . . . . .
C2 C 0.7629(2) 0.11825(13) 0.52282(10) 0.0403(6) Uani 1 1 d . . . . .
C11 C 0.9818(2) 0.12344(13) 0.50882(9) 0.0390(6) Uani 1 1 d . . . . .
C12 C 1.0678(3) 0.07863(14) 0.50111(11) 0.0454(7) Uani 1 1 d . . . . .
H12 H 1.061966 0.041244 0.518516 0.054 Uiso 1 1 calc R U . . .
C13 C 1.1621(3) 0.08760(14) 0.46842(11) 0.0448(7) Uani 1 1 d . . . . .
H13 H 1.217462 0.055635 0.462861 0.054 Uiso 1 1 calc R U . . .
C14 C 1.1766(2) 0.14277(13) 0.44364(10) 0.0423(6) Uani 1 1 d . . . . .
C15 C 1.0929(3) 0.18802(14) 0.45338(10) 0.0440(7) Uani 1 1 d . . . . .
H15 H 1.101663 0.226512 0.437881 0.053 Uiso 1 1 calc R U . . .
C16 C 0.9977(3) 0.17866(14) 0.48488(10) 0.0436(7) Uani 1 1 d . . . . .
H16 H 0.942071 0.210571 0.490257 0.052 Uiso 1 1 calc R U . . .
C17 C 1.2777(3) 0.15552(16) 0.40708(11) 0.0528(8) Uani 1 1 d . . . . .
C18 C 1.3662(4) 0.1039(2) 0.40344(18) 0.0823(13) Uani 1 1 d . . . . .
H18A H 1.399494 0.095464 0.436244 0.123 Uiso 1 1 calc R U . . .
H18B H 1.325867 0.067533 0.390910 0.123 Uiso 1 1 calc R U . . .
H18C H 1.430758 0.115293 0.380792 0.123 Uiso 1 1 calc R U . . .
C19 C 1.3470(4) 0.2125(2) 0.42420(17) 0.0792(12) Uani 1 1 d . . . . .
H19A H 1.291894 0.246944 0.426939 0.119 Uiso 1 1 calc R U . . .
H19B H 1.383610 0.204635 0.456478 0.119 Uiso 1 1 calc R U . . .
H19C H 1.409358 0.222115 0.400025 0.119 Uiso 1 1 calc R U . . .
C20 C 1.2244(4) 0.1698(3) 0.35662(14) 0.0924(15) Uani 1 1 d . . . . .
H20A H 1.167304 0.203305 0.359777 0.139 Uiso 1 1 calc R U . . .
H20B H 1.288170 0.181487 0.333739 0.139 Uiso 1 1 calc R U . . .
H20C H 1.183280 0.133727 0.343856 0.139 Uiso 1 1 calc R U . . .
C21 C 0.7433(2) 0.12801(13) 0.46845(10) 0.0390(6) Uani 1 1 d . . . . .
C22 C 0.7888(3) 0.08670(14) 0.43443(11) 0.0469(7) Uani 1 1 d . . . . .
H22 H 0.828358 0.051211 0.445902 0.056 Uiso 1 1 calc R U . . .
C23 C 0.7773(3) 0.09649(15) 0.38413(11) 0.0521(8) Uani 1 1 d . . . . .
H23 H 0.808057 0.067032 0.361830 0.062 Uiso 1 1 calc R U . . .
C24 C 0.7225(3) 0.14768(15) 0.36529(10) 0.0465(7) Uani 1 1 d . . . . .
C25 C 0.6750(3) 0.18822(15) 0.39946(11) 0.0486(7) Uani 1 1 d . . . . .
H25 H 0.635630 0.223684 0.387841 0.058 Uiso 1 1 calc R U . . .
C26 C 0.6836(2) 0.17836(14) 0.45034(10) 0.0439(7) Uani 1 1 d . . . . .
H26 H 0.648183 0.206392 0.472674 0.053 Uiso 1 1 calc R U . . .
C27 C 0.7163(3) 0.15892(17) 0.30930(11) 0.0569(8) Uani 1 1 d . . . . .
C28 C 0.7752(10) 0.1033(4) 0.2788(3) 0.080(3) Uani 0.468(8) 1 d . . P A 1
H28A H 0.731155 0.065775 0.285780 0.119 Uiso 0.468(8) 1 calc R U P A 1
H28B H 0.771437 0.112045 0.243276 0.119 Uiso 0.468(8) 1 calc R U P A 1
H28C H 0.858667 0.098302 0.288781 0.119 Uiso 0.468(8) 1 calc R U P A 1
C29 C 0.5879(8) 0.1622(5) 0.2928(3) 0.077(3) Uani 0.468(8) 1 d . . P A 1
H29A H 0.546774 0.124528 0.301979 0.115 Uiso 0.468(8) 1 calc R U P A 1
H29B H 0.548704 0.196767 0.308814 0.115 Uiso 0.468(8) 1 calc R U P A 1
H29C H 0.584794 0.167334 0.256798 0.115 Uiso 0.468(8) 1 calc R U P A 1
C30 C 0.7876(10) 0.2146(5) 0.2969(3) 0.074(3) Uani 0.468(8) 1 d . . P A 1
H30A H 0.869708 0.209387 0.308677 0.110 Uiso 0.468(8) 1 calc R U P A 1
H30B H 0.787882 0.220619 0.261041 0.110 Uiso 0.468(8) 1 calc R U P A 1
H30C H 0.751792 0.250053 0.313057 0.110 Uiso 0.468(8) 1 calc R U P A 1
C28' C 0.6517(9) 0.1086(4) 0.2846(2) 0.084(3) Uani 0.532(8) 1 d . . P A 2
H28D H 0.570743 0.105722 0.298068 0.126 Uiso 0.532(8) 1 calc R U P A 2
H28E H 0.647626 0.116517 0.248972 0.126 Uiso 0.532(8) 1 calc R U P A 2
H28F H 0.694099 0.070312 0.290424 0.126 Uiso 0.532(8) 1 calc R U P A 2
C29' C 0.6460(10) 0.2201(5) 0.2975(3) 0.099(4) Uani 0.532(8) 1 d . . P A 2
H29D H 0.686594 0.254381 0.313410 0.148 Uiso 0.532(8) 1 calc R U P A 2
H29E H 0.643734 0.226574 0.261685 0.148 Uiso 0.532(8) 1 calc R U P A 2
H29F H 0.564333 0.217005 0.310258 0.148 Uiso 0.532(8) 1 calc R U P A 2
C30' C 0.8438(9) 0.1673(6) 0.2909(3) 0.092(3) Uani 0.532(8) 1 d . . P A 2
H30D H 0.881220 0.201111 0.308676 0.137 Uiso 0.532(8) 1 calc R U P A 2
H30E H 0.889295 0.129962 0.296857 0.137 Uiso 0.532(8) 1 calc R U P A 2
H30F H 0.842822 0.176168 0.255405 0.137 Uiso 0.532(8) 1 calc R U P A 2
B31 B 0.8972(3) 0.10137(18) 0.59694(13) 0.0486(8) Uani 1 1 d . . . . .
O32 O 0.9981(2) 0.07447(15) 0.61489(8) 0.0757(8) Uani 1 1 d D . . . .
C33 C 0.9717(4) 0.0560(3) 0.66568(13) 0.071(2) Uani 0.596(8) 1 d D . P B 1
C33' C 0.9947(6) 0.0888(3) 0.66770(13) 0.077(4) Uani 0.404(8) 1 d D . P B 2
C34 C 0.8756(4) 0.1018(2) 0.68033(11) 0.0866(14) Uani 1 1 d D . . . .
O35 O 0.8195(2) 0.11582(15) 0.63286(8) 0.0777(8) Uani 1 1 d D . . . .
C36 C 1.0855(5) 0.0513(3) 0.69329(19) 0.140(3) Uani 1 1 d D . . . .
H36A H 1.069204 0.038964 0.727447 0.210 Uiso 0.596(8) 1 calc R U P B 1
H36B H 1.137020 0.021084 0.677434 0.210 Uiso 0.596(8) 1 calc R U P B 1
H36C H 1.125604 0.090926 0.693263 0.210 Uiso 0.596(8) 1 calc R U P B 1
H36D H 1.160008 0.051935 0.674321 0.210 Uiso 0.404(8) 1 calc R U P B 2
H36E H 1.099903 0.067861 0.726421 0.210 Uiso 0.404(8) 1 calc R U P B 2
H36F H 1.056689 0.009432 0.696065 0.210 Uiso 0.404(8) 1 calc R U P B 2
C37 C 0.9332(9) -0.0085(3) 0.6650(3) 0.108(3) Uani 0.596(8) 1 d D . P B 1
H37A H 0.857041 -0.011900 0.647429 0.162 Uiso 0.596(8) 1 calc R U P B 1
H37B H 0.993621 -0.033101 0.648191 0.162 Uiso 0.596(8) 1 calc R U P B 1
H37C H 0.923382 -0.022977 0.699060 0.162 Uiso 0.596(8) 1 calc R U P B 1
C37' C 1.0647(12) 0.1428(5) 0.6830(5) 0.111(5) Uani 0.404(8) 1 d D . P B 2
H37D H 1.149049 0.136365 0.675095 0.166 Uiso 0.404(8) 1 calc R U P B 2
H37E H 1.035392 0.178753 0.665406 0.166 Uiso 0.404(8) 1 calc R U P B 2
H37F H 1.055846 0.148992 0.718742 0.166 Uiso 0.404(8) 1 calc R U P B 2
C38 C 0.7931(13) 0.0779(11) 0.7185(4) 0.276(18) Uani 0.596(8) 1 d D . P B 1
H38A H 0.837645 0.069736 0.748983 0.415 Uiso 0.596(8) 1 calc R U P B 1
H38B H 0.730736 0.108030 0.725143 0.415 Uiso 0.596(8) 1 calc R U P B 1
H38C H 0.756495 0.040206 0.706624 0.415 Uiso 0.596(8) 1 calc R U P B 1
C39 C 0.9305(10) 0.1609(3) 0.6934(3) 0.143(6) Uani 0.596(8) 1 d D . P B 1
H39A H 0.983754 0.173941 0.666630 0.214 Uiso 0.596(8) 1 calc R U P B 1
H39B H 0.867767 0.191397 0.698094 0.214 Uiso 0.596(8) 1 calc R U P B 1
H39C H 0.976424 0.156593 0.724028 0.214 Uiso 0.596(8) 1 calc R U P B 1
C38' C 0.7992(14) 0.0499(7) 0.6951(7) 0.214(17) Uani 0.404(8) 1 d D . P B 2
H38D H 0.718882 0.064740 0.702963 0.322 Uiso 0.404(8) 1 calc R U P B 2
H38E H 0.794601 0.020649 0.667881 0.322 Uiso 0.404(8) 1 calc R U P B 2
H38F H 0.833402 0.030116 0.724318 0.322 Uiso 0.404(8) 1 calc R U P B 2
C39' C 0.826(2) 0.1447(10) 0.7172(6) 0.183(14) Uani 0.404(8) 1 d D . P B 2
H39D H 0.738526 0.142511 0.716577 0.274 Uiso 0.404(8) 1 calc R U P B 2
H39E H 0.854805 0.133926 0.750212 0.274 Uiso 0.404(8) 1 calc R U P B 2
H39F H 0.851287 0.186166 0.709056 0.274 Uiso 0.404(8) 1 calc R U P B 2
B41 B 0.6459(3) 0.11216(15) 0.55469(11) 0.0420(7) Uani 1 1 d . . . . .
O42 O 0.60867(18) 0.05949(10) 0.57590(8) 0.0527(6) Uani 1 1 d . . . . .
C43 C 0.4850(3) 0.06914(15) 0.59164(12) 0.0517(8) Uani 1 1 d . . . . .
C44 C 0.4759(3) 0.13919(15) 0.59448(12) 0.0537(8) Uani 1 1 d . . . . .
O45 O 0.5679(2) 0.15864(10) 0.55982(9) 0.0601(6) Uani 1 1 d . . . . .
C46 C 0.4659(4) 0.0364(2) 0.64026(16) 0.0817(13) Uani 1 1 d . . . . .
H46A H 0.383453 0.042402 0.651301 0.123 Uiso 1 1 calc R U . . .
H46B H 0.481066 -0.007141 0.635786 0.123 Uiso 1 1 calc R U . . .
H46C H 0.520806 0.052674 0.665155 0.123 Uiso 1 1 calc R U . . .
C47 C 0.4075(3) 0.0414(2) 0.55172(16) 0.0728(11) Uani 1 1 d . . . . .
H47A H 0.323272 0.046657 0.560466 0.109 Uiso 1 1 calc R U . . .
H47B H 0.423521 0.061676 0.520129 0.109 Uiso 1 1 calc R U . . .
H47C H 0.425555 -0.001999 0.548720 0.109 Uiso 1 1 calc R U . . .
C48 C 0.3565(4) 0.1651(2) 0.57805(16) 0.0772(12) Uani 1 1 d . . . . .
H48A H 0.294090 0.152243 0.601170 0.116 Uiso 1 1 calc R U . . .
H48B H 0.360979 0.209585 0.577569 0.116 Uiso 1 1 calc R U . . .
H48C H 0.337531 0.150194 0.544813 0.116 Uiso 1 1 calc R U . . .
C49 C 0.5105(4) 0.1653(2) 0.64458(14) 0.0780(12) Uani 1 1 d . . . . .
H49A H 0.451008 0.153392 0.669313 0.117 Uiso 1 1 calc R U . . .
H49B H 0.588904 0.149547 0.654269 0.117 Uiso 1 1 calc R U . . .
H49C H 0.513917 0.209708 0.642424 0.117 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.346(4) . ?
C1 C11 1.501(4) . ?
C1 B31 1.558(4) . ?
C2 C21 1.502(4) . ?
C2 B41 1.575(4) . ?
C11 C16 1.388(4) . ?
C11 C12 1.395(4) . ?
C12 C13 1.391(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.396(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.393(4) . ?
C14 C17 1.530(4) . ?
C15 C16 1.381(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.511(5) . ?
C17 C20 1.522(5) . ?
C17 C19 1.546(5) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
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 C26 1.384(4) . ?
C21 C22 1.390(4) . ?
C22 C23 1.383(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.380(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.390(4) . ?
C24 C27 1.535(4) . ?
C25 C26 1.396(4) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28' 1.482(8) . ?
C27 C30 1.500(9) . ?
C27 C29 1.509(9) . ?
C27 C30' 1.524(10) . ?
C27 C29' 1.592(11) . ?
C27 C28 1.617(9) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C28' H28D 0.9800 . ?
C28' H28E 0.9800 . ?
C28' H28F 0.9800 . ?
C29' H29D 0.9800 . ?
C29' H29E 0.9800 . ?
C29' H29F 0.9800 . ?
C30' H30D 0.9800 . ?
C30' H30E 0.9800 . ?
C30' H30F 0.9800 . ?
B31 O35 1.343(4) . ?
B31 O32 1.366(4) . ?
O32 C33 1.463(3) . ?
O32 C33' 1.463(3) . ?
C33 C36 1.481(4) . ?
C33 C37 1.482(4) . ?
C33 C34 1.527(8) . ?
C33' C34 1.407(8) . ?
C33' C36 1.482(4) . ?
C33' C37' 1.482(4) . ?
C34 C38 1.482(4) . ?
C34 O35 1.462(3) . ?
C34 C39' 1.482(4) . ?
C34 C39 1.482(4) . ?
C34 C38' 1.482(4) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C36 H36D 0.9800 . ?
C36 H36E 0.9800 . ?
C36 H36F 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C37' H37D 0.9800 . ?
C37' H37E 0.9800 . ?
C37' H37F 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C38' H38D 0.9800 . ?
C38' H38E 0.9800 . ?
C38' H38F 0.9800 . ?
C39' H39D 0.9800 . ?
C39' H39E 0.9800 . ?
C39' H39F 0.9800 . ?
B41 O45 1.352(4) . ?
B41 O42 1.359(4) . ?
O42 C43 1.465(4) . ?
C43 C46 1.514(5) . ?
C43 C47 1.514(5) . ?
C43 C44 1.547(5) . ?
C44 O45 1.457(3) . ?
C44 C48 1.521(5) . ?
C44 C49 1.521(5) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C11 121.4(2) . . ?
C2 C1 B31 121.3(3) . . ?
C11 C1 B31 117.1(2) . . ?
C1 C2 C21 120.2(2) . . ?
C1 C2 B41 124.5(2) . . ?
C21 C2 B41 115.2(2) . . ?
C16 C11 C12 117.4(2) . . ?
C16 C11 C1 120.3(3) . . ?
C12 C11 C1 122.3(3) . . ?
C11 C12 C13 121.3(3) . . ?
C11 C12 H12 119.3 . . ?
C13 C12 H12 119.3 . . ?
C12 C13 C14 121.1(3) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
C15 C14 C13 116.9(3) . . ?
C15 C14 C17 119.3(3) . . ?
C13 C14 C17 123.8(3) . . ?
C16 C15 C14 122.0(3) . . ?
C16 C15 H15 119.0 . . ?
C14 C15 H15 119.0 . . ?
C15 C16 C11 121.2(3) . . ?
C15 C16 H16 119.4 . . ?
C11 C16 H16 119.4 . . ?
C18 C17 C20 110.7(3) . . ?
C18 C17 C14 113.0(3) . . ?
C20 C17 C14 109.0(3) . . ?
C18 C17 C19 107.4(3) . . ?
C20 C17 C19 107.4(4) . . ?
C14 C17 C19 109.1(3) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C26 C21 C22 117.8(3) . . ?
C26 C21 C2 122.1(3) . . ?
C22 C21 C2 120.0(3) . . ?
C23 C22 C21 121.0(3) . . ?
C23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C22 C23 C24 122.1(3) . . ?
C22 C23 H23 118.9 . . ?
C24 C23 H23 118.9 . . ?
C23 C24 C25 116.7(3) . . ?
C23 C24 C27 121.0(3) . . ?
C25 C24 C27 122.3(3) . . ?
C24 C25 C26 121.9(3) . . ?
C24 C25 H25 119.0 . . ?
C26 C25 H25 119.0 . . ?
C21 C26 C25 120.4(3) . . ?
C21 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
C30 C27 C29 113.8(6) . . ?
C28' C27 C30' 113.7(6) . . ?
C28' C27 C24 110.3(4) . . ?
C30 C27 C24 109.1(4) . . ?
C29 C27 C24 110.1(4) . . ?
C30' C27 C24 107.4(4) . . ?
C28' C27 C29' 107.4(6) . . ?
C30' C27 C29' 107.3(7) . . ?
C24 C27 C29' 110.8(4) . . ?
C30 C27 C28 106.7(6) . . ?
C29 C27 C28 105.9(6) . . ?
C24 C27 C28 111.3(4) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C27 C28' H28D 109.5 . . ?
C27 C28' H28E 109.5 . . ?
H28D C28' H28E 109.5 . . ?
C27 C28' H28F 109.5 . . ?
H28D C28' H28F 109.5 . . ?
H28E C28' H28F 109.5 . . ?
C27 C29' H29D 109.5 . . ?
C27 C29' H29E 109.5 . . ?
H29D C29' H29E 109.5 . . ?
C27 C29' H29F 109.5 . . ?
H29D C29' H29F 109.5 . . ?
H29E C29' H29F 109.5 . . ?
C27 C30' H30D 109.5 . . ?
C27 C30' H30E 109.5 . . ?
H30D C30' H30E 109.5 . . ?
C27 C30' H30F 109.5 . . ?
H30D C30' H30F 109.5 . . ?
H30E C30' H30F 109.5 . . ?
O35 B31 O32 112.5(3) . . ?
O35 B31 C1 123.9(3) . . ?
O32 B31 C1 123.6(3) . . ?
B31 O32 C33 106.6(3) . . ?
B31 O32 C33' 103.4(3) . . ?
C36 C33 O32 108.5(3) . . ?
C36 C33 C37 101.0(6) . . ?
O32 C33 C37 108.3(5) . . ?
C36 C33 C34 121.4(5) . . ?
O32 C33 C34 101.7(4) . . ?
C37 C33 C34 115.4(6) . . ?
C34 C33' C36 130.6(5) . . ?
C34 C33' C37' 105.8(7) . . ?
C36 C33' C37' 87.3(8) . . ?
C34 C33' O32 107.8(4) . . ?
C36 C33' O32 108.5(3) . . ?
C37' C33' O32 115.6(8) . . ?
C33' C34 O35 103.8(3) . . ?
C38 C34 O35 114.7(7) . . ?
C33' C34 C39' 130.5(11) . . ?
O35 C34 C39' 107.0(8) . . ?
C38 C34 C33 112.7(10) . . ?
O35 C34 C33 102.4(3) . . ?
C38 C34 C39 113.9(10) . . ?
O35 C34 C39 101.7(5) . . ?
C33 C34 C39 110.4(6) . . ?
C33' C34 C38' 117.3(9) . . ?
O35 C34 C38' 98.7(7) . . ?
C39' C34 C38' 95.3(14) . . ?
B31 O35 C34 107.8(3) . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C33' C36 H36D 109.5 . . ?
C33' C36 H36E 109.5 . . ?
H36D C36 H36E 109.5 . . ?
C33' C36 H36F 109.5 . . ?
H36D C36 H36F 109.5 . . ?
H36E C36 H36F 109.5 . . ?
C33 C37 H37A 109.5 . . ?
C33 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C33 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C33' C37' H37D 109.5 . . ?
C33' C37' H37E 109.5 . . ?
H37D C37' H37E 109.5 . . ?
C33' C37' H37F 109.5 . . ?
H37D C37' H37F 109.5 . . ?
H37E C37' H37F 109.5 . . ?
C34 C38 H38A 109.5 . . ?
C34 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C34 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C34 C39 H39A 109.5 . . ?
C34 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C34 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C34 C38' H38D 109.5 . . ?
C34 C38' H38E 109.5 . . ?
H38D C38' H38E 109.5 . . ?
C34 C38' H38F 109.5 . . ?
H38D C38' H38F 109.5 . . ?
H38E C38' H38F 109.5 . . ?
C34 C39' H39D 109.5 . . ?
C34 C39' H39E 109.5 . . ?
H39D C39' H39E 109.5 . . ?
C34 C39' H39F 109.5 . . ?
H39D C39' H39F 109.5 . . ?
H39E C39' H39F 109.5 . . ?
O45 B41 O42 113.8(3) . . ?
O45 B41 C2 122.0(3) . . ?
O42 B41 C2 124.0(3) . . ?
B41 O42 C43 106.8(2) . . ?
O42 C43 C46 108.5(3) . . ?
O42 C43 C47 106.1(3) . . ?
C46 C43 C47 110.3(3) . . ?
O42 C43 C44 102.8(2) . . ?
C46 C43 C44 115.0(3) . . ?
C47 C43 C44 113.5(3) . . ?
O45 C44 C48 108.9(3) . . ?
O45 C44 C49 106.3(3) . . ?
C48 C44 C49 110.1(3) . . ?
O45 C44 C43 102.4(2) . . ?
C48 C44 C43 114.7(3) . . ?
C49 C44 C43 113.8(3) . . ?
B41 O45 C44 107.5(2) . . ?
C43 C46 H46A 109.5 . . ?
C43 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C43 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C43 C47 H47A 109.5 . . ?
C43 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C43 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C44 C48 H48A 109.5 . . ?
C44 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C44 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C44 C49 H49A 109.5 . . ?
C44 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C44 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C11 C1 C2 C21 6.3(4) . . . . ?
B31 C1 C2 C21 -178.4(3) . . . . ?
C11 C1 C2 B41 -176.1(3) . . . . ?
B31 C1 C2 B41 -0.8(5) . . . . ?
C2 C1 C11 C16 58.5(4) . . . . ?
B31 C1 C11 C16 -117.0(3) . . . . ?
C2 C1 C11 C12 -120.5(3) . . . . ?
B31 C1 C11 C12 63.9(4) . . . . ?
C16 C11 C12 C13 -3.7(4) . . . . ?
C1 C11 C12 C13 175.3(3) . . . . ?
C11 C12 C13 C14 2.6(4) . . . . ?
C12 C13 C14 C15 0.2(4) . . . . ?
C12 C13 C14 C17 -179.7(3) . . . . ?
C13 C14 C15 C16 -1.9(4) . . . . ?
C17 C14 C15 C16 178.0(3) . . . . ?
C14 C15 C16 C11 0.7(4) . . . . ?
C12 C11 C16 C15 2.1(4) . . . . ?
C1 C11 C16 C15 -177.0(3) . . . . ?
C15 C14 C17 C18 175.6(3) . . . . ?
C13 C14 C17 C18 -4.5(4) . . . . ?
C15 C14 C17 C20 -60.8(4) . . . . ?
C13 C14 C17 C20 119.1(4) . . . . ?
C15 C14 C17 C19 56.2(4) . . . . ?
C13 C14 C17 C19 -123.9(3) . . . . ?
C1 C2 C21 C26 -120.9(3) . . . . ?
B41 C2 C21 C26 61.3(4) . . . . ?
C1 C2 C21 C22 57.2(4) . . . . ?
B41 C2 C21 C22 -120.6(3) . . . . ?
C26 C21 C22 C23 1.6(4) . . . . ?
C2 C21 C22 C23 -176.5(3) . . . . ?
C21 C22 C23 C24 1.1(5) . . . . ?
C22 C23 C24 C25 -2.4(5) . . . . ?
C22 C23 C24 C27 177.0(3) . . . . ?
C23 C24 C25 C26 0.9(4) . . . . ?
C27 C24 C25 C26 -178.5(3) . . . . ?
C22 C21 C26 C25 -3.0(4) . . . . ?
C2 C21 C26 C25 175.1(3) . . . . ?
C24 C25 C26 C21 1.8(5) . . . . ?
C23 C24 C27 C28' 59.8(6) . . . . ?
C25 C24 C27 C28' -120.9(6) . . . . ?
C23 C24 C27 C30 -115.1(6) . . . . ?
C25 C24 C27 C30 64.3(7) . . . . ?
C23 C24 C27 C29 119.4(6) . . . . ?
C25 C24 C27 C29 -61.2(6) . . . . ?
C23 C24 C27 C30' -64.5(6) . . . . ?
C25 C24 C27 C30' 114.8(6) . . . . ?
C23 C24 C27 C29' 178.6(5) . . . . ?
C25 C24 C27 C29' -2.0(6) . . . . ?
C23 C24 C27 C28 2.3(6) . . . . ?
C25 C24 C27 C28 -178.3(5) . . . . ?
C2 C1 B31 O35 -24.1(5) . . . . ?
C11 C1 B31 O35 151.4(3) . . . . ?
C2 C1 B31 O32 155.2(3) . . . . ?
C11 C1 B31 O32 -29.3(5) . . . . ?
O35 B31 O32 C33 15.2(5) . . . . ?
C1 B31 O32 C33 -164.2(4) . . . . ?
O35 B31 O32 C33' -16.3(5) . . . . ?
C1 B31 O32 C33' 164.4(5) . . . . ?
B31 O32 C33 C36 -156.2(5) . . . . ?
B31 O32 C33 C37 95.0(6) . . . . ?
B31 O32 C33 C34 -27.0(4) . . . . ?
B31 O32 C33' C34 22.1(6) . . . . ?
B31 O32 C33' C36 168.1(6) . . . . ?
B31 O32 C33' C37' -95.9(8) . . . . ?
C36 C33' C34 O35 -155.0(6) . . . . ?
C37' C33' C34 O35 104.8(7) . . . . ?
O32 C33' C34 O35 -19.4(6) . . . . ?
C36 C33' C34 C39' 77.7(15) . . . . ?
C37' C33' C34 C39' -22.5(14) . . . . ?
O32 C33' C34 C39' -146.7(13) . . . . ?
C36 C33' C34 C38' -47.5(11) . . . . ?
C37' C33' C34 C38' -147.7(10) . . . . ?
O32 C33' C34 C38' 88.1(10) . . . . ?
C36 C33 C34 C38 -87.1(9) . . . . ?
O32 C33 C34 C38 152.4(8) . . . . ?
C37 C33 C34 C38 35.5(9) . . . . ?
C36 C33 C34 O35 149.1(4) . . . . ?
O32 C33 C34 O35 28.7(4) . . . . ?
C37 C33 C34 O35 -88.3(5) . . . . ?
C36 C33 C34 C39 41.5(6) . . . . ?
O32 C33 C34 C39 -79.0(5) . . . . ?
C37 C33 C34 C39 164.1(5) . . . . ?
O32 B31 O35 C34 4.6(5) . . . . ?
C1 B31 O35 C34 -176.1(3) . . . . ?
C33' C34 O35 B31 9.7(5) . . . . ?
C38 C34 O35 B31 -143.7(11) . . . . ?
C39' C34 O35 B31 150.4(12) . . . . ?
C33 C34 O35 B31 -21.2(4) . . . . ?
C39 C34 O35 B31 93.0(6) . . . . ?
C38' C34 O35 B31 -111.3(10) . . . . ?
C1 C2 B41 O45 117.6(4) . . . . ?
C21 C2 B41 O45 -64.7(4) . . . . ?
C1 C2 B41 O42 -68.0(4) . . . . ?
C21 C2 B41 O42 109.6(3) . . . . ?
O45 B41 O42 C43 8.0(4) . . . . ?
C2 B41 O42 C43 -166.7(3) . . . . ?
B41 O42 C43 C46 -142.9(3) . . . . ?
B41 O42 C43 C47 98.7(3) . . . . ?
B41 O42 C43 C44 -20.8(3) . . . . ?
O42 C43 C44 O45 25.4(3) . . . . ?
C46 C43 C44 O45 143.0(3) . . . . ?
C47 C43 C44 O45 -88.7(3) . . . . ?
O42 C43 C44 C48 143.2(3) . . . . ?
C46 C43 C44 C48 -99.2(4) . . . . ?
C47 C43 C44 C48 29.0(4) . . . . ?
O42 C43 C44 C49 -88.9(3) . . . . ?
C46 C43 C44 C49 28.7(4) . . . . ?
C47 C43 C44 C49 157.0(3) . . . . ?
O42 B41 O45 C44 9.6(4) . . . . ?
C2 B41 O45 C44 -175.6(3) . . . . ?
C48 C44 O45 B41 -143.4(3) . . . . ?
C49 C44 O45 B41 98.0(3) . . . . ?
C43 C44 O45 B41 -21.7(3) . . . . ?

_refine_diff_density_max         0.382
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.054

####################################################################### 
# 
# 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_wa2058
_database_code_depnum_ccdc_archive 'CCDC 1883330'
_audit_update_record             
;
2018-12-05 deposited with the CCDC.
2018-12-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H50 B2 Li2 O2'
_chemical_formula_sum            'C30 H50 B2 Li2 O2'
_chemical_formula_weight         478.20

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'
Li Li -0.0003 0.0001 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   35.713(3)
_cell_length_b                   8.9897(8)
_cell_length_c                   19.7599(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6343.9(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    11322
_cell_measurement_theta_min      1.8
_cell_measurement_theta_max      25.1

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.001
_exptl_crystal_F_000             2096
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    0.058
_shelx_estimated_absorpt_T_min   0.987
_shelx_estimated_absorpt_T_max   0.996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.633
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31552
_diffrn_reflns_av_unetI/netI     0.1403
_diffrn_reflns_av_R_equivalents  0.1540
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.061
_diffrn_reflns_theta_max         25.360
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5780
_reflns_number_gt                2112
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  SHELXL97
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0634P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5780
_refine_ls_number_parameters     349
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2007
_refine_ls_R_factor_gt           0.0703
_refine_ls_wR_factor_ref         0.1841
_refine_ls_wR_factor_gt          0.1408
_refine_ls_goodness_of_fit_ref   0.872
_refine_ls_restrained_S_all      0.872
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Li1 Li 0.27000(17) 0.5491(7) 0.6737(3) 0.0424(16) Uani 1 1 d . . . . .
Li2 Li 0.22353(18) 0.4048(7) 0.7990(3) 0.0468(17) Uani 1 1 d . . . . .
O1 O 0.30605(7) 0.4807(3) 0.60526(14) 0.0562(8) Uani 1 1 d . . . . .
O2 O 0.17990(7) 0.4717(3) 0.85185(13) 0.0521(7) Uani 1 1 d . . . . .
B1 B 0.26801(13) 0.8213(5) 0.6771(2) 0.0385(11) Uani 1 1 d . . . . .
H1A H 0.2741(9) 0.927(4) 0.6459(16) 0.044(10) Uiso 1 1 d . . . . .
H1B H 0.2438(10) 0.858(4) 0.7170(18) 0.060(11) Uiso 1 1 d . . . . .
H1C H 0.2548(8) 0.742(4) 0.6435(15) 0.028(8) Uiso 1 1 d . . . . .
B2 B 0.26344(13) 0.6277(6) 0.8043(2) 0.0405(11) Uani 1 1 d . . . . .
H2A H 0.2636(8) 0.521(4) 0.8376(15) 0.036(9) Uiso 1 1 d . . . . .
H2B H 0.2403(9) 0.606(4) 0.7634(16) 0.041(10) Uiso 1 1 d . . . . .
H2C H 0.2537(8) 0.724(4) 0.8403(15) 0.034(9) Uiso 1 1 d . . . . .
C1 C 0.30584(10) 0.7541(4) 0.71160(18) 0.0384(9) Uani 1 1 d . . . . .
C2 C 0.30339(11) 0.6637(4) 0.76918(18) 0.0377(9) Uani 1 1 d . . . . .
C11 C 0.34275(10) 0.7950(4) 0.68489(19) 0.0392(9) Uani 1 1 d . . . . .
C12 C 0.37603(10) 0.7492(4) 0.71671(19) 0.0403(10) Uani 1 1 d . . . . .
C13 C 0.41028(11) 0.8071(5) 0.6942(2) 0.0478(11) Uani 1 1 d . . . . .
H13 H 0.4325 0.7791 0.7175 0.057 Uiso 1 1 calc R U . . .
C14 C 0.41332(11) 0.9032(5) 0.6396(2) 0.0465(10) Uani 1 1 d . . . . .
C15 C 0.38035(11) 0.9366(5) 0.6058(2) 0.0538(11) Uani 1 1 d . . . . .
H15 H 0.3815 0.9980 0.5667 0.065 Uiso 1 1 calc R U . . .
C16 C 0.34636(11) 0.8848(5) 0.62654(19) 0.0484(11) Uani 1 1 d . . . . .
H16 H 0.3246 0.9096 0.6012 0.058 Uiso 1 1 calc R U . . .
C17 C 0.45098(11) 0.9742(5) 0.6228(2) 0.0525(11) Uani 1 1 d . . . . .
C18 C 0.45017(13) 1.0639(6) 0.5568(2) 0.0748(15) Uani 1 1 d . . . . .
H18A H 0.4306 1.1400 0.5595 0.112 Uiso 1 1 calc R U . . .
H18B H 0.4745 1.1119 0.5499 0.112 Uiso 1 1 calc R U . . .
H18C H 0.4449 0.9971 0.5188 0.112 Uiso 1 1 calc R U . . .
C19 C 0.46094(15) 1.0855(7) 0.6792(2) 0.0895(18) Uani 1 1 d . . . . .
H19A H 0.4413 1.1611 0.6825 0.134 Uiso 1 1 calc R U . . .
H19B H 0.4630 1.0326 0.7224 0.134 Uiso 1 1 calc R U . . .
H19C H 0.4849 1.1335 0.6687 0.134 Uiso 1 1 calc R U . . .
C20 C 0.48149(13) 0.8568(6) 0.6177(3) 0.102(2) Uani 1 1 d . . . . .
H20A H 0.5054 0.9047 0.6069 0.153 Uiso 1 1 calc R U . . .
H20B H 0.4837 0.8042 0.6610 0.153 Uiso 1 1 calc R U . . .
H20C H 0.4751 0.7857 0.5819 0.153 Uiso 1 1 calc R U . . .
C21 C 0.33835(11) 0.6089(4) 0.79931(17) 0.0382(9) Uani 1 1 d . . . . .
C22 C 0.37389(10) 0.6474(4) 0.77424(18) 0.0361(9) Uani 1 1 d . . . . .
C23 C 0.40632(11) 0.5866(4) 0.8036(2) 0.0456(10) Uani 1 1 d . . . . .
H23 H 0.4299 0.6088 0.7838 0.055 Uiso 1 1 calc R U . . .
C24 C 0.40542(10) 0.4958(5) 0.8602(2) 0.0457(10) Uani 1 1 d . . . . .
C25 C 0.37024(11) 0.4658(4) 0.88683(19) 0.0456(10) Uani 1 1 d . . . . .
H25 H 0.3685 0.4072 0.9267 0.055 Uiso 1 1 calc R U . . .
C26 C 0.33788(10) 0.5174(4) 0.85773(18) 0.0402(9) Uani 1 1 d . . . . .
H26 H 0.3145 0.4912 0.8773 0.048 Uiso 1 1 calc R U . . .
C27 C 0.44111(11) 0.4360(5) 0.8930(2) 0.0584(12) Uani 1 1 d . . . . .
C28 C 0.43690(14) 0.2666(6) 0.9029(3) 0.105(2) Uani 1 1 d . . . . .
H28A H 0.4147 0.2463 0.9305 0.157 Uiso 1 1 calc R U . . .
H28B H 0.4342 0.2182 0.8587 0.157 Uiso 1 1 calc R U . . .
H28C H 0.4592 0.2275 0.9259 0.157 Uiso 1 1 calc R U . . .
C29 C 0.47575(11) 0.4580(6) 0.8502(3) 0.0783(15) Uani 1 1 d . . . . .
H29A H 0.4723 0.4088 0.8064 0.117 Uiso 1 1 calc R U . . .
H29B H 0.4800 0.5645 0.8431 0.117 Uiso 1 1 calc R U . . .
H29C H 0.4974 0.4148 0.8735 0.117 Uiso 1 1 calc R U . . .
C30 C 0.44652(15) 0.5121(9) 0.9606(3) 0.122(3) Uani 1 1 d . . . . .
H30A H 0.4241 0.4980 0.9884 0.184 Uiso 1 1 calc R U . . .
H30B H 0.4682 0.4689 0.9837 0.184 Uiso 1 1 calc R U . . .
H30C H 0.4507 0.6186 0.9534 0.184 Uiso 1 1 calc R U . . .
C31 C 0.33454(14) 0.3848(6) 0.6337(3) 0.0816(16) Uani 1 1 d . . . . .
H31A H 0.3280 0.2803 0.6232 0.098 Uiso 1 1 calc R U . . .
H31B H 0.3343 0.3959 0.6835 0.098 Uiso 1 1 calc R U . . .
C32 C 0.37254(15) 0.4140(7) 0.6093(3) 0.113(2) Uani 1 1 d . . . . .
H32A H 0.3900 0.3446 0.6310 0.170 Uiso 1 1 calc R U . . .
H32B H 0.3734 0.4005 0.5602 0.170 Uiso 1 1 calc R U . . .
H32C H 0.3796 0.5163 0.6206 0.170 Uiso 1 1 calc R U . . .
C33 C 0.29719(16) 0.4419(7) 0.5380(2) 0.0887(18) Uani 1 1 d . . . . .
H33A H 0.2843 0.3445 0.5370 0.106 Uiso 1 1 calc R U . . .
H33B H 0.3204 0.4340 0.5108 0.106 Uiso 1 1 calc R U . . .
C34 C 0.27265(18) 0.5580(9) 0.5097(2) 0.144(3) Uani 1 1 d . . . . .
H34A H 0.2662 0.5327 0.4629 0.216 Uiso 1 1 calc R U . . .
H34B H 0.2497 0.5647 0.5367 0.216 Uiso 1 1 calc R U . . .
H34C H 0.2857 0.6539 0.5106 0.216 Uiso 1 1 calc R U . . .
C41 C 0.16489(14) 0.6170(5) 0.8455(3) 0.0740(14) Uani 1 1 d . . . . .
H41A H 0.1850 0.6912 0.8519 0.089 Uiso 1 1 calc R U . . .
H41B H 0.1457 0.6333 0.8809 0.089 Uiso 1 1 calc R U . . .
C42 C 0.14796(18) 0.6366(6) 0.7788(3) 0.098(2) Uani 1 1 d . . . . .
H42A H 0.1377 0.7374 0.7751 0.146 Uiso 1 1 calc R U . . .
H42B H 0.1670 0.6217 0.7437 0.146 Uiso 1 1 calc R U . . .
H42C H 0.1278 0.5639 0.7727 0.146 Uiso 1 1 calc R U . . .
C43 C 0.17592(13) 0.4094(6) 0.9200(2) 0.0665(13) Uani 1 1 d . . . . .
H43A H 0.1842 0.4836 0.9538 0.080 Uiso 1 1 calc R U . . .
H43B H 0.1921 0.3205 0.9244 0.080 Uiso 1 1 calc R U . . .
C44 C 0.13594(16) 0.3670(6) 0.9338(3) 0.0916(18) Uani 1 1 d . . . . .
H44A H 0.1339 0.3257 0.9795 0.137 Uiso 1 1 calc R U . . .
H44B H 0.1200 0.4554 0.9301 0.137 Uiso 1 1 calc R U . . .
H44C H 0.1278 0.2924 0.9007 0.137 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Li1 O1 1.966(7) . ?
Li1 C1 2.365(7) . ?
Li1 B1 2.449(8) . ?
Li1 B1 2.457(8) 8_655 ?
Li1 C2 2.458(7) . ?
Li1 B2 2.686(8) . ?
Li1 Li2 3.250(9) . ?
Li1 H1C 1.91(3) . ?
Li1 H2B 2.13(3) . ?
Li2 O2 1.970(7) . ?
Li2 C1 2.432(8) 8_655 ?
Li2 C2 2.443(7) 8_655 ?
Li2 B2 2.461(8) . ?
Li2 B2 2.537(8) 8_655 ?
Li2 B1 2.540(8) 8_655 ?
Li2 H2A 1.93(3) . ?
Li2 H2B 2.03(3) . ?
O1 C33 1.410(5) . ?
O1 C31 1.447(5) . ?
O2 C41 1.417(5) . ?
O2 C43 1.465(5) . ?
B1 C1 1.629(6) . ?
B1 Li1 2.457(8) 8_665 ?
B1 Li2 2.540(8) 8_665 ?
B1 H1A 1.15(3) . ?
B1 H1B 1.22(4) . ?
B1 H1C 1.08(3) . ?
B2 C2 1.619(6) . ?
B2 Li2 2.537(8) 8_665 ?
B2 H2A 1.16(3) . ?
B2 H2B 1.17(3) . ?
B2 H2C 1.17(3) . ?
C1 C2 1.401(5) . ?
C1 C11 1.467(5) . ?
C1 Li2 2.432(8) 8_665 ?
C2 C21 1.468(5) . ?
C2 Li2 2.443(7) 8_665 ?
C11 C12 1.406(5) . ?
C11 C16 1.413(5) . ?
C12 C13 1.402(5) . ?
C12 C22 1.461(5) . ?
C13 C14 1.386(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.387(5) . ?
C14 C17 1.525(5) . ?
C15 C16 1.363(5) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C20 1.520(6) . ?
C17 C18 1.533(6) . ?
C17 C19 1.540(6) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
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 C22 1.406(5) . ?
C21 C26 1.417(5) . ?
C22 C23 1.407(5) . ?
C23 C24 1.384(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.389(5) . ?
C24 C27 1.528(5) . ?
C25 C26 1.372(5) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C29 1.511(6) . ?
C27 C30 1.513(7) . ?
C27 C28 1.543(6) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.463(7) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.474(7) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C41 C42 1.461(6) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C44 1.503(7) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 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 Li1 C1 96.1(3) . . ?
O1 Li1 B1 110.5(3) . . ?
C1 Li1 B1 39.51(17) . . ?
O1 Li1 B1 96.9(3) . 8_655 ?
C1 Li1 B1 160.0(3) . 8_655 ?
B1 Li1 B1 144.7(3) . 8_655 ?
O1 Li1 C2 110.0(3) . . ?
C1 Li1 C2 33.70(15) . . ?
B1 Li1 C2 64.8(2) . . ?
B1 Li1 C2 126.6(3) 8_655 . ?
O1 Li1 B2 143.2(3) . . ?
C1 Li1 B2 62.5(2) . . ?
B1 Li1 B2 73.0(2) . . ?
B1 Li1 B2 98.3(3) 8_655 . ?
C2 Li1 B2 36.36(16) . . ?
O1 Li1 Li2 137.2(3) . . ?
C1 Li1 Li2 110.3(3) . . ?
B1 Li1 Li2 111.3(3) . . ?
B1 Li1 Li2 50.54(19) 8_655 . ?
C2 Li1 Li2 80.3(2) . . ?
B2 Li1 Li2 47.84(18) . . ?
O1 Li1 H1C 104.7(9) . . ?
C1 Li1 H1C 63.0(10) . . ?
B1 Li1 H1C 25.1(9) . . ?
B1 Li1 H1C 127.4(9) 8_655 . ?
C2 Li1 H1C 89.8(10) . . ?
B2 Li1 H1C 92.1(9) . . ?
Li2 Li1 H1C 117.1(9) . . ?
O1 Li1 H2B 167.1(10) . . ?
C1 Li1 H2B 79.5(9) . . ?
B1 Li1 H2B 73.8(9) . . ?
B1 Li1 H2B 84.5(9) 8_655 . ?
C2 Li1 H2B 60.1(9) . . ?
B2 Li1 H2B 24.9(9) . . ?
Li2 Li1 H2B 37.7(9) . . ?
H1C Li1 H2B 84.2(13) . . ?
O2 Li2 C1 101.9(3) . 8_655 ?
O2 Li2 C2 95.0(3) . 8_655 ?
C1 Li2 C2 33.40(15) 8_655 8_655 ?
O2 Li2 B2 100.8(3) . . ?
C1 Li2 B2 137.2(3) 8_655 . ?
C2 Li2 B2 163.8(3) 8_655 . ?
O2 Li2 B2 115.0(3) . 8_655 ?
C1 Li2 B2 64.0(2) 8_655 8_655 ?
C2 Li2 B2 37.90(17) 8_655 8_655 ?
B2 Li2 B2 133.7(3) . 8_655 ?
O2 Li2 B1 133.4(3) . 8_655 ?
C1 Li2 B1 38.19(16) 8_655 8_655 ?
C2 Li2 B1 63.7(2) 8_655 8_655 ?
B2 Li2 B1 102.3(3) . 8_655 ?
B2 Li2 B1 74.2(2) 8_655 8_655 ?
O2 Li2 Li1 133.3(3) . . ?
C1 Li2 Li1 84.4(2) 8_655 . ?
C2 Li2 Li1 111.8(3) 8_655 . ?
B2 Li2 Li1 54.0(2) . . ?
B2 Li2 Li1 109.3(3) 8_655 . ?
B1 Li2 Li1 48.34(18) 8_655 . ?
O2 Li2 H2A 102.2(9) . . ?
C1 Li2 H2A 154.5(9) 8_655 . ?
C2 Li2 H2A 150.2(11) 8_655 . ?
B2 Li2 H2A 27.4(10) . . ?
B2 Li2 H2A 112.3(10) 8_655 . ?
B1 Li2 H2A 116.5(9) 8_655 . ?
Li1 Li2 H2A 72.9(9) . . ?
O2 Li2 H2B 98.3(9) . . ?
C1 Li2 H2B 112.2(10) 8_655 . ?
C2 Li2 H2B 145.4(10) 8_655 . ?
B2 Li2 H2B 28.2(9) . . ?
B2 Li2 H2B 146.6(9) 8_655 . ?
B1 Li2 H2B 84.3(9) 8_655 . ?
Li1 Li2 H2B 39.7(9) . . ?
H2A Li2 H2B 55.6(13) . . ?
C33 O1 C31 112.1(4) . . ?
C33 O1 Li1 125.4(3) . . ?
C31 O1 Li1 112.3(3) . . ?
C41 O2 C43 113.4(3) . . ?
C41 O2 Li2 122.2(3) . . ?
C43 O2 Li2 116.6(3) . . ?
C1 B1 Li1 67.5(3) . . ?
C1 B1 Li1 141.1(3) . 8_665 ?
Li1 B1 Li1 148.0(2) . 8_665 ?
C1 B1 Li2 67.3(2) . 8_665 ?
Li1 B1 Li2 108.5(3) . 8_665 ?
Li1 B1 Li2 81.1(2) 8_665 8_665 ?
C1 B1 H1A 111.9(16) . . ?
Li1 B1 H1A 143.4(16) . . ?
Li1 B1 H1A 53.4(16) 8_665 . ?
Li2 B1 H1A 104.0(16) 8_665 . ?
C1 B1 H1B 114.8(17) . . ?
Li1 B1 H1B 108.1(18) . . ?
Li1 B1 H1B 53.0(18) 8_665 . ?
Li2 B1 H1B 52.4(17) 8_665 . ?
H1A B1 H1B 105(2) . . ?
C1 B1 H1C 111.8(16) . . ?
Li1 B1 H1C 48.4(16) . . ?
Li1 B1 H1C 107.1(16) 8_665 . ?
Li2 B1 H1C 145.9(15) 8_665 . ?
H1A B1 H1C 107(2) . . ?
H1B B1 H1C 106(2) . . ?
C2 B2 Li2 130.9(3) . . ?
C2 B2 Li2 67.9(3) . 8_665 ?
Li2 B2 Li2 154.7(2) . 8_665 ?
C2 B2 Li1 64.1(2) . . ?
Li2 B2 Li1 78.2(2) . . ?
Li2 B2 Li1 101.7(3) 8_665 . ?
C2 B2 H2A 113.8(15) . . ?
Li2 B2 H2A 50.0(15) . . ?
Li2 B2 H2A 146.2(15) 8_665 . ?
Li1 B2 H2A 109.1(15) . . ?
C2 B2 H2B 110.9(15) . . ?
Li2 B2 H2B 55.2(16) . . ?
Li2 B2 H2B 105.1(17) 8_665 . ?
Li1 B2 H2B 49.8(15) . . ?
H2A B2 H2B 105(2) . . ?
C2 B2 H2C 112.0(15) . . ?
Li2 B2 H2C 117.0(15) . . ?
Li2 B2 H2C 49.9(15) 8_665 . ?
Li1 B2 H2C 143.4(15) . . ?
H2A B2 H2C 105(2) . . ?
H2B B2 H2C 109(2) . . ?
C2 C1 C11 119.6(3) . . ?
C2 C1 B1 120.2(4) . . ?
C11 C1 B1 120.1(3) . . ?
C2 C1 Li1 76.8(3) . . ?
C11 C1 Li1 124.6(3) . . ?
B1 C1 Li1 73.0(3) . . ?
C2 C1 Li2 73.7(3) . 8_665 ?
C11 C1 Li2 120.2(3) . 8_665 ?
B1 C1 Li2 74.5(3) . 8_665 ?
Li1 C1 Li2 115.2(3) . 8_665 ?
C1 C2 C21 118.1(4) . . ?
C1 C2 B2 121.3(4) . . ?
C21 C2 B2 120.5(3) . . ?
C1 C2 Li2 72.9(3) . 8_665 ?
C21 C2 Li2 122.3(3) . 8_665 ?
B2 C2 Li2 74.2(3) . 8_665 ?
C1 C2 Li1 69.5(3) . . ?
C21 C2 Li1 125.7(3) . . ?
B2 C2 Li1 79.5(3) . . ?
Li2 C2 Li1 111.5(3) 8_665 . ?
C12 C11 C16 117.1(4) . . ?
C12 C11 C1 121.7(3) . . ?
C16 C11 C1 121.2(4) . . ?
C13 C12 C11 119.1(4) . . ?
C13 C12 C22 121.7(4) . . ?
C11 C12 C22 119.1(4) . . ?
C14 C13 C12 123.1(4) . . ?
C14 C13 H13 118.4 . . ?
C12 C13 H13 118.4 . . ?
C13 C14 C15 116.3(4) . . ?
C13 C14 C17 120.0(4) . . ?
C15 C14 C17 123.6(4) . . ?
C16 C15 C14 122.5(4) . . ?
C16 C15 H15 118.8 . . ?
C14 C15 H15 118.8 . . ?
C15 C16 C11 121.5(4) . . ?
C15 C16 H16 119.3 . . ?
C11 C16 H16 119.3 . . ?
C20 C17 C14 110.8(4) . . ?
C20 C17 C18 108.8(4) . . ?
C14 C17 C18 112.9(3) . . ?
C20 C17 C19 109.5(4) . . ?
C14 C17 C19 108.5(3) . . ?
C18 C17 C19 106.2(4) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C26 116.1(3) . . ?
C22 C21 C2 122.8(3) . . ?
C26 C21 C2 121.0(3) . . ?
C21 C22 C23 120.1(4) . . ?
C21 C22 C12 118.4(3) . . ?
C23 C22 C12 121.4(4) . . ?
C24 C23 C22 122.9(4) . . ?
C24 C23 H23 118.5 . . ?
C22 C23 H23 118.5 . . ?
C23 C24 C25 116.2(4) . . ?
C23 C24 C27 122.1(4) . . ?
C25 C24 C27 121.7(4) . . ?
C26 C25 C24 122.5(4) . . ?
C26 C25 H25 118.8 . . ?
C24 C25 H25 118.8 . . ?
C25 C26 C21 121.9(4) . . ?
C25 C26 H26 119.1 . . ?
C21 C26 H26 119.1 . . ?
C29 C27 C30 109.2(4) . . ?
C29 C27 C24 113.6(4) . . ?
C30 C27 C24 108.8(4) . . ?
C29 C27 C28 106.3(4) . . ?
C30 C27 C28 110.3(5) . . ?
C24 C27 C28 108.7(4) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O1 C31 C32 114.7(5) . . ?
O1 C31 H31A 108.6 . . ?
C32 C31 H31A 108.6 . . ?
O1 C31 H31B 108.6 . . ?
C32 C31 H31B 108.6 . . ?
H31A C31 H31B 107.6 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O1 C33 C34 108.4(5) . . ?
O1 C33 H33A 110.0 . . ?
C34 C33 H33A 110.0 . . ?
O1 C33 H33B 110.0 . . ?
C34 C33 H33B 110.0 . . ?
H33A C33 H33B 108.4 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O2 C41 C42 110.4(4) . . ?
O2 C41 H41A 109.6 . . ?
C42 C41 H41A 109.6 . . ?
O2 C41 H41B 109.6 . . ?
C42 C41 H41B 109.6 . . ?
H41A C41 H41B 108.1 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O2 C43 C44 110.8(4) . . ?
O2 C43 H43A 109.5 . . ?
C44 C43 H43A 109.5 . . ?
O2 C43 H43B 109.5 . . ?
C44 C43 H43B 109.5 . . ?
H43A C43 H43B 108.1 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Li1 B1 C1 C2 -63.0(3) . . . . ?
Li1 B1 C1 C2 98.4(6) 8_665 . . . ?
Li2 B1 C1 C2 60.1(3) 8_665 . . . ?
Li1 B1 C1 C11 120.6(4) . . . . ?
Li1 B1 C1 C11 -78.0(6) 8_665 . . . ?
Li2 B1 C1 C11 -116.3(4) 8_665 . . . ?
Li1 B1 C1 Li1 161.4(6) 8_665 . . . ?
Li2 B1 C1 Li1 123.1(3) 8_665 . . . ?
Li1 B1 C1 Li2 -123.1(3) . . . 8_665 ?
Li1 B1 C1 Li2 38.3(5) 8_665 . . 8_665 ?
C11 C1 C2 C21 -2.1(5) . . . . ?
B1 C1 C2 C21 -178.5(3) . . . . ?
Li1 C1 C2 C21 120.4(3) . . . . ?
Li2 C1 C2 C21 -118.0(3) 8_665 . . . ?
C11 C1 C2 B2 174.5(3) . . . . ?
B1 C1 C2 B2 -1.9(5) . . . . ?
Li1 C1 C2 B2 -63.0(4) . . . . ?
Li2 C1 C2 B2 58.6(3) 8_665 . . . ?
C11 C1 C2 Li2 115.9(4) . . . 8_665 ?
B1 C1 C2 Li2 -60.5(4) . . . 8_665 ?
Li1 C1 C2 Li2 -121.6(2) . . . 8_665 ?
C11 C1 C2 Li1 -122.5(4) . . . . ?
B1 C1 C2 Li1 61.1(3) . . . . ?
Li2 C1 C2 Li1 121.6(2) 8_665 . . . ?
Li2 B2 C2 C1 101.9(5) . . . . ?
Li2 B2 C2 C1 -58.0(3) 8_665 . . . ?
Li1 B2 C2 C1 58.1(3) . . . . ?
Li2 B2 C2 C21 -81.5(5) . . . . ?
Li2 B2 C2 C21 118.6(4) 8_665 . . . ?
Li1 B2 C2 C21 -125.4(4) . . . . ?
Li2 B2 C2 Li2 159.9(5) . . . 8_665 ?
Li1 B2 C2 Li2 116.1(3) . . . 8_665 ?
Li2 B2 C2 Li1 43.8(4) . . . . ?
Li2 B2 C2 Li1 -116.1(3) 8_665 . . . ?
C2 C1 C11 C12 -1.8(5) . . . . ?
B1 C1 C11 C12 174.6(4) . . . . ?
Li1 C1 C11 C12 -95.9(4) . . . . ?
Li2 C1 C11 C12 85.8(4) 8_665 . . . ?
C2 C1 C11 C16 179.4(3) . . . . ?
B1 C1 C11 C16 -4.2(5) . . . . ?
Li1 C1 C11 C16 85.3(5) . . . . ?
Li2 C1 C11 C16 -93.0(4) 8_665 . . . ?
C16 C11 C12 C13 7.0(5) . . . . ?
C1 C11 C12 C13 -171.9(4) . . . . ?
C16 C11 C12 C22 -175.6(3) . . . . ?
C1 C11 C12 C22 5.6(5) . . . . ?
C11 C12 C13 C14 -3.0(6) . . . . ?
C22 C12 C13 C14 179.6(4) . . . . ?
C12 C13 C14 C15 -2.2(6) . . . . ?
C12 C13 C14 C17 173.5(4) . . . . ?
C13 C14 C15 C16 3.2(6) . . . . ?
C17 C14 C15 C16 -172.3(4) . . . . ?
C14 C15 C16 C11 1.0(6) . . . . ?
C12 C11 C16 C15 -6.1(6) . . . . ?
C1 C11 C16 C15 172.7(4) . . . . ?
C13 C14 C17 C20 51.7(5) . . . . ?
C15 C14 C17 C20 -133.0(5) . . . . ?
C13 C14 C17 C18 174.0(4) . . . . ?
C15 C14 C17 C18 -10.6(6) . . . . ?
C13 C14 C17 C19 -68.6(5) . . . . ?
C15 C14 C17 C19 106.8(5) . . . . ?
C1 C2 C21 C22 2.2(5) . . . . ?
B2 C2 C21 C22 -174.4(4) . . . . ?
Li2 C2 C21 C22 -84.5(4) 8_665 . . . ?
Li1 C2 C21 C22 86.2(4) . . . . ?
C1 C2 C21 C26 179.8(3) . . . . ?
B2 C2 C21 C26 3.1(5) . . . . ?
Li2 C2 C21 C26 93.1(4) 8_665 . . . ?
Li1 C2 C21 C26 -96.3(4) . . . . ?
C26 C21 C22 C23 4.9(5) . . . . ?
C2 C21 C22 C23 -177.5(4) . . . . ?
C26 C21 C22 C12 -176.2(3) . . . . ?
C2 C21 C22 C12 1.5(5) . . . . ?
C13 C12 C22 C21 172.0(4) . . . . ?
C11 C12 C22 C21 -5.3(5) . . . . ?
C13 C12 C22 C23 -9.0(6) . . . . ?
C11 C12 C22 C23 173.6(4) . . . . ?
C21 C22 C23 C24 -4.4(6) . . . . ?
C12 C22 C23 C24 176.7(4) . . . . ?
C22 C23 C24 C25 0.5(6) . . . . ?
C22 C23 C24 C27 -177.5(4) . . . . ?
C23 C24 C25 C26 2.6(6) . . . . ?
C27 C24 C25 C26 -179.4(4) . . . . ?
C24 C25 C26 C21 -1.8(6) . . . . ?
C22 C21 C26 C25 -2.0(5) . . . . ?
C2 C21 C26 C25 -179.7(4) . . . . ?
C23 C24 C27 C29 -12.1(6) . . . . ?
C25 C24 C27 C29 170.0(4) . . . . ?
C23 C24 C27 C30 109.8(5) . . . . ?
C25 C24 C27 C30 -68.1(6) . . . . ?
C23 C24 C27 C28 -130.1(5) . . . . ?
C25 C24 C27 C28 52.0(6) . . . . ?
C33 O1 C31 C32 75.2(5) . . . . ?
Li1 O1 C31 C32 -137.4(4) . . . . ?
C31 O1 C33 C34 -171.3(5) . . . . ?
Li1 O1 C33 C34 46.5(6) . . . . ?
C43 O2 C41 C42 -144.1(4) . . . . ?
Li2 O2 C41 C42 67.8(6) . . . . ?
C41 O2 C43 C44 73.0(5) . . . . ?
Li2 O2 C43 C44 -137.0(4) . . . . ?

_refine_diff_density_max         0.195
_refine_diff_density_min         -0.195
_refine_diff_density_rms         0.038

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_wa1986
_database_code_depnum_ccdc_archive 'CCDC 1883333'
_audit_update_record             
;
2018-12-05 deposited with the CCDC.
2018-12-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H24 Br2'
_chemical_formula_sum            'C22 H24 Br2'
_chemical_formula_weight         448.23

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.9767(3)
_cell_length_b                   18.5254(7)
_cell_length_c                   29.8956(10)
_cell_angle_alpha                90
_cell_angle_beta                 92.319(3)
_cell_angle_gamma                90
_cell_volume                     6074.2(3)
_cell_formula_units_Z            12
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    52697
_cell_measurement_theta_min      1.3
_cell_measurement_theta_max      27.7

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_F_000             2712
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    4.004
_shelx_estimated_absorpt_T_min   0.343
_shelx_estimated_absorpt_T_max   0.624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.489
_exptl_absorpt_correction_T_max  0.807
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            76173
_diffrn_reflns_av_unetI/netI     0.0791
_diffrn_reflns_av_R_equivalents  0.1444
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         1.293
_diffrn_reflns_theta_max         27.208
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             13403
_reflns_number_gt                9718
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  "S'SHELXL (Sheldrick, 2008)"
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  SHELXL97
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0812P)²+0.4530P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0035(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         13403
_refine_ls_number_parameters     650
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0619
_refine_ls_wR_factor_ref         0.1617
_refine_ls_wR_factor_gt          0.1446
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.70465(4) 0.51117(3) 0.65500(2) 0.05603(14) Uani 1 1 d . . . . .
Br2 Br 0.70637(4) 0.33516(3) 0.66873(2) 0.05591(14) Uani 1 1 d . . . . .
C1 C 0.5574(4) 0.4590(2) 0.65823(15) 0.0465(9) Uani 1 1 d . . . . .
C2 C 0.5577(4) 0.3859(2) 0.66254(14) 0.0454(9) Uani 1 1 d . . . . .
C3 C 0.4460(4) 0.3454(2) 0.66127(14) 0.0425(9) Uani 1 1 d . . . . .
C4 C 0.4442(4) 0.2696(2) 0.65881(15) 0.0472(9) Uani 1 1 d . . . . .
H4A H 0.5188 0.2437 0.6581 0.057 Uiso 1 1 calc R U . . .
C5 C 0.3361(4) 0.2324(2) 0.65745(16) 0.0483(10) Uani 1 1 d . . . . .
H5A H 0.3373 0.1813 0.6548 0.058 Uiso 1 1 calc R U . . .
C6 C 0.2234(4) 0.2681(2) 0.65984(15) 0.0449(9) Uani 1 1 d . . . . .
C7 C 0.2255(4) 0.3423(2) 0.66254(15) 0.0439(9) Uani 1 1 d . . . . .
H7A H 0.1503 0.3673 0.6647 0.053 Uiso 1 1 calc R U . . .
C8 C 0.3337(3) 0.3829(2) 0.66231(13) 0.0401(8) Uani 1 1 d . . . . .
C9 C 0.3335(4) 0.4615(2) 0.66050(14) 0.0409(8) Uani 1 1 d . . . . .
C10 C 0.2237(4) 0.5021(2) 0.66056(14) 0.0439(9) Uani 1 1 d . . . . .
H10A H 0.1490 0.4772 0.6641 0.053 Uiso 1 1 calc R U . . .
C11 C 0.2209(4) 0.5760(2) 0.65572(15) 0.0440(9) Uani 1 1 d . . . . .
C12 C 0.3332(4) 0.6117(2) 0.65107(17) 0.0513(10) Uani 1 1 d . . . . .
H12A H 0.3339 0.6627 0.6476 0.062 Uiso 1 1 calc R U . . .
C13 C 0.4410(4) 0.5747(2) 0.65138(17) 0.0493(10) Uani 1 1 d . . . . .
H13A H 0.5150 0.6003 0.6480 0.059 Uiso 1 1 calc R U . . .
C14 C 0.4441(4) 0.4992(2) 0.65657(14) 0.0431(9) Uani 1 1 d . . . . .
C15 C 0.1051(4) 0.2245(2) 0.65805(17) 0.0506(10) Uani 1 1 d . . . . .
C16 C 0.1093(5) 0.1677(3) 0.6954(2) 0.0695(14) Uani 1 1 d . . . . .
H16A H 0.1809 0.1367 0.6924 0.104 Uiso 1 1 calc R U . . .
H16B H 0.1145 0.1919 0.7246 0.104 Uiso 1 1 calc R U . . .
H16C H 0.0352 0.1381 0.6932 0.104 Uiso 1 1 calc R U . . .
C17 C 0.0926(5) 0.1862(3) 0.6129(2) 0.0647(13) Uani 1 1 d . . . . .
H17A H 0.1642 0.1557 0.6088 0.097 Uiso 1 1 calc R U . . .
H17B H 0.0190 0.1563 0.6119 0.097 Uiso 1 1 calc R U . . .
H17C H 0.0866 0.2222 0.5889 0.097 Uiso 1 1 calc R U . . .
C18 C -0.0070(4) 0.2717(3) 0.6637(2) 0.0732(17) Uani 1 1 d . . . . .
H18A H 0.0000 0.2966 0.6926 0.110 Uiso 1 1 calc R U . . .
H18B H -0.0126 0.3075 0.6395 0.110 Uiso 1 1 calc R U . . .
H18C H -0.0803 0.2415 0.6626 0.110 Uiso 1 1 calc R U . . .
C19 C 0.1033(4) 0.6198(2) 0.65642(17) 0.0508(10) Uani 1 1 d . . . . .
C20 C -0.0099(4) 0.5717(3) 0.6533(3) 0.0744(17) Uani 1 1 d . . . . .
H20A H -0.0832 0.6018 0.6538 0.112 Uiso 1 1 calc R U . . .
H20B H -0.0105 0.5442 0.6253 0.112 Uiso 1 1 calc R U . . .
H20C H -0.0085 0.5383 0.6787 0.112 Uiso 1 1 calc R U . . .
C21 C 0.0963(5) 0.6727(3) 0.6169(2) 0.0632(13) Uani 1 1 d . . . . .
H21A H 0.0205 0.7005 0.6177 0.095 Uiso 1 1 calc R U . . .
H21B H 0.1661 0.7056 0.6191 0.095 Uiso 1 1 calc R U . . .
H21C H 0.0978 0.6457 0.5888 0.095 Uiso 1 1 calc R U . . .
C22 C 0.1032(5) 0.6612(3) 0.7009(2) 0.0701(14) Uani 1 1 d . . . . .
H22A H 0.0284 0.6899 0.7022 0.105 Uiso 1 1 calc R U . . .
H22B H 0.1071 0.6269 0.7259 0.105 Uiso 1 1 calc R U . . .
H22C H 0.1741 0.6934 0.7031 0.105 Uiso 1 1 calc R U . . .
Br1A Br 0.18664(5) 0.70949(4) 0.45044(2) 0.07284(18) Uani 1 1 d . . . . .
Br2A Br 0.14069(5) 0.82471(3) 0.53118(2) 0.06788(17) Uani 1 1 d . . . . .
C1A C 0.3054(4) 0.7223(3) 0.49733(16) 0.0535(10) Uani 1 1 d . . . . .
C2A C 0.2845(4) 0.7682(2) 0.53133(16) 0.0498(10) Uani 1 1 d . . . . .
C3A C 0.3703(4) 0.7750(2) 0.56885(15) 0.0463(9) Uani 1 1 d . . . . .
C4A C 0.3499(4) 0.8218(2) 0.60519(17) 0.0510(10) Uani 1 1 d . . . . .
H4AA H 0.2801 0.8522 0.6043 0.061 Uiso 1 1 calc R U . . .
C5A C 0.4296(4) 0.8238(2) 0.64165(17) 0.0534(11) Uani 1 1 d . . . . .
H5AA H 0.4123 0.8542 0.6662 0.064 Uiso 1 1 calc R U . . .
C6A C 0.5369(4) 0.7817(2) 0.64371(15) 0.0469(9) Uani 1 1 d . . . . .
C7A C 0.5581(4) 0.7379(2) 0.60744(14) 0.0449(9) Uani 1 1 d . . . . .
H7AA H 0.6305 0.7098 0.6080 0.054 Uiso 1 1 calc R U . . .
C8A C 0.4778(4) 0.7330(2) 0.56976(14) 0.0425(9) Uani 1 1 d . . . . .
C9A C 0.5026(4) 0.6867(2) 0.53188(15) 0.0438(9) Uani 1 1 d . . . . .
C10A C 0.6129(4) 0.6470(2) 0.52963(15) 0.0482(10) Uani 1 1 d . . . . .
H10B H 0.6700 0.6495 0.5543 0.058 Uiso 1 1 calc R U . . .
C11A C 0.6414(4) 0.6049(3) 0.49324(16) 0.0528(10) Uani 1 1 d . . . . .
C12A C 0.5544(5) 0.6024(3) 0.45735(17) 0.0633(13) Uani 1 1 d . . . . .
H12B H 0.5717 0.5748 0.4316 0.076 Uiso 1 1 calc R U . . .
C13A C 0.4465(5) 0.6382(3) 0.45847(17) 0.0621(12) Uani 1 1 d . . . . .
H13B H 0.3893 0.6339 0.4339 0.075 Uiso 1 1 calc R U . . .
C14A C 0.4176(4) 0.6817(2) 0.49542(16) 0.0495(10) Uani 1 1 d . . . . .
C15A C 0.6209(4) 0.7837(3) 0.68559(16) 0.0539(11) Uani 1 1 d . . . . .
C16A C 0.5537(7) 0.7479(4) 0.7240(2) 0.095(2) Uani 1 1 d . . . . .
H16D H 0.5341 0.6978 0.7160 0.142 Uiso 1 1 calc R U . . .
H16E H 0.6060 0.7487 0.7513 0.142 Uiso 1 1 calc R U . . .
H16F H 0.4782 0.7744 0.7291 0.142 Uiso 1 1 calc R U . . .
C17A C 0.6507(6) 0.8614(3) 0.6984(2) 0.0789(17) Uani 1 1 d . . . . .
H17D H 0.7046 0.8619 0.7253 0.118 Uiso 1 1 calc R U . . .
H17E H 0.6915 0.8850 0.6738 0.118 Uiso 1 1 calc R U . . .
H17F H 0.5752 0.8872 0.7044 0.118 Uiso 1 1 calc R U . . .
C18A C 0.7409(5) 0.7443(4) 0.6789(2) 0.0774(17) Uani 1 1 d . . . . .
H18D H 0.7241 0.6940 0.6706 0.116 Uiso 1 1 calc R U . . .
H18E H 0.7847 0.7680 0.6550 0.116 Uiso 1 1 calc R U . . .
H18F H 0.7909 0.7457 0.7068 0.116 Uiso 1 1 calc R U . . .
C19A C 0.7639(5) 0.5661(3) 0.49008(18) 0.0621(13) Uani 1 1 d . . . . .
C20A C 0.8325(7) 0.5628(5) 0.5345(2) 0.119(3) Uani 1 1 d . . . . .
H20D H 0.8458 0.6119 0.5459 0.179 Uiso 1 1 calc R U . . .
H20E H 0.7852 0.5352 0.5557 0.179 Uiso 1 1 calc R U . . .
H20F H 0.9114 0.5392 0.5309 0.179 Uiso 1 1 calc R U . . .
C21A C 0.8398(6) 0.6070(4) 0.4567(2) 0.0840(18) Uani 1 1 d . . . . .
H21D H 0.7952 0.6092 0.4277 0.126 Uiso 1 1 calc R U . . .
H21E H 0.8553 0.6561 0.4678 0.126 Uiso 1 1 calc R U . . .
H21F H 0.9175 0.5820 0.4533 0.126 Uiso 1 1 calc R U . . .
C22A C 0.7429(7) 0.4900(3) 0.4721(3) 0.093(2) Uani 1 1 d . . . . .
H22D H 0.6981 0.4924 0.4431 0.139 Uiso 1 1 calc R U . . .
H22E H 0.8217 0.4663 0.4684 0.139 Uiso 1 1 calc R U . . .
H22F H 0.6955 0.4623 0.4932 0.139 Uiso 1 1 calc R U . . .
Br1B Br 0.74109(5) 0.12668(3) 0.63165(2) 0.06843(17) Uani 1 1 d . . . . .
Br2B Br 0.65143(5) 0.06181(3) 0.72741(2) 0.06921(17) Uani 1 1 d . . . . .
C1B C 0.5825(4) 0.0878(2) 0.63639(17) 0.0516(10) Uani 1 1 d . . . . .
C2B C 0.5464(4) 0.0594(2) 0.67547(17) 0.0520(10) Uani 1 1 d . . . . .
C3B C 0.4277(4) 0.0273(2) 0.67894(15) 0.0479(9) Uani 1 1 d . . . . .
C4B C 0.3871(5) -0.0020(3) 0.71968(17) 0.0572(11) Uani 1 1 d . . . . .
H4BA H 0.4395 -0.0003 0.7458 0.069 Uiso 1 1 calc R U . . .
C5B C 0.2751(5) -0.0324(3) 0.72205(17) 0.0570(11) Uani 1 1 d . . . . .
H5BA H 0.2511 -0.0522 0.7497 0.068 Uiso 1 1 calc R U . . .
C6B C 0.1936(4) -0.0353(2) 0.68444(15) 0.0453(9) Uani 1 1 d . . . . .
C7B C 0.2330(4) -0.0074(2) 0.64479(15) 0.0442(9) Uani 1 1 d . . . . .
H7BA H 0.1797 -0.0095 0.6190 0.053 Uiso 1 1 calc R U . . .
C8B C 0.3494(4) 0.0243(2) 0.64091(15) 0.0430(9) Uani 1 1 d . . . . .
C9B C 0.3875(4) 0.0559(2) 0.59898(15) 0.0438(9) Uani 1 1 d . . . . .
C10B C 0.3108(4) 0.0559(2) 0.55970(16) 0.0473(9) Uani 1 1 d . . . . .
H10C H 0.2346 0.0317 0.5605 0.057 Uiso 1 1 calc R U . . .
C11B C 0.3407(4) 0.0889(2) 0.52053(16) 0.0498(10) Uani 1 1 d . . . . .
C12B C 0.4556(5) 0.1231(3) 0.52032(19) 0.0614(12) Uani 1 1 d . . . . .
H12C H 0.4794 0.1467 0.4938 0.074 Uiso 1 1 calc R U . . .
C13B C 0.5338(4) 0.1232(3) 0.55722(19) 0.0595(12) Uani 1 1 d . . . . .
H13C H 0.6105 0.1466 0.5558 0.071 Uiso 1 1 calc R U . . .
C14B C 0.5025(4) 0.0894(2) 0.59699(16) 0.0489(10) Uani 1 1 d . . . . .
C15B C 0.0675(4) -0.0702(2) 0.68904(16) 0.0515(10) Uani 1 1 d . . . . .
C16B C 0.0041(6) -0.0353(4) 0.7281(3) 0.092(2) Uani 1 1 d . . . . .
H16G H 0.0553 -0.0405 0.7555 0.137 Uiso 1 1 calc R U . . .
H16H H -0.0093 0.0161 0.7218 0.137 Uiso 1 1 calc R U . . .
H16I H -0.0746 -0.0590 0.7321 0.137 Uiso 1 1 calc R U . . .
C17B C 0.0861(6) -0.1497(3) 0.6999(3) 0.0827(18) Uani 1 1 d . . . . .
H17G H 0.1376 -0.1544 0.7273 0.124 Uiso 1 1 calc R U . . .
H17H H 0.0069 -0.1725 0.7043 0.124 Uiso 1 1 calc R U . . .
H17I H 0.1259 -0.1734 0.6751 0.124 Uiso 1 1 calc R U . . .
C18B C -0.0109(6) -0.0622(5) 0.6473(2) 0.100(2) Uani 1 1 d . . . . .
H18G H -0.0224 -0.0108 0.6405 0.149 Uiso 1 1 calc R U . . .
H18H H 0.0286 -0.0857 0.6223 0.149 Uiso 1 1 calc R U . . .
H18I H -0.0904 -0.0847 0.6515 0.149 Uiso 1 1 calc R U . . .
C19B C 0.2556(5) 0.0923(3) 0.47889(17) 0.0581(12) Uani 1 1 d . . . . .
C20B C 0.1426(6) 0.0451(4) 0.4834(2) 0.0808(18) Uani 1 1 d . . . . .
H20G H 0.0906 0.0488 0.4560 0.121 Uiso 1 1 calc R U . . .
H20H H 0.1676 -0.0053 0.4879 0.121 Uiso 1 1 calc R U . . .
H20I H 0.0971 0.0614 0.5090 0.121 Uiso 1 1 calc R U . . .
C21B C 0.3246(6) 0.0683(4) 0.4381(2) 0.0791(17) Uani 1 1 d . . . . .
H21G H 0.2701 0.0705 0.4113 0.119 Uiso 1 1 calc R U . . .
H21H H 0.3944 0.1004 0.4342 0.119 Uiso 1 1 calc R U . . .
H21I H 0.3536 0.0187 0.4425 0.119 Uiso 1 1 calc R U . . .
C22B C 0.2134(5) 0.1703(3) 0.4722(2) 0.0682(14) Uani 1 1 d . . . . .
H22G H 0.1586 0.1734 0.4456 0.102 Uiso 1 1 calc R U . . .
H22H H 0.1701 0.1862 0.4985 0.102 Uiso 1 1 calc R U . . .
H22I H 0.2844 0.2014 0.4683 0.102 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C1 1.890(4) . ?
Br2 C2 1.886(4) . ?
C1 C2 1.359(6) . ?
C1 C14 1.450(6) . ?
C2 C3 1.436(6) . ?
C3 C4 1.408(6) . ?
C3 C8 1.417(5) . ?
C4 C5 1.371(6) . ?
C4 H4A 0.9500 . ?
C5 C6 1.406(6) . ?
C5 H5A 0.9500 . ?
C6 C7 1.378(6) . ?
C6 C15 1.528(6) . ?
C7 C8 1.406(5) . ?
C7 H7A 0.9500 . ?
C8 C9 1.456(6) . ?
C9 C14 1.410(5) . ?
C9 C10 1.420(6) . ?
C10 C11 1.377(6) . ?
C10 H10A 0.9500 . ?
C11 C12 1.410(6) . ?
C11 C19 1.527(6) . ?
C12 C13 1.368(6) . ?
C12 H12A 0.9500 . ?
C13 C14 1.406(6) . ?
C13 H13A 0.9500 . ?
C15 C18 1.525(6) . ?
C15 C17 1.527(7) . ?
C15 C16 1.535(7) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.529(6) . ?
C19 C21 1.533(7) . ?
C19 C22 1.536(8) . ?
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 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
Br1A C1A 1.890(5) . ?
Br2A C2A 1.893(4) . ?
C1A C2A 1.353(7) . ?
C1A C14A 1.446(6) . ?
C2A C3A 1.441(6) . ?
C3A C8A 1.413(6) . ?
C3A C4A 1.415(6) . ?
C4A C5A 1.371(7) . ?
C4A H4AA 0.9500 . ?
C5A C6A 1.412(6) . ?
C5A H5AA 0.9500 . ?
C6A C7A 1.381(6) . ?
C6A C15A 1.525(6) . ?
C7A C8A 1.405(6) . ?
C7A H7AA 0.9500 . ?
C8A C9A 1.455(6) . ?
C9A C14A 1.409(6) . ?
C9A C10A 1.420(6) . ?
C10A C11A 1.385(6) . ?
C10A H10B 0.9500 . ?
C11A C12A 1.408(7) . ?
C11A C19A 1.532(7) . ?
C12A C13A 1.359(7) . ?
C12A H12B 0.9500 . ?
C13A C14A 1.414(7) . ?
C13A H13B 0.9500 . ?
C15A C17A 1.521(7) . ?
C15A C18A 1.526(7) . ?
C15A C16A 1.540(8) . ?
C16A H16D 0.9800 . ?
C16A H16E 0.9800 . ?
C16A H16F 0.9800 . ?
C17A H17D 0.9800 . ?
C17A H17E 0.9800 . ?
C17A H17F 0.9800 . ?
C18A H18D 0.9800 . ?
C18A H18E 0.9800 . ?
C18A H18F 0.9800 . ?
C19A C20A 1.501(9) . ?
C19A C22A 1.522(8) . ?
C19A C21A 1.527(8) . ?
C20A H20D 0.9800 . ?
C20A H20E 0.9800 . ?
C20A H20F 0.9800 . ?
C21A H21D 0.9800 . ?
C21A H21E 0.9800 . ?
C21A H21F 0.9800 . ?
C22A H22D 0.9800 . ?
C22A H22E 0.9800 . ?
C22A H22F 0.9800 . ?
Br1B C1B 1.894(5) . ?
Br2B C2B 1.896(5) . ?
C1B C2B 1.355(7) . ?
C1B C14B 1.441(7) . ?
C2B C3B 1.440(6) . ?
C3B C8B 1.398(6) . ?
C3B C4B 1.421(7) . ?
C4B C5B 1.357(7) . ?
C4B H4BA 0.9500 . ?
C5B C6B 1.409(7) . ?
C5B H5BA 0.9500 . ?
C6B C7B 1.379(6) . ?
C6B C15B 1.539(6) . ?
C7B C8B 1.415(6) . ?
C7B H7BA 0.9500 . ?
C8B C9B 1.460(6) . ?
C9B C14B 1.410(6) . ?
C9B C10B 1.417(6) . ?
C10B C11B 1.372(6) . ?
C10B H10C 0.9500 . ?
C11B C12B 1.412(7) . ?
C11B C19B 1.527(7) . ?
C12B C13B 1.370(7) . ?
C12B H12C 0.9500 . ?
C13B C14B 1.399(7) . ?
C13B H13C 0.9500 . ?
C15B C18B 1.496(8) . ?
C15B C17B 1.520(7) . ?
C15B C16B 1.527(7) . ?
C16B H16G 0.9800 . ?
C16B H16H 0.9800 . ?
C16B H16I 0.9800 . ?
C17B H17G 0.9800 . ?
C17B H17H 0.9800 . ?
C17B H17I 0.9800 . ?
C18B H18G 0.9800 . ?
C18B H18H 0.9800 . ?
C18B H18I 0.9800 . ?
C19B C22B 1.528(7) . ?
C19B C20B 1.528(7) . ?
C19B C21B 1.529(8) . ?
C20B H20G 0.9800 . ?
C20B H20H 0.9800 . ?
C20B H20I 0.9800 . ?
C21B H21G 0.9800 . ?
C21B H21H 0.9800 . ?
C21B H21I 0.9800 . ?
C22B H22G 0.9800 . ?
C22B H22H 0.9800 . ?
C22B H22I 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C14 121.0(4) . . ?
C2 C1 Br1 121.0(3) . . ?
C14 C1 Br1 118.0(3) . . ?
C1 C2 C3 121.2(4) . . ?
C1 C2 Br2 120.3(3) . . ?
C3 C2 Br2 118.4(3) . . ?
C4 C3 C8 118.6(4) . . ?
C4 C3 C2 122.2(4) . . ?
C8 C3 C2 119.1(4) . . ?
C5 C4 C3 120.9(4) . . ?
C5 C4 H4A 119.6 . . ?
C3 C4 H4A 119.6 . . ?
C4 C5 C6 121.7(4) . . ?
C4 C5 H5A 119.2 . . ?
C6 C5 H5A 119.2 . . ?
C7 C6 C5 117.3(4) . . ?
C7 C6 C15 122.8(4) . . ?
C5 C6 C15 119.9(4) . . ?
C6 C7 C8 123.0(4) . . ?
C6 C7 H7A 118.5 . . ?
C8 C7 H7A 118.5 . . ?
C7 C8 C3 118.4(4) . . ?
C7 C8 C9 122.3(4) . . ?
C3 C8 C9 119.3(4) . . ?
C14 C9 C10 118.0(4) . . ?
C14 C9 C8 119.9(4) . . ?
C10 C9 C8 122.0(4) . . ?
C11 C10 C9 122.8(4) . . ?
C11 C10 H10A 118.6 . . ?
C9 C10 H10A 118.6 . . ?
C10 C11 C12 117.5(4) . . ?
C10 C11 C19 122.9(4) . . ?
C12 C11 C19 119.6(4) . . ?
C13 C12 C11 121.5(4) . . ?
C13 C12 H12A 119.2 . . ?
C11 C12 H12A 119.2 . . ?
C12 C13 C14 121.0(4) . . ?
C12 C13 H13A 119.5 . . ?
C14 C13 H13A 119.5 . . ?
C13 C14 C9 119.1(4) . . ?
C13 C14 C1 122.1(4) . . ?
C9 C14 C1 118.8(4) . . ?
C18 C15 C17 108.7(4) . . ?
C18 C15 C6 112.4(4) . . ?
C17 C15 C6 108.8(4) . . ?
C18 C15 C16 108.3(4) . . ?
C17 C15 C16 109.0(4) . . ?
C6 C15 C16 109.7(4) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C11 C19 C20 112.0(4) . . ?
C11 C19 C21 110.2(4) . . ?
C20 C19 C21 108.0(4) . . ?
C11 C19 C22 107.9(4) . . ?
C20 C19 C22 108.4(5) . . ?
C21 C19 C22 110.2(4) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C2A C1A C14A 121.9(4) . . ?
C2A C1A Br1A 120.2(4) . . ?
C14A C1A Br1A 117.9(4) . . ?
C1A C2A C3A 120.9(4) . . ?
C1A C2A Br2A 120.9(4) . . ?
C3A C2A Br2A 118.2(3) . . ?
C8A C3A C4A 118.7(4) . . ?
C8A C3A C2A 119.1(4) . . ?
C4A C3A C2A 122.2(4) . . ?
C5A C4A C3A 120.7(4) . . ?
C5A C4A H4AA 119.6 . . ?
C3A C4A H4AA 119.6 . . ?
C4A C5A C6A 121.6(4) . . ?
C4A C5A H5AA 119.2 . . ?
C6A C5A H5AA 119.2 . . ?
C7A C6A C5A 117.2(4) . . ?
C7A C6A C15A 122.9(4) . . ?
C5A C6A C15A 119.8(4) . . ?
C6A C7A C8A 123.2(4) . . ?
C6A C7A H7AA 118.4 . . ?
C8A C7A H7AA 118.4 . . ?
C7A C8A C3A 118.4(4) . . ?
C7A C8A C9A 122.1(4) . . ?
C3A C8A C9A 119.5(4) . . ?
C14A C9A C10A 118.0(4) . . ?
C14A C9A C8A 120.1(4) . . ?
C10A C9A C8A 121.9(4) . . ?
C11A C10A C9A 123.3(4) . . ?
C11A C10A H10B 118.4 . . ?
C9A C10A H10B 118.4 . . ?
C10A C11A C12A 116.7(4) . . ?
C10A C11A C19A 122.7(4) . . ?
C12A C11A C19A 120.5(4) . . ?
C13A C12A C11A 122.0(5) . . ?
C13A C12A H12B 119.0 . . ?
C11A C12A H12B 119.0 . . ?
C12A C13A C14A 121.4(5) . . ?
C12A C13A H13B 119.3 . . ?
C14A C13A H13B 119.3 . . ?
C9A C14A C13A 118.6(4) . . ?
C9A C14A C1A 118.3(4) . . ?
C13A C14A C1A 123.1(4) . . ?
C17A C15A C6A 110.3(4) . . ?
C17A C15A C18A 107.9(4) . . ?
C6A C15A C18A 112.1(4) . . ?
C17A C15A C16A 108.9(5) . . ?
C6A C15A C16A 108.1(4) . . ?
C18A C15A C16A 109.5(5) . . ?
C15A C16A H16D 109.5 . . ?
C15A C16A H16E 109.5 . . ?
H16D C16A H16E 109.5 . . ?
C15A C16A H16F 109.5 . . ?
H16D C16A H16F 109.5 . . ?
H16E C16A H16F 109.5 . . ?
C15A C17A H17D 109.5 . . ?
C15A C17A H17E 109.5 . . ?
H17D C17A H17E 109.5 . . ?
C15A C17A H17F 109.5 . . ?
H17D C17A H17F 109.5 . . ?
H17E C17A H17F 109.5 . . ?
C15A C18A H18D 109.5 . . ?
C15A C18A H18E 109.5 . . ?
H18D C18A H18E 109.5 . . ?
C15A C18A H18F 109.5 . . ?
H18D C18A H18F 109.5 . . ?
H18E C18A H18F 109.5 . . ?
C20A C19A C22A 109.8(6) . . ?
C20A C19A C21A 109.3(6) . . ?
C22A C19A C21A 107.9(5) . . ?
C20A C19A C11A 112.0(4) . . ?
C22A C19A C11A 109.7(5) . . ?
C21A C19A C11A 108.1(4) . . ?
C19A C20A H20D 109.5 . . ?
C19A C20A H20E 109.5 . . ?
H20D C20A H20E 109.5 . . ?
C19A C20A H20F 109.5 . . ?
H20D C20A H20F 109.5 . . ?
H20E C20A H20F 109.5 . . ?
C19A C21A H21D 109.5 . . ?
C19A C21A H21E 109.5 . . ?
H21D C21A H21E 109.5 . . ?
C19A C21A H21F 109.5 . . ?
H21D C21A H21F 109.5 . . ?
H21E C21A H21F 109.5 . . ?
C19A C22A H22D 109.5 . . ?
C19A C22A H22E 109.5 . . ?
H22D C22A H22E 109.5 . . ?
C19A C22A H22F 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 109.5 . . ?
C2B C1B C14B 121.5(4) . . ?
C2B C1B Br1B 120.9(4) . . ?
C14B C1B Br1B 117.6(3) . . ?
C1B C2B C3B 121.3(4) . . ?
C1B C2B Br2B 120.5(4) . . ?
C3B C2B Br2B 118.2(4) . . ?
C8B C3B C4B 118.6(4) . . ?
C8B C3B C2B 119.1(4) . . ?
C4B C3B C2B 122.3(4) . . ?
C5B C4B C3B 121.3(5) . . ?
C5B C4B H4BA 119.4 . . ?
C3B C4B H4BA 119.4 . . ?
C4B C5B C6B 121.4(4) . . ?
C4B C5B H5BA 119.3 . . ?
C6B C5B H5BA 119.3 . . ?
C7B C6B C5B 117.4(4) . . ?
C7B C6B C15B 123.3(4) . . ?
C5B C6B C15B 119.3(4) . . ?
C6B C7B C8B 122.8(4) . . ?
C6B C7B H7BA 118.6 . . ?
C8B C7B H7BA 118.6 . . ?
C3B C8B C7B 118.5(4) . . ?
C3B C8B C9B 119.6(4) . . ?
C7B C8B C9B 121.8(4) . . ?
C14B C9B C10B 117.9(4) . . ?
C14B C9B C8B 120.0(4) . . ?
C10B C9B C8B 122.1(4) . . ?
C11B C10B C9B 123.6(4) . . ?
C11B C10B H10C 118.2 . . ?
C9B C10B H10C 118.2 . . ?
C10B C11B C12B 116.6(4) . . ?
C10B C11B C19B 123.7(4) . . ?
C12B C11B C19B 119.7(4) . . ?
C13B C12B C11B 121.9(5) . . ?
C13B C12B H12C 119.1 . . ?
C11B C12B H12C 119.1 . . ?
C12B C13B C14B 121.1(4) . . ?
C12B C13B H13C 119.5 . . ?
C14B C13B H13C 119.5 . . ?
C13B C14B C9B 119.0(4) . . ?
C13B C14B C1B 122.7(4) . . ?
C9B C14B C1B 118.3(4) . . ?
C18B C15B C17B 110.0(5) . . ?
C18B C15B C16B 109.4(5) . . ?
C17B C15B C16B 108.0(5) . . ?
C18B C15B C6B 111.9(4) . . ?
C17B C15B C6B 108.2(4) . . ?
C16B C15B C6B 109.3(4) . . ?
C15B C16B H16G 109.5 . . ?
C15B C16B H16H 109.5 . . ?
H16G C16B H16H 109.5 . . ?
C15B C16B H16I 109.5 . . ?
H16G C16B H16I 109.5 . . ?
H16H C16B H16I 109.5 . . ?
C15B C17B H17G 109.5 . . ?
C15B C17B H17H 109.5 . . ?
H17G C17B H17H 109.5 . . ?
C15B C17B H17I 109.5 . . ?
H17G C17B H17I 109.5 . . ?
H17H C17B H17I 109.5 . . ?
C15B C18B H18G 109.5 . . ?
C15B C18B H18H 109.5 . . ?
H18G C18B H18H 109.5 . . ?
C15B C18B H18I 109.5 . . ?
H18G C18B H18I 109.5 . . ?
H18H C18B H18I 109.5 . . ?
C11B C19B C22B 108.5(4) . . ?
C11B C19B C20B 112.1(4) . . ?
C22B C19B C20B 108.1(5) . . ?
C11B C19B C21B 109.4(4) . . ?
C22B C19B C21B 109.2(4) . . ?
C20B C19B C21B 109.5(5) . . ?
C19B C20B H20G 109.5 . . ?
C19B C20B H20H 109.5 . . ?
H20G C20B H20H 109.5 . . ?
C19B C20B H20I 109.5 . . ?
H20G C20B H20I 109.5 . . ?
H20H C20B H20I 109.5 . . ?
C19B C21B H21G 109.5 . . ?
C19B C21B H21H 109.5 . . ?
H21G C21B H21H 109.5 . . ?
C19B C21B H21I 109.5 . . ?
H21G C21B H21I 109.5 . . ?
H21H C21B H21I 109.5 . . ?
C19B C22B H22G 109.5 . . ?
C19B C22B H22H 109.5 . . ?
H22G C22B H22H 109.5 . . ?
C19B C22B H22I 109.5 . . ?
H22G C22B H22I 109.5 . . ?
H22H C22B H22I 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C14 C1 C2 C3 6.1(6) . . . . ?
Br1 C1 C2 C3 -174.8(3) . . . . ?
C14 C1 C2 Br2 -175.7(3) . . . . ?
Br1 C1 C2 Br2 3.5(5) . . . . ?
C1 C2 C3 C4 170.1(4) . . . . ?
Br2 C2 C3 C4 -8.2(6) . . . . ?
C1 C2 C3 C8 -9.6(6) . . . . ?
Br2 C2 C3 C8 172.1(3) . . . . ?
C8 C3 C4 C5 0.0(7) . . . . ?
C2 C3 C4 C5 -179.7(4) . . . . ?
C3 C4 C5 C6 -2.0(7) . . . . ?
C4 C5 C6 C7 1.5(7) . . . . ?
C4 C5 C6 C15 179.8(4) . . . . ?
C5 C6 C7 C8 1.0(7) . . . . ?
C15 C6 C7 C8 -177.3(4) . . . . ?
C6 C7 C8 C3 -2.9(6) . . . . ?
C6 C7 C8 C9 173.5(4) . . . . ?
C4 C3 C8 C7 2.4(6) . . . . ?
C2 C3 C8 C7 -177.9(4) . . . . ?
C4 C3 C8 C9 -174.1(4) . . . . ?
C2 C3 C8 C9 5.6(6) . . . . ?
C7 C8 C9 C14 -174.7(4) . . . . ?
C3 C8 C9 C14 1.6(6) . . . . ?
C7 C8 C9 C10 2.4(6) . . . . ?
C3 C8 C9 C10 178.8(4) . . . . ?
C14 C9 C10 C11 1.9(6) . . . . ?
C8 C9 C10 C11 -175.3(4) . . . . ?
C9 C10 C11 C12 -0.7(7) . . . . ?
C9 C10 C11 C19 -179.1(4) . . . . ?
C10 C11 C12 C13 -0.1(7) . . . . ?
C19 C11 C12 C13 178.4(5) . . . . ?
C11 C12 C13 C14 -0.3(8) . . . . ?
C12 C13 C14 C9 1.4(7) . . . . ?
C12 C13 C14 C1 -178.3(4) . . . . ?
C10 C9 C14 C13 -2.1(6) . . . . ?
C8 C9 C14 C13 175.1(4) . . . . ?
C10 C9 C14 C1 177.6(4) . . . . ?
C8 C9 C14 C1 -5.2(6) . . . . ?
C2 C1 C14 C13 -178.9(4) . . . . ?
Br1 C1 C14 C13 1.9(6) . . . . ?
C2 C1 C14 C9 1.4(6) . . . . ?
Br1 C1 C14 C9 -177.8(3) . . . . ?
C7 C6 C15 C18 -5.0(7) . . . . ?
C5 C6 C15 C18 176.8(5) . . . . ?
C7 C6 C15 C17 115.4(5) . . . . ?
C5 C6 C15 C17 -62.8(6) . . . . ?
C7 C6 C15 C16 -125.5(5) . . . . ?
C5 C6 C15 C16 56.3(6) . . . . ?
C10 C11 C19 C20 -11.8(7) . . . . ?
C12 C11 C19 C20 169.8(5) . . . . ?
C10 C11 C19 C21 -132.1(5) . . . . ?
C12 C11 C19 C21 49.5(6) . . . . ?
C10 C11 C19 C22 107.4(5) . . . . ?
C12 C11 C19 C22 -70.9(5) . . . . ?
C14A C1A C2A C3A -4.2(7) . . . . ?
Br1A C1A C2A C3A 175.7(3) . . . . ?
C14A C1A C2A Br2A 176.4(3) . . . . ?
Br1A C1A C2A Br2A -3.6(5) . . . . ?
C1A C2A C3A C8A 0.3(6) . . . . ?
Br2A C2A C3A C8A 179.6(3) . . . . ?
C1A C2A C3A C4A -179.1(4) . . . . ?
Br2A C2A C3A C4A 0.3(6) . . . . ?
C8A C3A C4A C5A -3.3(6) . . . . ?
C2A C3A C4A C5A 176.0(4) . . . . ?
C3A C4A C5A C6A 2.5(7) . . . . ?
C4A C5A C6A C7A -0.4(7) . . . . ?
C4A C5A C6A C15A -178.0(4) . . . . ?
C5A C6A C7A C8A -1.0(6) . . . . ?
C15A C6A C7A C8A 176.5(4) . . . . ?
C6A C7A C8A C3A 0.2(6) . . . . ?
C6A C7A C8A C9A 179.7(4) . . . . ?
C4A C3A C8A C7A 2.0(6) . . . . ?
C2A C3A C8A C7A -177.4(4) . . . . ?
C4A C3A C8A C9A -177.6(4) . . . . ?
C2A C3A C8A C9A 3.1(6) . . . . ?
C7A C8A C9A C14A 178.0(4) . . . . ?
C3A C8A C9A C14A -2.5(6) . . . . ?
C7A C8A C9A C10A -3.8(6) . . . . ?
C3A C8A C9A C10A 175.7(4) . . . . ?
C14A C9A C10A C11A 1.1(7) . . . . ?
C8A C9A C10A C11A -177.2(4) . . . . ?
C9A C10A C11A C12A -0.2(7) . . . . ?
C9A C10A C11A C19A 176.3(4) . . . . ?
C10A C11A C12A C13A -1.3(8) . . . . ?
C19A C11A C12A C13A -177.8(5) . . . . ?
C11A C12A C13A C14A 1.8(9) . . . . ?
C10A C9A C14A C13A -0.5(6) . . . . ?
C8A C9A C14A C13A 177.8(4) . . . . ?
C10A C9A C14A C1A -179.6(4) . . . . ?
C8A C9A C14A C1A -1.2(6) . . . . ?
C12A C13A C14A C9A -0.9(8) . . . . ?
C12A C13A C14A C1A 178.1(5) . . . . ?
C2A C1A C14A C9A 4.7(7) . . . . ?
Br1A C1A C14A C9A -175.2(3) . . . . ?
C2A C1A C14A C13A -174.3(5) . . . . ?
Br1A C1A C14A C13A 5.8(6) . . . . ?
C7A C6A C15A C17A 131.7(5) . . . . ?
C5A C6A C15A C17A -50.9(6) . . . . ?
C7A C6A C15A C18A 11.4(7) . . . . ?
C5A C6A C15A C18A -171.1(5) . . . . ?
C7A C6A C15A C16A -109.4(5) . . . . ?
C5A C6A C15A C16A 68.1(6) . . . . ?
C10A C11A C19A C20A 15.0(8) . . . . ?
C12A C11A C19A C20A -168.6(6) . . . . ?
C10A C11A C19A C22A 137.2(5) . . . . ?
C12A C11A C19A C22A -46.5(7) . . . . ?
C10A C11A C19A C21A -105.4(6) . . . . ?
C12A C11A C19A C21A 71.0(7) . . . . ?
C14B C1B C2B C3B 2.1(7) . . . . ?
Br1B C1B C2B C3B -177.7(3) . . . . ?
C14B C1B C2B Br2B -177.3(3) . . . . ?
Br1B C1B C2B Br2B 3.0(5) . . . . ?
C1B C2B C3B C8B 1.2(7) . . . . ?
Br2B C2B C3B C8B -179.4(3) . . . . ?
C1B C2B C3B C4B -179.1(4) . . . . ?
Br2B C2B C3B C4B 0.3(6) . . . . ?
C8B C3B C4B C5B 0.1(7) . . . . ?
C2B C3B C4B C5B -179.6(5) . . . . ?
C3B C4B C5B C6B -1.0(8) . . . . ?
C4B C5B C6B C7B 1.3(7) . . . . ?
C4B C5B C6B C15B -179.8(4) . . . . ?
C5B C6B C7B C8B -0.9(6) . . . . ?
C15B C6B C7B C8B -179.7(4) . . . . ?
C4B C3B C8B C7B 0.4(6) . . . . ?
C2B C3B C8B C7B -180.0(4) . . . . ?
C4B C3B C8B C9B 178.2(4) . . . . ?
C2B C3B C8B C9B -2.2(6) . . . . ?
C6B C7B C8B C3B 0.0(6) . . . . ?
C6B C7B C8B C9B -177.7(4) . . . . ?
C3B C8B C9B C14B -0.2(6) . . . . ?
C7B C8B C9B C14B 177.5(4) . . . . ?
C3B C8B C9B C10B -178.6(4) . . . . ?
C7B C8B C9B C10B -0.8(6) . . . . ?
C14B C9B C10B C11B -2.5(6) . . . . ?
C8B C9B C10B C11B 175.9(4) . . . . ?
C9B C10B C11B C12B 1.2(7) . . . . ?
C9B C10B C11B C19B -176.7(4) . . . . ?
C10B C11B C12B C13B 0.2(7) . . . . ?
C19B C11B C12B C13B 178.2(5) . . . . ?
C11B C12B C13B C14B -0.2(8) . . . . ?
C12B C13B C14B C9B -1.1(7) . . . . ?
C12B C13B C14B C1B 179.4(5) . . . . ?
C10B C9B C14B C13B 2.4(6) . . . . ?
C8B C9B C14B C13B -176.1(4) . . . . ?
C10B C9B C14B C1B -178.2(4) . . . . ?
C8B C9B C14B C1B 3.4(6) . . . . ?
C2B C1B C14B C13B 175.0(5) . . . . ?
Br1B C1B C14B C13B -5.2(6) . . . . ?
C2B C1B C14B C9B -4.4(7) . . . . ?
Br1B C1B C14B C9B 175.4(3) . . . . ?
C7B C6B C15B C18B -6.7(7) . . . . ?
C5B C6B C15B C18B 174.5(5) . . . . ?
C7B C6B C15B C17B 114.7(5) . . . . ?
C5B C6B C15B C17B -64.1(6) . . . . ?
C7B C6B C15B C16B -128.0(5) . . . . ?
C5B C6B C15B C16B 53.2(6) . . . . ?
C10B C11B C19B C22B 110.4(5) . . . . ?
C12B C11B C19B C22B -67.5(6) . . . . ?
C10B C11B C19B C20B -8.9(7) . . . . ?
C12B C11B C19B C20B 173.2(5) . . . . ?
C10B C11B C19B C21B -130.6(5) . . . . ?
C12B C11B C19B C21B 51.6(6) . . . . ?

_refine_diff_density_max         0.797
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.127

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_wa1891
_database_code_depnum_ccdc_archive 'CCDC 1883329'
_audit_update_record             
;
2018-12-05 deposited with the CCDC.
2018-12-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
; 
 ; 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H48 B2 O4'
_chemical_formula_sum            'C34 H48 B2 O4'
_chemical_formula_weight         542.34

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   11.3684(4)
_cell_length_b                   13.4509(5)
_cell_length_c                   21.2477(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3249.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    46941
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      26.5

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_F_000             1176
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.210
_exptl_absorpt_coefficient_mu    0.069
_shelx_estimated_absorpt_T_min   0.969
_shelx_estimated_absorpt_T_max   0.986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.964
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'

_exptl_special_details           
; 
 ; 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            40689
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_av_R_equivalents  0.0785
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.346
_diffrn_reflns_theta_max         25.996
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6323
_reflns_number_gt                5984
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.780
_reflns_Friedel_fraction_max     0.991
_reflns_Friedel_fraction_full    0.998

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  ?

_refine_special_details          
; 
 ; 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0566P)²+0.3483P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0110(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
; 
 Flack x determined using 2491 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.2(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6323
_refine_ls_number_parameters     362
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0381
_refine_ls_wR_factor_ref         0.0964
_refine_ls_wR_factor_gt          0.0947
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.41726(17) 0.39783(13) 0.59883(8) 0.0235(4) Uani 1 1 d . . . . .
C2 C 0.37540(17) 0.34999(13) 0.65148(8) 0.0244(4) Uani 1 1 d . . . . .
C3 C 0.26690(17) 0.38320(14) 0.68078(8) 0.0243(4) Uani 1 1 d . . . . .
C4 C 0.22655(19) 0.34086(15) 0.73780(9) 0.0315(4) Uani 1 1 d . . . . .
H4 H 0.2691 0.2872 0.7559 0.038 Uiso 1 1 calc R U . . .
C5 C 0.1284(2) 0.37509(17) 0.76745(9) 0.0346(5) Uani 1 1 d . . . . .
H5 H 0.1045 0.3452 0.8059 0.041 Uiso 1 1 calc R U . . .
C6 C 0.06141(17) 0.45370(15) 0.74249(9) 0.0289(4) Uani 1 1 d . . . . .
C7 C 0.09806(17) 0.49411(14) 0.68627(8) 0.0260(4) Uani 1 1 d . . . . .
H7 H 0.0526 0.5458 0.6679 0.031 Uiso 1 1 calc R U . . .
C8 C 0.20070(16) 0.46170(14) 0.65473(8) 0.0237(4) Uani 1 1 d . . . . .
C9 C 0.24259(16) 0.50961(13) 0.59759(8) 0.0227(4) Uani 1 1 d . . . . .
C10 C 0.18087(17) 0.58763(14) 0.56812(9) 0.0272(4) Uani 1 1 d . . . . .
H10 H 0.1084 0.6086 0.5860 0.033 Uiso 1 1 calc R U . . .
C11 C 0.22027(18) 0.63487(14) 0.51476(9) 0.0278(4) Uani 1 1 d . . . . .
C12 C 0.32606(18) 0.60162(14) 0.48822(9) 0.0286(4) Uani 1 1 d . . . . .
H12 H 0.3547 0.6317 0.4508 0.034 Uiso 1 1 calc R U . . .
C13 C 0.38883(17) 0.52579(14) 0.51580(9) 0.0268(4) Uani 1 1 d . . . . .
H13 H 0.4603 0.5048 0.4969 0.032 Uiso 1 1 calc R U . . .
C14 C 0.35067(16) 0.47851(13) 0.57098(8) 0.0227(4) Uani 1 1 d . . . . .
C15 C -0.04505(19) 0.49302(17) 0.77906(10) 0.0359(5) Uani 1 1 d . . . . .
C16 C -0.0043(3) 0.5248(3) 0.84496(12) 0.0570(7) Uani 1 1 d . . . . .
H16A H -0.0718 0.5495 0.8690 0.086 Uiso 1 1 calc R U . . .
H16B H 0.0548 0.5775 0.8412 0.086 Uiso 1 1 calc R U . . .
H16C H 0.0301 0.4675 0.8668 0.086 Uiso 1 1 calc R U . . .
C17 C -0.1367(2) 0.4097(2) 0.78561(13) 0.0482(6) Uani 1 1 d . . . . .
H17A H -0.1625 0.3885 0.7437 0.072 Uiso 1 1 calc R U . . .
H17B H -0.2044 0.4344 0.8095 0.072 Uiso 1 1 calc R U . . .
H17C H -0.1015 0.3532 0.8078 0.072 Uiso 1 1 calc R U . . .
C18 C -0.1034(2) 0.5812(2) 0.74709(13) 0.0505(6) Uani 1 1 d . . . . .
H18A H -0.1300 0.5617 0.7050 0.076 Uiso 1 1 calc R U . . .
H18B H -0.0468 0.6359 0.7435 0.076 Uiso 1 1 calc R U . . .
H18C H -0.1711 0.6030 0.7721 0.076 Uiso 1 1 calc R U . . .
C19 C 0.1503(2) 0.72218(16) 0.48726(10) 0.0340(5) Uani 1 1 d . . . . .
C20 C 0.1441(3) 0.80479(18) 0.53722(13) 0.0509(6) Uani 1 1 d . . . . .
H20A H 0.0999 0.8614 0.5204 0.076 Uiso 1 1 calc R U . . .
H20B H 0.2239 0.8262 0.5482 0.076 Uiso 1 1 calc R U . . .
H20C H 0.1045 0.7794 0.5749 0.076 Uiso 1 1 calc R U . . .
C21 C 0.0263(2) 0.68757(19) 0.46997(11) 0.0423(5) Uani 1 1 d . . . . .
H21A H -0.0182 0.7435 0.4525 0.063 Uiso 1 1 calc R U . . .
H21B H -0.0136 0.6627 0.5077 0.063 Uiso 1 1 calc R U . . .
H21C H 0.0312 0.6343 0.4386 0.063 Uiso 1 1 calc R U . . .
C22 C 0.2078(2) 0.7658(2) 0.42813(13) 0.0519(7) Uani 1 1 d . . . . .
H22A H 0.1602 0.8213 0.4126 0.078 Uiso 1 1 calc R U . . .
H22B H 0.2129 0.7143 0.3956 0.078 Uiso 1 1 calc R U . . .
H22C H 0.2870 0.7895 0.4384 0.078 Uiso 1 1 calc R U . . .
B31 B 0.53815(19) 0.36599(16) 0.56934(10) 0.0265(4) Uani 1 1 d . . . . .
O32 O 0.62165(13) 0.43129(12) 0.54945(9) 0.0418(4) Uani 1 1 d . . . . .
C33 C 0.72788(19) 0.37342(19) 0.53695(11) 0.0403(5) Uani 1 1 d . . . . .
C34 C 0.6773(2) 0.26943(18) 0.52375(10) 0.0375(5) Uani 1 1 d . . . . .
O35 O 0.56818(14) 0.26923(11) 0.56043(7) 0.0360(4) Uani 1 1 d . . . . .
C36 C 0.7944(2) 0.4199(2) 0.48265(16) 0.0612(8) Uani 1 1 d . . . . .
H36A H 0.7466 0.4158 0.4443 0.092 Uiso 1 1 calc R U . . .
H36B H 0.8685 0.3841 0.4762 0.092 Uiso 1 1 calc R U . . .
H36C H 0.8110 0.4897 0.4923 0.092 Uiso 1 1 calc R U . . .
C37 C 0.7998(2) 0.3778(3) 0.59714(15) 0.0680(9) Uani 1 1 d . . . . .
H37A H 0.8298 0.4454 0.6032 0.102 Uiso 1 1 calc R U . . .
H37B H 0.8659 0.3313 0.5941 0.102 Uiso 1 1 calc R U . . .
H37C H 0.7500 0.3595 0.6330 0.102 Uiso 1 1 calc R U . . .
C38 C 0.7537(3) 0.1835(2) 0.54487(14) 0.0600(8) Uani 1 1 d . . . . .
H38A H 0.7146 0.1206 0.5346 0.090 Uiso 1 1 calc R U . . .
H38B H 0.7661 0.1875 0.5904 0.090 Uiso 1 1 calc R U . . .
H38C H 0.8297 0.1867 0.5232 0.090 Uiso 1 1 calc R U . . .
C39 C 0.6402(3) 0.2541(2) 0.45578(12) 0.0546(7) Uani 1 1 d . . . . .
H39A H 0.5906 0.3097 0.4423 0.082 Uiso 1 1 calc R U . . .
H39B H 0.5960 0.1918 0.4522 0.082 Uiso 1 1 calc R U . . .
H39C H 0.7103 0.2508 0.4290 0.082 Uiso 1 1 calc R U . . .
B41 B 0.44566(19) 0.26230(16) 0.68341(9) 0.0261(4) Uani 1 1 d . . . . .
O42 O 0.55755(12) 0.27239(11) 0.70411(7) 0.0313(3) Uani 1 1 d . . . . .
C43 C 0.58295(19) 0.18526(16) 0.74300(9) 0.0332(4) Uani 1 1 d . . . . .
C44 C 0.4898(2) 0.10853(16) 0.72057(11) 0.0373(5) Uani 1 1 d . . . . .
O45 O 0.39641(13) 0.17281(11) 0.69620(8) 0.0376(4) Uani 1 1 d . . . . .
C46 C 0.5675(3) 0.2190(2) 0.81066(11) 0.0511(6) Uani 1 1 d . . . . .
H46A H 0.4856 0.2388 0.8176 0.077 Uiso 1 1 calc R U . . .
H46B H 0.6194 0.2757 0.8189 0.077 Uiso 1 1 calc R U . . .
H46C H 0.5876 0.1643 0.8391 0.077 Uiso 1 1 calc R U . . .
C47 C 0.7091(2) 0.1540(2) 0.73197(13) 0.0490(6) Uani 1 1 d . . . . .
H47A H 0.7183 0.1314 0.6884 0.073 Uiso 1 1 calc R U . . .
H47B H 0.7294 0.0996 0.7607 0.073 Uiso 1 1 calc R U . . .
H47C H 0.7614 0.2106 0.7396 0.073 Uiso 1 1 calc R U . . .
C48 C 0.5292(3) 0.0454(2) 0.66549(14) 0.0580(7) Uani 1 1 d . . . . .
H48A H 0.5615 0.0884 0.6325 0.087 Uiso 1 1 calc R U . . .
H48B H 0.4617 0.0084 0.6488 0.087 Uiso 1 1 calc R U . . .
H48C H 0.5897 -0.0014 0.6795 0.087 Uiso 1 1 calc R U . . .
C49 C 0.4396(2) 0.0442(2) 0.77284(15) 0.0555(7) Uani 1 1 d . . . . .
H49A H 0.4148 0.0866 0.8079 0.083 Uiso 1 1 calc R U . . .
H49B H 0.4999 -0.0025 0.7874 0.083 Uiso 1 1 calc R U . . .
H49C H 0.3717 0.0071 0.7569 0.083 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.375(3) . ?
C1 C14 1.450(3) . ?
C1 B31 1.570(3) . ?
C2 C3 1.452(3) . ?
C2 B41 1.578(3) . ?
C3 C8 1.410(3) . ?
C3 C4 1.415(3) . ?
C4 C5 1.362(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.407(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.377(3) . ?
C6 C15 1.532(3) . ?
C7 C8 1.414(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.455(3) . ?
C9 C10 1.409(3) . ?
C9 C14 1.416(3) . ?
C10 C11 1.375(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.402(3) . ?
C11 C19 1.534(3) . ?
C12 C13 1.376(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.403(3) . ?
C13 H13 0.9500 . ?
C15 C18 1.520(3) . ?
C15 C16 1.535(3) . ?
C15 C17 1.536(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C21 1.530(3) . ?
C19 C22 1.533(3) . ?
C19 C20 1.538(3) . ?
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 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
B31 O35 1.359(3) . ?
B31 O32 1.361(3) . ?
O32 C33 1.461(3) . ?
C33 C36 1.514(4) . ?
C33 C37 1.519(4) . ?
C33 C34 1.538(4) . ?
C34 O35 1.465(2) . ?
C34 C38 1.514(3) . ?
C34 C39 1.518(3) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
B41 O42 1.353(3) . ?
B41 O45 1.355(3) . ?
O42 C43 1.463(2) . ?
C43 C47 1.513(3) . ?
C43 C46 1.518(3) . ?
C43 C44 1.554(3) . ?
C44 O45 1.464(2) . ?
C44 C48 1.514(4) . ?
C44 C49 1.519(3) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C14 120.11(17) . . ?
C2 C1 B31 119.99(17) . . ?
C14 C1 B31 119.90(17) . . ?
C1 C2 C3 119.91(17) . . ?
C1 C2 B41 121.62(17) . . ?
C3 C2 B41 118.40(16) . . ?
C8 C3 C4 117.68(18) . . ?
C8 C3 C2 121.03(17) . . ?
C4 C3 C2 121.23(17) . . ?
C5 C4 C3 121.71(19) . . ?
C5 C4 H4 119.1 . . ?
C3 C4 H4 119.1 . . ?
C4 C5 C6 121.55(18) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C7 C6 C5 117.39(18) . . ?
C7 C6 C15 122.86(19) . . ?
C5 C6 C15 119.71(18) . . ?
C6 C7 C8 122.61(18) . . ?
C6 C7 H7 118.7 . . ?
C8 C7 H7 118.7 . . ?
C3 C8 C7 119.02(17) . . ?
C3 C8 C9 118.99(16) . . ?
C7 C8 C9 121.93(17) . . ?
C10 C9 C14 118.34(17) . . ?
C10 C9 C8 122.53(17) . . ?
C14 C9 C8 119.11(16) . . ?
C11 C10 C9 123.26(18) . . ?
C11 C10 H10 118.4 . . ?
C9 C10 H10 118.4 . . ?
C10 C11 C12 117.64(17) . . ?
C10 C11 C19 119.94(18) . . ?
C12 C11 C19 122.41(17) . . ?
C13 C12 C11 120.67(18) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C12 C13 C14 122.13(18) . . ?
C12 C13 H13 118.9 . . ?
C14 C13 H13 118.9 . . ?
C13 C14 C9 117.92(16) . . ?
C13 C14 C1 121.28(17) . . ?
C9 C14 C1 120.76(16) . . ?
C18 C15 C6 112.80(18) . . ?
C18 C15 C16 108.8(2) . . ?
C6 C15 C16 108.68(19) . . ?
C18 C15 C17 108.3(2) . . ?
C6 C15 C17 109.26(19) . . ?
C16 C15 C17 108.9(2) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C21 C19 C22 108.21(19) . . ?
C21 C19 C11 109.66(18) . . ?
C22 C19 C11 112.58(19) . . ?
C21 C19 C20 110.1(2) . . ?
C22 C19 C20 108.0(2) . . ?
C11 C19 C20 108.30(17) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O35 B31 O32 113.57(18) . . ?
O35 B31 C1 122.47(18) . . ?
O32 B31 C1 123.96(18) . . ?
B31 O32 C33 106.81(17) . . ?
O32 C33 C36 109.3(2) . . ?
O32 C33 C37 105.7(2) . . ?
C36 C33 C37 110.9(2) . . ?
O32 C33 C34 102.05(17) . . ?
C36 C33 C34 115.0(2) . . ?
C37 C33 C34 112.9(2) . . ?
O35 C34 C38 109.05(19) . . ?
O35 C34 C39 105.70(19) . . ?
C38 C34 C39 109.7(2) . . ?
O35 C34 C33 102.77(16) . . ?
C38 C34 C33 115.2(2) . . ?
C39 C34 C33 113.6(2) . . ?
B31 O35 C34 106.57(16) . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C33 C37 H37A 109.5 . . ?
C33 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C33 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C34 C38 H38A 109.5 . . ?
C34 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C34 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C34 C39 H39A 109.5 . . ?
C34 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C34 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O42 B41 O45 114.35(17) . . ?
O42 B41 C2 122.74(18) . . ?
O45 B41 C2 122.77(18) . . ?
B41 O42 C43 106.79(16) . . ?
O42 C43 C47 108.82(18) . . ?
O42 C43 C46 105.82(18) . . ?
C47 C43 C46 109.9(2) . . ?
O42 C43 C44 102.97(15) . . ?
C47 C43 C44 114.4(2) . . ?
C46 C43 C44 114.2(2) . . ?
O45 C44 C48 105.79(19) . . ?
O45 C44 C49 108.83(19) . . ?
C48 C44 C49 110.9(2) . . ?
O45 C44 C43 102.15(16) . . ?
C48 C44 C43 114.1(2) . . ?
C49 C44 C43 114.2(2) . . ?
B41 O45 C44 107.22(16) . . ?
C43 C46 H46A 109.5 . . ?
C43 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C43 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C43 C47 H47A 109.5 . . ?
C43 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C43 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C44 C48 H48A 109.5 . . ?
C44 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C44 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C44 C49 H49A 109.5 . . ?
C44 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C44 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C14 C1 C2 C3 -2.7(3) . . . . ?
B31 C1 C2 C3 176.53(16) . . . . ?
C14 C1 C2 B41 -179.63(16) . . . . ?
B31 C1 C2 B41 -0.4(3) . . . . ?
C1 C2 C3 C8 2.5(3) . . . . ?
B41 C2 C3 C8 179.53(16) . . . . ?
C1 C2 C3 C4 -174.82(18) . . . . ?
B41 C2 C3 C4 2.2(3) . . . . ?
C8 C3 C4 C5 -1.0(3) . . . . ?
C2 C3 C4 C5 176.38(19) . . . . ?
C3 C4 C5 C6 0.7(3) . . . . ?
C4 C5 C6 C7 0.8(3) . . . . ?
C4 C5 C6 C15 -177.1(2) . . . . ?
C5 C6 C7 C8 -2.0(3) . . . . ?
C15 C6 C7 C8 175.86(18) . . . . ?
C4 C3 C8 C7 -0.1(3) . . . . ?
C2 C3 C8 C7 -177.52(16) . . . . ?
C4 C3 C8 C9 177.40(17) . . . . ?
C2 C3 C8 C9 0.0(3) . . . . ?
C6 C7 C8 C3 1.7(3) . . . . ?
C6 C7 C8 C9 -175.78(17) . . . . ?
C3 C8 C9 C10 179.13(17) . . . . ?
C7 C8 C9 C10 -3.4(3) . . . . ?
C3 C8 C9 C14 -2.2(2) . . . . ?
C7 C8 C9 C14 175.24(17) . . . . ?
C14 C9 C10 C11 0.1(3) . . . . ?
C8 C9 C10 C11 178.79(18) . . . . ?
C9 C10 C11 C12 1.3(3) . . . . ?
C9 C10 C11 C19 -177.37(18) . . . . ?
C10 C11 C12 C13 -1.4(3) . . . . ?
C19 C11 C12 C13 177.22(18) . . . . ?
C11 C12 C13 C14 0.1(3) . . . . ?
C12 C13 C14 C9 1.4(3) . . . . ?
C12 C13 C14 C1 179.14(18) . . . . ?
C10 C9 C14 C13 -1.4(2) . . . . ?
C8 C9 C14 C13 179.84(16) . . . . ?
C10 C9 C14 C1 -179.25(16) . . . . ?
C8 C9 C14 C1 2.0(3) . . . . ?
C2 C1 C14 C13 -177.30(17) . . . . ?
B31 C1 C14 C13 3.5(3) . . . . ?
C2 C1 C14 C9 0.4(3) . . . . ?
B31 C1 C14 C9 -178.77(16) . . . . ?
C7 C6 C15 C18 -0.8(3) . . . . ?
C5 C6 C15 C18 177.0(2) . . . . ?
C7 C6 C15 C16 -121.6(2) . . . . ?
C5 C6 C15 C16 56.3(3) . . . . ?
C7 C6 C15 C17 119.7(2) . . . . ?
C5 C6 C15 C17 -62.5(3) . . . . ?
C10 C11 C19 C21 -59.8(2) . . . . ?
C12 C11 C19 C21 121.6(2) . . . . ?
C10 C11 C19 C22 179.7(2) . . . . ?
C12 C11 C19 C22 1.1(3) . . . . ?
C10 C11 C19 C20 60.4(3) . . . . ?
C12 C11 C19 C20 -118.3(2) . . . . ?
C2 C1 B31 O35 45.1(3) . . . . ?
C14 C1 B31 O35 -135.75(19) . . . . ?
C2 C1 B31 O32 -136.0(2) . . . . ?
C14 C1 B31 O32 43.2(3) . . . . ?
O35 B31 O32 C33 -11.8(2) . . . . ?
C1 B31 O32 C33 169.17(18) . . . . ?
B31 O32 C33 C36 146.8(2) . . . . ?
B31 O32 C33 C37 -93.8(2) . . . . ?
B31 O32 C33 C34 24.5(2) . . . . ?
O32 C33 C34 O35 -28.0(2) . . . . ?
C36 C33 C34 O35 -146.3(2) . . . . ?
C37 C33 C34 O35 85.0(2) . . . . ?
O32 C33 C34 C38 -146.52(19) . . . . ?
C36 C33 C34 C38 95.2(3) . . . . ?
C37 C33 C34 C38 -33.5(3) . . . . ?
O32 C33 C34 C39 85.7(2) . . . . ?
C36 C33 C34 C39 -32.6(3) . . . . ?
C37 C33 C34 C39 -161.3(2) . . . . ?
O32 B31 O35 C34 -7.4(2) . . . . ?
C1 B31 O35 C34 171.60(18) . . . . ?
C38 C34 O35 B31 144.9(2) . . . . ?
C39 C34 O35 B31 -97.2(2) . . . . ?
C33 C34 O35 B31 22.2(2) . . . . ?
C1 C2 B41 O42 56.9(3) . . . . ?
C3 C2 B41 O42 -120.1(2) . . . . ?
C1 C2 B41 O45 -127.7(2) . . . . ?
C3 C2 B41 O45 55.3(3) . . . . ?
O45 B41 O42 C43 -8.5(2) . . . . ?
C2 B41 O42 C43 167.28(17) . . . . ?
B41 O42 C43 C47 142.59(19) . . . . ?
B41 O42 C43 C46 -99.4(2) . . . . ?
B41 O42 C43 C44 20.8(2) . . . . ?
O42 C43 C44 O45 -25.0(2) . . . . ?
C47 C43 C44 O45 -142.91(19) . . . . ?
C46 C43 C44 O45 89.2(2) . . . . ?
O42 C43 C44 C48 88.7(2) . . . . ?
C47 C43 C44 C48 -29.2(3) . . . . ?
C46 C43 C44 C48 -157.1(2) . . . . ?
O42 C43 C44 C49 -142.29(19) . . . . ?
C47 C43 C44 C49 99.8(2) . . . . ?
C46 C43 C44 C49 -28.1(3) . . . . ?
O42 B41 O45 C44 -8.9(2) . . . . ?
C2 B41 O45 C44 175.37(17) . . . . ?
C48 C44 O45 B41 -98.8(2) . . . . ?
C49 C44 O45 B41 142.0(2) . . . . ?
C43 C44 O45 B41 20.9(2) . . . . ?

_refine_diff_density_max         0.185
_refine_diff_density_min         -0.132
_refine_diff_density_rms         0.032

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_wa2093
_database_code_depnum_ccdc_archive 'CCDC 1883331'
_audit_update_record             
;
2018-12-05 deposited with the CCDC.
2018-12-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H62 B2 S2'
_chemical_formula_sum            'C48 H62 B2 S2'
_chemical_formula_weight         724.71

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   33.375(2)
_cell_length_b                   11.0282(7)
_cell_length_c                   11.7509(8)
_cell_angle_alpha                90
_cell_angle_beta                 98.494(5)
_cell_angle_gamma                90
_cell_volume                     4277.7(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    15341
_cell_measurement_theta_min      3.3
_cell_measurement_theta_max      25.8

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_F_000             1568
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    0.156
_shelx_estimated_absorpt_T_min   0.956
_shelx_estimated_absorpt_T_max   0.980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.561
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24969
_diffrn_reflns_av_unetI/netI     0.0663
_diffrn_reflns_av_R_equivalents  0.0996
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.297
_diffrn_reflns_theta_max         25.655
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4025
_reflns_number_gt                2900
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  SHELXL
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0538P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4025
_refine_ls_number_parameters     239
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0488
_refine_ls_wR_factor_ref         0.1081
_refine_ls_wR_factor_gt          0.0990
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_restrained_S_all      0.981
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.55057(2) 0.72654(5) 0.49375(5) 0.02860(16) Uani 1 1 d . . . . .
B1 B 0.51695(7) 0.6011(2) 0.5782(2) 0.0215(5) Uani 1 1 d . . . . .
H1 H 0.5224(6) 0.642(2) 0.665(2) 0.023(5) Uiso 1 1 d . . . . .
C1 C 0.47132(5) 0.60687(17) 0.51344(17) 0.0190(4) Uani 1 1 d . . . . .
C2 C 0.45647(6) 0.51728(18) 0.43670(17) 0.0199(4) Uani 1 1 d . . . . .
C3 C 0.51791(10) 0.8477(3) 0.4384(4) 0.0737(12) Uani 1 1 d . . . . .
H3A H 0.5122 0.8991 0.5021 0.111 Uiso 1 1 calc R U . . .
H3B H 0.5311 0.8961 0.3847 0.111 Uiso 1 1 calc R U . . .
H3C H 0.4925 0.8143 0.3981 0.111 Uiso 1 1 calc R U . . .
C4 C 0.55564(10) 0.6506(3) 0.3631(2) 0.0536(8) Uani 1 1 d . . . . .
H4A H 0.5733 0.5798 0.3798 0.080 Uiso 1 1 calc R U . . .
H4B H 0.5289 0.6242 0.3254 0.080 Uiso 1 1 calc R U . . .
H4C H 0.5675 0.7060 0.3121 0.080 Uiso 1 1 calc R U . . .
C11 C 0.44382(5) 0.70304(17) 0.54092(17) 0.0196(4) Uani 1 1 d . . . . .
C12 C 0.40298(5) 0.70849(17) 0.48756(17) 0.0192(4) Uani 1 1 d . . . . .
C13 C 0.37648(6) 0.79447(18) 0.52701(17) 0.0211(4) Uani 1 1 d . . . . .
H13 H 0.3492 0.7975 0.4901 0.025 Uiso 1 1 calc R U . . .
C14 C 0.38849(6) 0.87365(18) 0.61622(18) 0.0218(4) Uani 1 1 d . . . . .
C15 C 0.42981(6) 0.87111(19) 0.66492(18) 0.0238(4) Uani 1 1 d . . . . .
H15 H 0.4395 0.9265 0.7247 0.029 Uiso 1 1 calc R U . . .
C16 C 0.45628(6) 0.79002(18) 0.62744(17) 0.0213(4) Uani 1 1 d . . . . .
H16 H 0.4840 0.7925 0.6609 0.026 Uiso 1 1 calc R U . . .
C17 C 0.35921(6) 0.9592(2) 0.66675(19) 0.0268(5) Uani 1 1 d . . . . .
C18 C 0.35617(8) 0.9193(3) 0.7893(2) 0.0500(7) Uani 1 1 d . . . . .
H18A H 0.3832 0.9199 0.8352 0.075 Uiso 1 1 calc R U . . .
H18B H 0.3385 0.9752 0.8234 0.075 Uiso 1 1 calc R U . . .
H18C H 0.3449 0.8372 0.7882 0.075 Uiso 1 1 calc R U . . .
C19 C 0.37506(8) 1.0897(2) 0.6671(3) 0.0487(7) Uani 1 1 d . . . . .
H19A H 0.3769 1.1148 0.5881 0.073 Uiso 1 1 calc R U . . .
H19B H 0.3564 1.1437 0.6999 0.073 Uiso 1 1 calc R U . . .
H19C H 0.4019 1.0939 0.7136 0.073 Uiso 1 1 calc R U . . .
C20 C 0.31664(7) 0.9576(2) 0.5969(2) 0.0401(6) Uani 1 1 d . . . . .
H20A H 0.3181 0.9831 0.5177 0.060 Uiso 1 1 calc R U . . .
H20B H 0.3055 0.8753 0.5966 0.060 Uiso 1 1 calc R U . . .
H20C H 0.2991 1.0134 0.6318 0.060 Uiso 1 1 calc R U . . .
C21 C 0.41509(6) 0.52627(18) 0.37498(17) 0.0204(4) Uani 1 1 d . . . . .
C22 C 0.38899(5) 0.62213(18) 0.39673(17) 0.0190(4) Uani 1 1 d . . . . .
C23 C 0.35010(5) 0.63129(18) 0.32979(17) 0.0207(4) Uani 1 1 d . . . . .
H23 H 0.3330 0.6964 0.3447 0.025 Uiso 1 1 calc R U . . .
C24 C 0.33610(6) 0.55000(19) 0.24418(18) 0.0232(4) Uani 1 1 d . . . . .
C25 C 0.36204(6) 0.4527(2) 0.22598(19) 0.0268(5) Uani 1 1 d . . . . .
H25 H 0.3532 0.3941 0.1685 0.032 Uiso 1 1 calc R U . . .
C26 C 0.39971(6) 0.44126(19) 0.28947(19) 0.0255(5) Uani 1 1 d . . . . .
H26 H 0.4161 0.3739 0.2756 0.031 Uiso 1 1 calc R U . . .
C27 C 0.29493(6) 0.5605(2) 0.1679(2) 0.0297(5) Uani 1 1 d . . . . .
C28 C 0.27089(7) 0.4429(3) 0.1771(3) 0.0474(7) Uani 1 1 d . . . . .
H28A H 0.2670 0.4301 0.2572 0.071 Uiso 1 1 calc R U . . .
H28B H 0.2444 0.4493 0.1285 0.071 Uiso 1 1 calc R U . . .
H28C H 0.2859 0.3743 0.1512 0.071 Uiso 1 1 calc R U . . .
C29 C 0.26951(7) 0.6659(2) 0.2042(2) 0.0407(6) Uani 1 1 d . . . . .
H29A H 0.2650 0.6540 0.2839 0.061 Uiso 1 1 calc R U . . .
H29B H 0.2840 0.7424 0.1980 0.061 Uiso 1 1 calc R U . . .
H29C H 0.2434 0.6685 0.1537 0.061 Uiso 1 1 calc R U . . .
C30 C 0.30134(8) 0.5822(3) 0.0438(2) 0.0520(8) Uani 1 1 d . . . . .
H30A H 0.2750 0.5890 -0.0052 0.078 Uiso 1 1 calc R U . . .
H30B H 0.3167 0.6574 0.0392 0.078 Uiso 1 1 calc R U . . .
H30C H 0.3165 0.5142 0.0175 0.078 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C4 1.778(3) . ?
S1 C3 1.785(3) . ?
S1 B1 2.118(2) . ?
B1 C1 1.600(3) . ?
B1 C2 1.603(3) 5_666 ?
B1 H1 1.10(2) . ?
C1 C2 1.380(3) . ?
C1 C11 1.469(3) . ?
C2 C21 1.465(3) . ?
C2 B1 1.603(3) 5_666 ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C11 C12 1.415(3) . ?
C11 C16 1.415(3) . ?
C12 C13 1.420(3) . ?
C12 C22 1.455(3) . ?
C13 C14 1.378(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.413(3) . ?
C14 C17 1.539(3) . ?
C15 C16 1.374(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.524(3) . ?
C17 C20 1.532(3) . ?
C17 C19 1.533(3) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
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 C26 1.414(3) . ?
C21 C22 1.417(3) . ?
C22 C23 1.419(3) . ?
C23 C24 1.377(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.415(3) . ?
C24 C27 1.530(3) . ?
C25 C26 1.370(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C30 1.525(3) . ?
C27 C29 1.535(3) . ?
C27 C28 1.538(3) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 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
C4 S1 C3 99.70(18) . . ?
C4 S1 B1 102.80(11) . . ?
C3 S1 B1 108.79(11) . . ?
C1 B1 C2 118.94(18) . 5_666 ?
C1 B1 S1 106.51(14) . . ?
C2 B1 S1 98.09(12) 5_666 . ?
C1 B1 H1 116.0(11) . . ?
C2 B1 H1 114.5(11) 5_666 . ?
S1 B1 H1 98.0(11) . . ?
C2 C1 C11 118.99(17) . . ?
C2 C1 B1 120.49(17) . . ?
C11 C1 B1 120.38(17) . . ?
C1 C2 C21 119.77(17) . . ?
C1 C2 B1 120.23(18) . 5_666 ?
C21 C2 B1 119.84(18) . 5_666 ?
S1 C3 H3A 109.5 . . ?
S1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
S1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
S1 C4 H4A 109.5 . . ?
S1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
S1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C12 C11 C16 116.83(16) . . ?
C12 C11 C1 121.70(18) . . ?
C16 C11 C1 121.35(17) . . ?
C11 C12 C13 119.29(18) . . ?
C11 C12 C22 118.75(16) . . ?
C13 C12 C22 121.91(17) . . ?
C14 C13 C12 123.11(18) . . ?
C14 C13 H13 118.4 . . ?
C12 C13 H13 118.4 . . ?
C13 C14 C15 116.90(17) . . ?
C13 C14 C17 123.51(18) . . ?
C15 C14 C17 119.55(19) . . ?
C16 C15 C14 121.2(2) . . ?
C16 C15 H15 119.4 . . ?
C14 C15 H15 119.4 . . ?
C15 C16 C11 122.45(18) . . ?
C15 C16 H16 118.8 . . ?
C11 C16 H16 118.8 . . ?
C18 C17 C20 108.49(19) . . ?
C18 C17 C19 109.8(2) . . ?
C20 C17 C19 107.7(2) . . ?
C18 C17 C14 108.80(18) . . ?
C20 C17 C14 112.19(18) . . ?
C19 C17 C14 109.75(17) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C26 C21 C22 117.03(18) . . ?
C26 C21 C2 121.57(17) . . ?
C22 C21 C2 121.38(18) . . ?
C21 C22 C23 119.32(18) . . ?
C21 C22 C12 118.78(17) . . ?
C23 C22 C12 121.90(17) . . ?
C24 C23 C22 122.87(18) . . ?
C24 C23 H23 118.6 . . ?
C22 C23 H23 118.6 . . ?
C23 C24 C25 117.08(19) . . ?
C23 C24 C27 123.84(18) . . ?
C25 C24 C27 119.08(19) . . ?
C26 C25 C24 121.4(2) . . ?
C26 C25 H25 119.3 . . ?
C24 C25 H25 119.3 . . ?
C25 C26 C21 122.25(19) . . ?
C25 C26 H26 118.9 . . ?
C21 C26 H26 118.9 . . ?
C30 C27 C24 109.35(17) . . ?
C30 C27 C29 107.9(2) . . ?
C24 C27 C29 112.37(19) . . ?
C30 C27 C28 110.3(2) . . ?
C24 C27 C28 109.14(19) . . ?
C29 C27 C28 107.68(19) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 B1 C1 C2 -6.7(3) 5_666 . . . ?
S1 B1 C1 C2 102.68(18) . . . . ?
C2 B1 C1 C11 169.03(16) 5_666 . . . ?
S1 B1 C1 C11 -81.60(19) . . . . ?
C11 C1 C2 C21 6.5(3) . . . . ?
B1 C1 C2 C21 -177.76(17) . . . . ?
C11 C1 C2 B1 -169.00(16) . . . 5_666 ?
B1 C1 C2 B1 6.8(3) . . . 5_666 ?
C2 C1 C11 C12 -2.4(3) . . . . ?
B1 C1 C11 C12 -178.14(17) . . . . ?
C2 C1 C11 C16 173.54(18) . . . . ?
B1 C1 C11 C16 -2.2(3) . . . . ?
C16 C11 C12 C13 -3.5(3) . . . . ?
C1 C11 C12 C13 172.57(17) . . . . ?
C16 C11 C12 C22 178.97(17) . . . . ?
C1 C11 C12 C22 -5.0(3) . . . . ?
C11 C12 C13 C14 -0.4(3) . . . . ?
C22 C12 C13 C14 177.05(18) . . . . ?
C12 C13 C14 C15 3.4(3) . . . . ?
C12 C13 C14 C17 -174.33(18) . . . . ?
C13 C14 C15 C16 -2.4(3) . . . . ?
C17 C14 C15 C16 175.42(19) . . . . ?
C14 C15 C16 C11 -1.6(3) . . . . ?
C12 C11 C16 C15 4.6(3) . . . . ?
C1 C11 C16 C15 -171.54(18) . . . . ?
C13 C14 C17 C18 112.8(2) . . . . ?
C15 C14 C17 C18 -64.8(3) . . . . ?
C13 C14 C17 C20 -7.2(3) . . . . ?
C15 C14 C17 C20 175.1(2) . . . . ?
C13 C14 C17 C19 -127.0(2) . . . . ?
C15 C14 C17 C19 55.4(3) . . . . ?
C1 C2 C21 C26 175.27(19) . . . . ?
B1 C2 C21 C26 -9.2(3) 5_666 . . . ?
C1 C2 C21 C22 -3.4(3) . . . . ?
B1 C2 C21 C22 172.09(17) 5_666 . . . ?
C26 C21 C22 C23 -2.7(3) . . . . ?
C2 C21 C22 C23 176.07(17) . . . . ?
C26 C21 C22 C12 177.31(17) . . . . ?
C2 C21 C22 C12 -4.0(3) . . . . ?
C11 C12 C22 C21 7.9(3) . . . . ?
C13 C12 C22 C21 -169.51(17) . . . . ?
C11 C12 C22 C23 -172.09(17) . . . . ?
C13 C12 C22 C23 10.4(3) . . . . ?
C21 C22 C23 C24 0.6(3) . . . . ?
C12 C22 C23 C24 -179.38(18) . . . . ?
C22 C23 C24 C25 1.3(3) . . . . ?
C22 C23 C24 C27 -177.69(18) . . . . ?
C23 C24 C25 C26 -1.1(3) . . . . ?
C27 C24 C25 C26 177.9(2) . . . . ?
C24 C25 C26 C21 -1.0(3) . . . . ?
C22 C21 C26 C25 2.9(3) . . . . ?
C2 C21 C26 C25 -175.8(2) . . . . ?
C23 C24 C27 C30 115.1(2) . . . . ?
C25 C24 C27 C30 -63.9(3) . . . . ?
C23 C24 C27 C29 -4.8(3) . . . . ?
C25 C24 C27 C29 176.2(2) . . . . ?
C23 C24 C27 C28 -124.1(2) . . . . ?
C25 C24 C27 C28 56.8(3) . . . . ?

_refine_diff_density_max         0.202
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.042

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_wa2238_sq
_database_code_depnum_ccdc_archive 'CCDC 1883332'
_audit_update_record             
;
2018-12-18 deposited with the CCDC.
2018-12-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H50 B2 O2'
_chemical_formula_sum            'C44 H50 B2 O2'
_chemical_formula_weight         632.46

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 3'

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

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

_cell_length_a                   15.7492(16)
_cell_length_b                   15.7492(16)
_cell_length_c                   14.4036(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3094.0(7)
_cell_formula_units_Z            3
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5983
_cell_measurement_theta_min      3.19
_cell_measurement_theta_max      25.78

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.018
_exptl_crystal_F_000             1020
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.060
_shelx_estimated_absorpt_T_min   0.992
_shelx_estimated_absorpt_T_max   0.998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.438
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27007
_diffrn_reflns_av_unetI/netI     0.1585
_diffrn_reflns_av_R_equivalents  0.1974
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.199
_diffrn_reflns_theta_max         25.842
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3914
_reflns_number_gt                1870
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 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. 
;

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  SHELXL
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3914
_refine_ls_number_parameters     218
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.2055
_refine_ls_R_factor_gt           0.1282
_refine_ls_wR_factor_ref         0.2931
_refine_ls_wR_factor_gt          0.2607
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_restrained_S_all      1.173
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


# SQUEEZE RESULTS 
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.012 -0.008 -0.000 1161 132 ' '
_platon_squeeze_void_probe_radius 0.50
_platon_squeeze_details          ?


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
B1 B 0.4638(4) 0.9002(4) 0.4768(5) 0.0311(14) Uani 1 1 d . . . . .
O1 O 0.4030(3) 0.8011(3) 0.4745(3) 0.0509(12) Uani 1 1 d . . . . .
H1 H 0.349502 0.748320 0.473523 0.076 Uiso 1 1 d R U . . .
C1 C 0.5462(4) 0.9492(4) 0.5520(4) 0.0278(11) Uani 1 1 d . . . . .
C2 C 0.5657(4) 1.0388(4) 0.5884(4) 0.0311(12) Uani 1 1 d . . . . .
C11 C 0.6192(4) 1.0740(4) 0.6744(4) 0.0357(13) Uani 1 1 d . . . . .
C12 C 0.6593(4) 1.0215(4) 0.7202(4) 0.0317(12) Uani 1 1 d . . . . .
C13 C 0.7003(4) 1.0524(4) 0.8096(4) 0.0353(13) Uani 1 1 d . . . . .
H13 H 0.724886 1.015576 0.839952 0.042 Uiso 1 1 calc R U . . .
C14 C 0.7069(5) 1.1314(5) 0.8553(4) 0.0443(15) Uani 1 1 d . . . . .
C15 C 0.6710(5) 1.1857(5) 0.8069(5) 0.0504(17) Uani 1 1 d . . . . .
H15 H 0.676282 1.242605 0.835299 0.060 Uiso 1 1 calc R U . . .
C16 C 0.6286(5) 1.1585(5) 0.7198(5) 0.0458(16) Uani 1 1 d . . . . .
H16 H 0.605391 1.196770 0.689917 0.055 Uiso 1 1 calc R U . . .
C17 C 0.7511(6) 1.1632(6) 0.9530(5) 0.061(2) Uani 1 1 d . . . . .
C18 C 0.6822(14) 1.1607(14) 1.0153(12) 0.174(7) Uani 1 1 d . U . . .
H18A H 0.648644 1.192704 0.987306 0.260 Uiso 1 1 calc R U . . .
H18B H 0.634101 1.092463 1.029983 0.260 Uiso 1 1 calc R U . . .
H18C H 0.715335 1.195339 1.072330 0.260 Uiso 1 1 calc R U . . .
C19 C 0.8410(9) 1.2762(9) 0.9427(8) 0.108(4) Uani 1 1 d . U . . .
H19A H 0.889738 1.278387 0.898966 0.163 Uiso 1 1 calc R U . . .
H19B H 0.815363 1.317495 0.919580 0.163 Uiso 1 1 calc R U . . .
H19C H 0.871797 1.300360 1.003423 0.163 Uiso 1 1 calc R U . . .
C20 C 0.8090(5) 1.1177(5) 0.9843(5) 0.0578(18) Uani 1 1 d . U . . .
H20A H 0.854769 1.123673 0.935255 0.087 Uiso 1 1 calc R U . . .
H20B H 0.845817 1.151049 1.040421 0.087 Uiso 1 1 calc R U . . .
H20C H 0.764584 1.048173 0.998073 0.087 Uiso 1 1 calc R U . . .
C21 C 0.5972(4) 0.9002(4) 0.5927(3) 0.0267(11) Uani 1 1 d . . . . .
C22 C 0.6562(4) 0.9390(4) 0.6722(4) 0.0283(12) Uani 1 1 d . . . . .
C23 C 0.7141(4) 0.8977(4) 0.7016(4) 0.0306(12) Uani 1 1 d . . . . .
H23 H 0.752596 0.922934 0.756176 0.037 Uiso 1 1 calc R U . . .
C24 C 0.7172(4) 0.8226(4) 0.6545(4) 0.0311(12) Uani 1 1 d . . . . .
C25 C 0.6558(4) 0.7835(4) 0.5766(4) 0.0315(12) Uani 1 1 d . . . . .
H25 H 0.654345 0.730420 0.543916 0.038 Uiso 1 1 calc R U . . .
C26 C 0.5977(4) 0.8205(4) 0.5466(4) 0.0311(12) Uani 1 1 d . . . . .
H26 H 0.556943 0.792110 0.493827 0.037 Uiso 1 1 calc R U . . .
C27 C 0.7877(4) 0.7860(4) 0.6806(4) 0.0365(13) Uani 1 1 d . . . . .
C28 C 0.8634(4) 0.8148(5) 0.6018(5) 0.0454(15) Uani 1 1 d . . . . .
H28A H 0.829253 0.786370 0.543193 0.068 Uiso 1 1 calc R U . . .
H28B H 0.901124 0.886335 0.596215 0.068 Uiso 1 1 calc R U . . .
H28C H 0.907852 0.789845 0.615793 0.068 Uiso 1 1 calc R U . . .
C29 C 0.8425(5) 0.8311(5) 0.7715(4) 0.0410(14) Uani 1 1 d . . . . .
H29A H 0.886576 0.805630 0.785305 0.062 Uiso 1 1 calc R U . . .
H29B H 0.880889 0.902597 0.765174 0.062 Uiso 1 1 calc R U . . .
H29C H 0.795155 0.813958 0.822173 0.062 Uiso 1 1 calc R U . . .
C30 C 0.7297(5) 0.6720(4) 0.6900(5) 0.0491(16) Uani 1 1 d . . . . .
H30A H 0.694501 0.642896 0.632014 0.074 Uiso 1 1 calc R U . . .
H30B H 0.775487 0.648446 0.702752 0.074 Uiso 1 1 calc R U . . .
H30C H 0.682548 0.653127 0.741113 0.074 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
B1 O1 1.363(7) . ?
B1 C1 1.566(8) . ?
B1 C2 1.570(8) 4_676 ?
O1 H1 0.8372 . ?
C1 C2 1.389(7) . ?
C1 C21 1.484(7) . ?
C2 C11 1.444(7) . ?
C11 C16 1.423(8) . ?
C11 C12 1.428(8) . ?
C12 C13 1.413(8) . ?
C12 C22 1.452(7) . ?
C13 C14 1.365(8) . ?
C13 H13 0.9500 . ?
C14 C15 1.422(9) . ?
C14 C17 1.538(9) . ?
C15 C16 1.385(9) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.394(18) . ?
C17 C20 1.484(10) . ?
C17 C19 1.635(14) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
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 C26 1.423(7) . ?
C21 C22 1.408(7) . ?
C22 C23 1.424(7) . ?
C23 C24 1.386(7) . ?
C23 H23 0.9500 . ?
C24 C25 1.406(8) . ?
C24 C27 1.530(8) . ?
C25 C26 1.377(8) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C29 1.533(8) . ?
C27 C28 1.541(8) . ?
C27 C30 1.561(8) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 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 B1 C1 121.0(5) . . ?
O1 B1 C2 115.6(5) . 4_676 ?
C1 B1 C2 122.5(5) . 4_676 ?
B1 O1 H1 156.9 . . ?
C2 C1 C21 118.6(5) . . ?
C2 C1 B1 118.0(5) . . ?
C21 C1 B1 123.2(4) . . ?
C1 C2 C11 120.2(5) . . ?
C1 C2 B1 114.5(5) . 4_676 ?
C11 C2 B1 124.9(5) . 4_676 ?
C16 C11 C2 121.4(5) . . ?
C16 C11 C12 117.4(5) . . ?
C2 C11 C12 121.1(5) . . ?
C13 C12 C22 123.2(5) . . ?
C13 C12 C11 118.7(5) . . ?
C22 C12 C11 118.1(5) . . ?
C14 C13 C12 124.6(5) . . ?
C14 C13 H13 117.7 . . ?
C12 C13 H13 117.7 . . ?
C13 C14 C15 116.1(5) . . ?
C13 C14 C17 123.7(6) . . ?
C15 C14 C17 120.3(5) . . ?
C16 C15 C14 122.2(6) . . ?
C16 C15 H15 118.9 . . ?
C14 C15 H15 118.9 . . ?
C15 C16 C11 121.0(6) . . ?
C15 C16 H16 119.5 . . ?
C11 C16 H16 119.5 . . ?
C18 C17 C20 116.6(10) . . ?
C18 C17 C14 111.1(10) . . ?
C20 C17 C14 114.1(6) . . ?
C18 C17 C19 109.1(10) . . ?
C20 C17 C19 98.4(7) . . ?
C14 C17 C19 106.0(7) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C26 C21 C22 117.9(5) . . ?
C26 C21 C1 121.2(4) . . ?
C22 C21 C1 120.4(5) . . ?
C23 C22 C21 118.6(5) . . ?
C23 C22 C12 121.6(5) . . ?
C21 C22 C12 119.7(5) . . ?
C24 C23 C22 123.2(5) . . ?
C24 C23 H23 118.4 . . ?
C22 C23 H23 118.4 . . ?
C23 C24 C25 117.0(5) . . ?
C23 C24 C27 122.8(5) . . ?
C25 C24 C27 120.1(5) . . ?
C26 C25 C24 121.5(5) . . ?
C26 C25 H25 119.2 . . ?
C24 C25 H25 119.2 . . ?
C25 C26 C21 121.6(5) . . ?
C25 C26 H26 119.2 . . ?
C21 C26 H26 119.2 . . ?
C29 C27 C24 112.5(4) . . ?
C29 C27 C28 108.6(5) . . ?
C24 C27 C28 107.9(5) . . ?
C29 C27 C30 109.2(5) . . ?
C24 C27 C30 109.6(5) . . ?
C28 C27 C30 108.9(5) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?

_refine_diff_density_max         1.107
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.091



####################################################################### 
# 
# 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_wa2498
_database_code_depnum_ccdc_archive 'CCDC 1883336'
_audit_update_record             
;
2018-12-05 deposited with the CCDC.
2018-12-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C70 H74 B2'
_chemical_formula_sum            'C70 H74 B2'
_chemical_formula_weight         936.91

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'

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

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

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

_cell_length_a                   11.0286(9)
_cell_length_b                   11.0444(9)
_cell_length_c                   13.2897(11)
_cell_angle_alpha                94.589(7)
_cell_angle_beta                 98.390(6)
_cell_angle_gamma                115.448(6)
_cell_volume                     1427.5(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    20397
_cell_measurement_theta_min      3.4
_cell_measurement_theta_max      27.98

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_F_000             504
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.240
_exptl_absorpt_coefficient_mu    0.061
_shelx_estimated_absorpt_T_min   0.984
_shelx_estimated_absorpt_T_max   0.986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.609
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20397
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.404
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             5818
_reflns_number_gt                4257
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  SHELXL
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0948P)²+0.2285P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5818
_refine_ls_number_parameters     356
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0626
_refine_ls_wR_factor_ref         0.1765
_refine_ls_wR_factor_gt          0.1625
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
B1 B 0.0945(2) 0.6149(2) 0.58643(14) 0.0299(4) Uani 1 1 d . . . . .
C1 C 0.13827(17) 0.50546(17) 0.54663(13) 0.0305(4) Uani 1 1 d . . . . .
C11 C 0.05030(17) 0.40004(17) 0.46258(13) 0.0310(4) Uani 1 1 d . . . . .
C12 C 0.09546(18) 0.30894(18) 0.42496(13) 0.0327(4) Uani 1 1 d . . . . .
H12 H 0.038904 0.241768 0.367060 0.039 Uiso 1 1 calc R U . . .
C13 C 0.22092(17) 0.31143(17) 0.46851(13) 0.0309(4) Uani 1 1 d . . . . .
C3 C 0.30525(17) 0.41117(17) 0.55477(13) 0.0305(4) Uani 1 1 d . . . . .
C2 C 0.26234(17) 0.50856(18) 0.58968(13) 0.0321(4) Uani 1 1 d . . . . .
H2 H 0.321194 0.579029 0.644995 0.039 Uiso 1 1 calc R U . . .
C14 C 0.26712(18) 0.21682(17) 0.42294(13) 0.0311(4) Uani 1 1 d . . . . .
C15 C 0.40058(18) 0.23368(17) 0.46074(13) 0.0309(4) Uani 1 1 d . . . . .
C16 C 0.44819(19) 0.1537(2) 0.40558(14) 0.0374(4) Uani 1 1 d . . . . .
H16 H 0.539852 0.167547 0.426876 0.045 Uiso 1 1 calc R U . . .
C17 C 0.3653(2) 0.0564(2) 0.32178(15) 0.0424(5) Uani 1 1 d . . . . .
H17 H 0.401732 0.006648 0.285304 0.051 Uiso 1 1 calc R U . . .
C18 C 0.2279(2) 0.0294(2) 0.28935(14) 0.0392(4) Uani 1 1 d . . . . .
C19 C 0.18260(19) 0.11165(19) 0.34028(14) 0.0363(4) Uani 1 1 d . . . . .
H19 H 0.090575 0.096543 0.318546 0.044 Uiso 1 1 calc R U . . .
C41 C 0.1322(2) -0.0877(2) 0.20113(17) 0.0523(6) Uani 1 1 d . U . . .
C42 C 0.1935(5) -0.0584(6) 0.1012(3) 0.0849(19) Uani 0.687(9) 1 d . U P A 1
H42A H 0.196005 0.026574 0.082429 0.127 Uiso 0.687(9) 1 calc R U P A 1
H42B H 0.286624 -0.050322 0.114102 0.127 Uiso 0.687(9) 1 calc R U P A 1
H42C H 0.135968 -0.133183 0.044625 0.127 Uiso 0.687(9) 1 calc R U P A 1
C43 C -0.0115(5) -0.0994(7) 0.1757(5) 0.0747(18) Uani 0.687(9) 1 d . U P A 1
H43A H -0.006546 -0.012268 0.160130 0.112 Uiso 0.687(9) 1 calc R U P A 1
H43B H -0.064922 -0.170082 0.115705 0.112 Uiso 0.687(9) 1 calc R U P A 1
H43C H -0.055917 -0.123215 0.234784 0.112 Uiso 0.687(9) 1 calc R U P A 1
C44 C 0.1310(7) -0.2166(4) 0.2254(4) 0.085(2) Uani 0.687(9) 1 d . U P A 1
H44A H 0.225333 -0.205113 0.241321 0.127 Uiso 0.687(9) 1 calc R U P A 1
H44B H 0.088006 -0.241639 0.284936 0.127 Uiso 0.687(9) 1 calc R U P A 1
H44C H 0.079001 -0.288507 0.165857 0.127 Uiso 0.687(9) 1 calc R U P A 1
C42' C 0.2012(14) -0.1479(16) 0.1398(10) 0.103(5) Uani 0.313(9) 1 d . U P A 2
H42D H 0.260908 -0.173120 0.186400 0.155 Uiso 0.313(9) 1 calc R U P A 2
H42E H 0.131883 -0.229021 0.092717 0.155 Uiso 0.313(9) 1 calc R U P A 2
H42F H 0.256098 -0.081378 0.100043 0.155 Uiso 0.313(9) 1 calc R U P A 2
C43' C 0.0414(17) -0.0490(13) 0.1321(10) 0.080(4) Uani 0.313(9) 1 d . U P A 2
H43D H -0.003400 -0.009488 0.173358 0.120 Uiso 0.313(9) 1 calc R U P A 2
H43E H 0.095773 0.017915 0.092263 0.120 Uiso 0.313(9) 1 calc R U P A 2
H43F H -0.028442 -0.129728 0.084937 0.120 Uiso 0.313(9) 1 calc R U P A 2
C44' C 0.039(2) -0.2125(13) 0.2583(11) 0.127(6) Uani 0.313(9) 1 d . U P A 2
H44D H 0.098565 -0.238197 0.304078 0.190 Uiso 0.313(9) 1 calc R U P A 2
H44E H -0.013946 -0.182474 0.298761 0.190 Uiso 0.313(9) 1 calc R U P A 2
H44F H -0.024658 -0.290876 0.206193 0.190 Uiso 0.313(9) 1 calc R U P A 2
C4 C 0.43373(17) 0.41259(17) 0.60459(13) 0.0304(4) Uani 1 1 d . . . . .
C5 C 0.48163(17) 0.32719(18) 0.55693(13) 0.0314(4) Uani 1 1 d . . . . .
C6 C 0.60481(19) 0.33069(19) 0.60711(15) 0.0379(4) Uani 1 1 d . . . . .
H6 H 0.639984 0.275522 0.575979 0.045 Uiso 1 1 calc R U . . .
C7 C 0.6756(2) 0.4127(2) 0.70070(15) 0.0408(4) Uani 1 1 d . . . . .
H7 H 0.758770 0.412918 0.732240 0.049 Uiso 1 1 calc R U . . .
C8 C 0.62816(18) 0.49577(19) 0.75061(14) 0.0353(4) Uani 1 1 d . . . . .
C9 C 0.50795(18) 0.49426(19) 0.70071(14) 0.0350(4) Uani 1 1 d . . . . .
H9 H 0.474197 0.550367 0.732436 0.042 Uiso 1 1 calc R U . . .
C31 C 0.7065(2) 0.5804(2) 0.85720(15) 0.0428(5) Uani 1 1 d . . . . .
C32 C 0.8551(2) 0.6732(3) 0.8514(2) 0.0654(7) Uani 1 1 d . . . . .
H32A H 0.856435 0.734665 0.801932 0.098 Uiso 1 1 calc R U . . .
H32B H 0.905234 0.726442 0.919566 0.098 Uiso 1 1 calc R U . . .
H32C H 0.898794 0.617730 0.829163 0.098 Uiso 1 1 calc R U . . .
C33 C 0.6437(3) 0.6708(3) 0.8953(2) 0.0718(8) Uani 1 1 d . . . . .
H33A H 0.643676 0.731961 0.845756 0.108 Uiso 1 1 calc R U . . .
H33B H 0.549343 0.613846 0.902060 0.108 Uiso 1 1 calc R U . . .
H33C H 0.697904 0.724546 0.962446 0.108 Uiso 1 1 calc R U . . .
C34 C 0.7063(4) 0.4862(3) 0.93392(19) 0.0807(9) Uani 1 1 d . . . . .
H34A H 0.611641 0.426332 0.938202 0.121 Uiso 1 1 calc R U . . .
H34B H 0.750360 0.431238 0.911409 0.121 Uiso 1 1 calc R U . . .
H34C H 0.756800 0.539950 1.001813 0.121 Uiso 1 1 calc R U . . .
C21 C 0.19115(17) 0.74295(18) 0.66977(13) 0.0312(4) Uani 1 1 d . . . . .
C26 C 0.2444(2) 0.8733(2) 0.64017(17) 0.0432(5) Uani 1 1 d . . . . .
C25 C 0.3211(2) 0.9891(2) 0.7136(2) 0.0625(7) Uani 1 1 d . . . . .
H25 H 0.356100 1.075254 0.691587 0.075 Uiso 1 1 calc R U . . .
C24 C 0.3484(3) 0.9832(3) 0.8177(2) 0.0705(8) Uani 1 1 d . . . . .
C23 C 0.2966(3) 0.8554(3) 0.84668(18) 0.0666(8) Uani 1 1 d . . . . .
H23 H 0.313884 0.848637 0.917655 0.080 Uiso 1 1 calc R U . . .
C22 C 0.2196(2) 0.7358(2) 0.77538(15) 0.0447(5) Uani 1 1 d . . . . .
C27 C 0.2173(3) 0.8882(3) 0.5288(2) 0.0594(6) Uani 1 1 d . . . . .
H27A H 0.144264 0.916590 0.516365 0.089 Uiso 1 1 calc R U . . .
H27B H 0.189027 0.801027 0.485175 0.089 Uiso 1 1 calc R U . . .
H27C H 0.301008 0.956853 0.512120 0.089 Uiso 1 1 calc R U . . .
C29 C 0.4294(4) 1.1120(4) 0.8942(3) 0.1161(15) Uani 1 1 d . . . . .
H29A H 0.520407 1.161399 0.878305 0.174 Uiso 1 1 calc R U . . .
H29B H 0.438892 1.089587 0.963895 0.174 Uiso 1 1 calc R U . . .
H29C H 0.381422 1.168968 0.890289 0.174 Uiso 1 1 calc R U . . .
C28 C 0.1643(3) 0.5996(3) 0.81217(19) 0.0651(7) Uani 1 1 d . . . . .
H28A H 0.233998 0.566355 0.817654 0.098 Uiso 1 1 calc R U . . .
H28B H 0.081980 0.534558 0.762872 0.098 Uiso 1 1 calc R U . . .
H28C H 0.141220 0.609617 0.879804 0.098 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
B1 C1 1.565(2) . ?
B1 C11 1.566(2) 2_566 ?
B1 C21 1.572(2) . ?
C1 C2 1.389(2) . ?
C1 C11 1.432(2) . ?
C11 C12 1.390(2) . ?
C12 C13 1.408(2) . ?
C12 H12 0.9500 . ?
C13 C3 1.414(2) . ?
C13 C14 1.471(2) . ?
C3 C2 1.420(2) . ?
C3 C4 1.467(2) . ?
C2 H2 0.9500 . ?
C14 C15 1.410(2) . ?
C14 C19 1.411(2) . ?
C15 C16 1.414(2) . ?
C15 C5 1.470(2) . ?
C16 C17 1.378(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.404(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.387(2) . ?
C18 C41 1.544(3) . ?
C19 H19 0.9500 . ?
C41 C44 1.480(5) . ?
C41 C43' 1.480(11) . ?
C41 C42' 1.488(11) . ?
C41 C43 1.518(5) . ?
C41 C42 1.571(5) . ?
C41 C44' 1.648(15) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C42' H42D 0.9800 . ?
C42' H42E 0.9800 . ?
C42' H42F 0.9800 . ?
C43' H43D 0.9800 . ?
C43' H43E 0.9800 . ?
C43' H43F 0.9800 . ?
C44' H44D 0.9800 . ?
C44' H44E 0.9800 . ?
C44' H44F 0.9800 . ?
C4 C9 1.411(2) . ?
C4 C5 1.414(2) . ?
C5 C6 1.407(2) . ?
C6 C7 1.380(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.404(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.386(2) . ?
C8 C31 1.537(2) . ?
C9 H9 0.9500 . ?
C31 C34 1.514(3) . ?
C31 C32 1.533(3) . ?
C31 C33 1.533(3) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C21 C22 1.409(3) . ?
C21 C26 1.415(3) . ?
C26 C25 1.390(3) . ?
C26 C27 1.504(3) . ?
C25 C24 1.385(4) . ?
C25 H25 0.9500 . ?
C24 C23 1.388(4) . ?
C24 C29 1.506(3) . ?
C23 C22 1.401(3) . ?
C23 H23 0.9500 . ?
C22 C28 1.514(3) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 B1 C11 118.50(15) . 2_566 ?
C1 B1 C21 123.24(15) . . ?
C11 B1 C21 118.20(14) 2_566 . ?
C2 C1 C11 118.45(14) . . ?
C2 C1 B1 121.72(15) . . ?
C11 C1 B1 119.82(14) . . ?
C12 C11 C1 118.52(15) . . ?
C12 C11 B1 119.93(15) . 2_566 ?
C1 C11 B1 121.55(14) . 2_566 ?
C11 C12 C13 123.18(15) . . ?
C11 C12 H12 118.4 . . ?
C13 C12 H12 118.4 . . ?
C12 C13 C3 118.55(15) . . ?
C12 C13 C14 121.11(15) . . ?
C3 C13 C14 120.28(15) . . ?
C13 C3 C2 118.15(15) . . ?
C13 C3 C4 119.79(14) . . ?
C2 C3 C4 122.06(15) . . ?
C1 C2 C3 122.99(15) . . ?
C1 C2 H2 118.5 . . ?
C3 C2 H2 118.5 . . ?
C15 C14 C19 118.98(15) . . ?
C15 C14 C13 119.30(15) . . ?
C19 C14 C13 121.70(15) . . ?
C14 C15 C16 117.54(16) . . ?
C14 C15 C5 119.64(15) . . ?
C16 C15 C5 122.76(15) . . ?
C17 C16 C15 121.81(17) . . ?
C17 C16 H16 119.1 . . ?
C15 C16 H16 119.1 . . ?
C16 C17 C18 121.18(16) . . ?
C16 C17 H17 119.4 . . ?
C18 C17 H17 119.4 . . ?
C19 C18 C17 117.11(17) . . ?
C19 C18 C41 121.95(17) . . ?
C17 C18 C41 120.94(16) . . ?
C18 C19 C14 122.94(17) . . ?
C18 C19 H19 118.5 . . ?
C14 C19 H19 118.5 . . ?
C43' C41 C42' 110.3(8) . . ?
C44 C41 C43 111.9(4) . . ?
C44 C41 C18 109.7(2) . . ?
C43' C41 C18 111.8(4) . . ?
C42' C41 C18 115.6(5) . . ?
C43 C41 C18 113.3(2) . . ?
C44 C41 C42 106.9(4) . . ?
C43 C41 C42 106.7(4) . . ?
C18 C41 C42 108.1(2) . . ?
C43' C41 C44' 109.4(9) . . ?
C42' C41 C44' 103.9(9) . . ?
C18 C41 C44' 105.3(4) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C41 C42' H42D 109.5 . . ?
C41 C42' H42E 109.5 . . ?
H42D C42' H42E 109.5 . . ?
C41 C42' H42F 109.5 . . ?
H42D C42' H42F 109.5 . . ?
H42E C42' H42F 109.5 . . ?
C41 C43' H43D 109.5 . . ?
C41 C43' H43E 109.5 . . ?
H43D C43' H43E 109.5 . . ?
C41 C43' H43F 109.5 . . ?
H43D C43' H43F 109.5 . . ?
H43E C43' H43F 109.5 . . ?
C41 C44' H44D 109.5 . . ?
C41 C44' H44E 109.5 . . ?
H44D C44' H44E 109.5 . . ?
C41 C44' H44F 109.5 . . ?
H44D C44' H44F 109.5 . . ?
H44E C44' H44F 109.5 . . ?
C9 C4 C5 119.45(15) . . ?
C9 C4 C3 121.21(15) . . ?
C5 C4 C3 119.32(14) . . ?
C6 C5 C4 117.78(15) . . ?
C6 C5 C15 121.79(15) . . ?
C4 C5 C15 120.36(14) . . ?
C7 C6 C5 121.31(16) . . ?
C7 C6 H6 119.3 . . ?
C5 C6 H6 119.3 . . ?
C6 C7 C8 121.86(16) . . ?
C6 C7 H7 119.1 . . ?
C8 C7 H7 119.1 . . ?
C9 C8 C7 117.04(16) . . ?
C9 C8 C31 122.75(16) . . ?
C7 C8 C31 120.19(16) . . ?
C8 C9 C4 122.54(16) . . ?
C8 C9 H9 118.7 . . ?
C4 C9 H9 118.7 . . ?
C34 C31 C32 108.8(2) . . ?
C34 C31 C33 109.3(2) . . ?
C32 C31 C33 107.7(2) . . ?
C34 C31 C8 109.34(18) . . ?
C32 C31 C8 109.51(17) . . ?
C33 C31 C8 112.14(16) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C22 C21 C26 117.54(17) . . ?
C22 C21 B1 122.87(17) . . ?
C26 C21 B1 119.41(16) . . ?
C25 C26 C21 120.6(2) . . ?
C25 C26 C27 119.2(2) . . ?
C21 C26 C27 120.29(18) . . ?
C24 C25 C26 122.3(3) . . ?
C24 C25 H25 118.8 . . ?
C26 C25 H25 118.8 . . ?
C25 C24 C23 117.1(2) . . ?
C25 C24 C29 120.1(3) . . ?
C23 C24 C29 122.8(3) . . ?
C24 C23 C22 122.6(2) . . ?
C24 C23 H23 118.7 . . ?
C22 C23 H23 118.7 . . ?
C23 C22 C21 119.9(2) . . ?
C23 C22 C28 120.0(2) . . ?
C21 C22 C28 120.12(19) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C24 C29 H29A 109.5 . . ?
C24 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C24 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C22 C28 H28A 109.5 . . ?
C22 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C22 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C11 B1 C1 C2 -176.97(16) 2_566 . . . ?
C21 B1 C1 C2 5.9(3) . . . . ?
C11 B1 C1 C11 4.1(3) 2_566 . . . ?
C21 B1 C1 C11 -173.07(17) . . . . ?
C2 C1 C11 C12 -2.7(3) . . . . ?
B1 C1 C11 C12 176.29(16) . . . . ?
C2 C1 C11 B1 176.81(16) . . . 2_566 ?
B1 C1 C11 B1 -4.2(3) . . . 2_566 ?
C1 C11 C12 C13 3.0(3) . . . . ?
B1 C11 C12 C13 -176.50(17) 2_566 . . . ?
C11 C12 C13 C3 0.1(3) . . . . ?
C11 C12 C13 C14 -177.13(17) . . . . ?
C12 C13 C3 C2 -3.3(3) . . . . ?
C14 C13 C3 C2 173.89(16) . . . . ?
C12 C13 C3 C4 177.34(16) . . . . ?
C14 C13 C3 C4 -5.4(3) . . . . ?
C11 C1 C2 C3 -0.6(3) . . . . ?
B1 C1 C2 C3 -179.58(17) . . . . ?
C13 C3 C2 C1 3.7(3) . . . . ?
C4 C3 C2 C1 -177.01(17) . . . . ?
C12 C13 C14 C15 172.01(17) . . . . ?
C3 C13 C14 C15 -5.1(3) . . . . ?
C12 C13 C14 C19 -6.2(3) . . . . ?
C3 C13 C14 C19 176.65(17) . . . . ?
C19 C14 C15 C16 7.2(3) . . . . ?
C13 C14 C15 C16 -171.04(16) . . . . ?
C19 C14 C15 C5 -169.99(16) . . . . ?
C13 C14 C15 C5 11.8(2) . . . . ?
C14 C15 C16 C17 -4.1(3) . . . . ?
C5 C15 C16 C17 172.99(18) . . . . ?
C15 C16 C17 C18 -2.0(3) . . . . ?
C16 C17 C18 C19 4.7(3) . . . . ?
C16 C17 C18 C41 -174.9(2) . . . . ?
C17 C18 C19 C14 -1.4(3) . . . . ?
C41 C18 C19 C14 178.21(19) . . . . ?
C15 C14 C19 C18 -4.6(3) . . . . ?
C13 C14 C19 C18 173.59(18) . . . . ?
C19 C18 C41 C44 -124.4(4) . . . . ?
C17 C18 C41 C44 55.3(4) . . . . ?
C19 C18 C41 C43' 40.5(9) . . . . ?
C17 C18 C41 C43' -139.9(9) . . . . ?
C19 C18 C41 C42' 167.7(8) . . . . ?
C17 C18 C41 C42' -12.6(9) . . . . ?
C19 C18 C41 C43 1.5(5) . . . . ?
C17 C18 C41 C43 -178.9(4) . . . . ?
C19 C18 C41 C42 119.4(3) . . . . ?
C17 C18 C41 C42 -60.9(4) . . . . ?
C19 C18 C41 C44' -78.2(9) . . . . ?
C17 C18 C41 C44' 101.4(9) . . . . ?
C13 C3 C4 C9 -168.68(17) . . . . ?
C2 C3 C4 C9 12.0(3) . . . . ?
C13 C3 C4 C5 9.2(3) . . . . ?
C2 C3 C4 C5 -170.05(17) . . . . ?
C9 C4 C5 C6 -1.7(3) . . . . ?
C3 C4 C5 C6 -179.69(17) . . . . ?
C9 C4 C5 C15 175.35(16) . . . . ?
C3 C4 C5 C15 -2.6(3) . . . . ?
C14 C15 C5 C6 169.00(17) . . . . ?
C16 C15 C5 C6 -8.1(3) . . . . ?
C14 C15 C5 C4 -8.0(3) . . . . ?
C16 C15 C5 C4 174.98(17) . . . . ?
C4 C5 C6 C7 1.2(3) . . . . ?
C15 C5 C6 C7 -175.85(18) . . . . ?
C5 C6 C7 C8 0.4(3) . . . . ?
C6 C7 C8 C9 -1.3(3) . . . . ?
C6 C7 C8 C31 177.06(19) . . . . ?
C7 C8 C9 C4 0.7(3) . . . . ?
C31 C8 C9 C4 -177.60(18) . . . . ?
C5 C4 C9 C8 0.8(3) . . . . ?
C3 C4 C9 C8 178.72(17) . . . . ?
C9 C8 C31 C34 116.0(2) . . . . ?
C7 C8 C31 C34 -62.3(3) . . . . ?
C9 C8 C31 C32 -124.9(2) . . . . ?
C7 C8 C31 C32 56.8(3) . . . . ?
C9 C8 C31 C33 -5.4(3) . . . . ?
C7 C8 C31 C33 176.3(2) . . . . ?
C1 B1 C21 C22 -75.1(2) . . . . ?
C11 B1 C21 C22 107.7(2) 2_566 . . . ?
C1 B1 C21 C26 109.95(19) . . . . ?
C11 B1 C21 C26 -67.2(2) 2_566 . . . ?
C22 C21 C26 C25 -0.3(3) . . . . ?
B1 C21 C26 C25 174.89(17) . . . . ?
C22 C21 C26 C27 -179.74(18) . . . . ?
B1 C21 C26 C27 -4.5(3) . . . . ?
C21 C26 C25 C24 -0.4(3) . . . . ?
C27 C26 C25 C24 179.1(2) . . . . ?
C26 C25 C24 C23 0.5(3) . . . . ?
C26 C25 C24 C29 -178.5(3) . . . . ?
C25 C24 C23 C22 0.0(4) . . . . ?
C29 C24 C23 C22 179.1(3) . . . . ?
C24 C23 C22 C21 -0.7(3) . . . . ?
C24 C23 C22 C28 -179.2(2) . . . . ?
C26 C21 C22 C23 0.8(3) . . . . ?
B1 C21 C22 C23 -174.19(18) . . . . ?
C26 C21 C22 C28 179.30(18) . . . . ?
B1 C21 C22 C28 4.3(3) . . . . ?

_refine_diff_density_max         0.429
_refine_diff_density_min         -0.183
_refine_diff_density_rms         0.040

####################################################################### 
# 
# 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_wa2371
_database_code_depnum_ccdc_archive 'CCDC 1883334'
_audit_update_record             
;
2018-12-05 deposited with the CCDC.
2018-12-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H34 B2 S4, 2(C H Cl3)'
_chemical_formula_sum            'C48 H36 B2 Cl6 S4'
_chemical_formula_weight         975.33

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   8.4808(12)
_cell_length_b                   10.1241(17)
_cell_length_c                   14.101(2)
_cell_angle_alpha                107.102(13)
_cell_angle_beta                 100.164(12)
_cell_angle_gamma                93.247(13)
_cell_volume                     1131.4(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    4939
_cell_measurement_theta_min      3.26
_cell_measurement_theta_max      25.83

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_F_000             500
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.600
_shelx_estimated_absorpt_T_min   0.926
_shelx_estimated_absorpt_T_max   0.982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.805
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8326
_diffrn_reflns_av_unetI/netI     0.1130
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.350
_diffrn_reflns_theta_max         25.661
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             4214
_reflns_number_gt                2333
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  SHELXL
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0515P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4214
_refine_ls_number_parameters     274
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1248
_refine_ls_R_factor_gt           0.0608
_refine_ls_wR_factor_ref         0.1373
_refine_ls_wR_factor_gt          0.1167
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_restrained_S_all      0.922
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
B1 B 0.5775(6) 0.6088(6) 0.9634(4) 0.0417(12) Uani 1 1 d . . . . .
S2 S 0.14841(17) -0.04450(13) 0.69255(9) 0.0534(4) Uani 1 1 d . . . . .
S1 S 0.54828(16) 0.36930(13) 0.55208(8) 0.0468(3) Uani 1 1 d . . . . .
C1 C 0.5085(5) 0.4620(4) 0.8878(3) 0.0393(10) Uani 1 1 d . . . . .
C11 C 0.4274(5) 0.3607(4) 0.9215(3) 0.0406(11) Uani 1 1 d . . . . .
C12 C 0.3538(6) 0.2373(4) 0.8509(3) 0.0411(11) Uani 1 1 d . . . . .
H12 H 0.298380 0.171384 0.873047 0.049 Uiso 1 1 calc R U . . .
C13 C 0.3578(5) 0.2053(4) 0.7464(3) 0.0398(10) Uani 1 1 d . . . . .
C14 C 0.2726(5) 0.0812(4) 0.6711(3) 0.0425(11) Uani 1 1 d . . . . .
C15 C 0.2756(6) 0.0507(5) 0.5675(3) 0.0444(12) Uani 1 1 d . . . . .
C5 C 0.3689(5) 0.1454(4) 0.5356(3) 0.0394(11) Uani 1 1 d . . . . .
C4 C 0.4519(5) 0.2660(4) 0.6083(3) 0.0381(10) Uani 1 1 d . . . . .
C3 C 0.4460(5) 0.3004(4) 0.7147(3) 0.0394(11) Uani 1 1 d . . . . .
C2 C 0.5190(5) 0.4291(4) 0.7860(3) 0.0399(10) Uani 1 1 d . . . . .
H2 H 0.576170 0.494243 0.764008 0.048 Uiso 1 1 calc R U . . .
C17 C 0.1022(6) -0.1356(5) 0.5654(4) 0.0536(13) Uani 1 1 d . . . . .
H17 H 0.031154 -0.219669 0.537621 0.064 Uiso 1 1 calc R U . . .
C16 C 0.1773(6) -0.0753(5) 0.5088(3) 0.0494(12) Uani 1 1 d . . . . .
H16 H 0.165581 -0.113269 0.437479 0.059 Uiso 1 1 calc R U . . .
C6 C 0.3874(6) 0.1405(5) 0.4359(3) 0.0506(13) Uani 1 1 d . . . . .
H6 H 0.339636 0.065653 0.377124 0.061 Uiso 1 1 calc R U . . .
C7 C 0.4785(6) 0.2513(5) 0.4329(3) 0.0535(13) Uani 1 1 d . . . . .
H7 H 0.501956 0.263481 0.372421 0.064 Uiso 1 1 calc R U . . .
C21 C 0.6378(5) 0.7312(4) 0.9250(3) 0.0396(10) Uani 1 1 d . . . . .
C22 C 0.8007(6) 0.7617(5) 0.9255(3) 0.0539(13) Uani 1 1 d . . . . .
C23 C 0.8492(7) 0.8774(7) 0.8951(4) 0.0687(18) Uani 1 1 d . . . . .
H23 H 0.960218 0.899145 0.896490 0.082 Uiso 1 1 calc R U . . .
C24 C 0.7377(8) 0.9594(6) 0.8632(4) 0.0633(15) Uani 1 1 d . . . . .
C25 C 0.5791(7) 0.9257(5) 0.8613(4) 0.0539(13) Uani 1 1 d . . . . .
H25 H 0.501748 0.979940 0.838832 0.065 Uiso 1 1 calc R U . . .
C26 C 0.5265(6) 0.8135(5) 0.8915(3) 0.0445(11) Uani 1 1 d . . . . .
C28 C 0.9197(7) 0.6693(8) 0.9576(4) 0.0775(19) Uani 1 1 d . . . . .
H28A H 0.914303 0.668628 1.026266 0.116 Uiso 1 1 calc R U . . .
H28B H 1.028997 0.705041 0.956479 0.116 Uiso 1 1 calc R U . . .
H28C H 0.892870 0.574383 0.910683 0.116 Uiso 1 1 calc R U . . .
C29 C 0.7934(10) 1.0855(6) 0.8337(5) 0.095(2) Uani 1 1 d . . . . .
H29A H 0.709210 1.099281 0.781290 0.142 Uiso 1 1 calc R U . . .
H29B H 0.892556 1.069462 0.807420 0.142 Uiso 1 1 calc R U . . .
H29C H 0.814131 1.168517 0.893330 0.142 Uiso 1 1 calc R U . . .
C27 C 0.3495(6) 0.7857(5) 0.8926(4) 0.0543(13) Uani 1 1 d . . . . .
H27A H 0.294216 0.865372 0.884666 0.081 Uiso 1 1 calc R U . . .
H27B H 0.338743 0.771594 0.957070 0.081 Uiso 1 1 calc R U . . .
H27C H 0.301108 0.702093 0.836648 0.081 Uiso 1 1 calc R U . . .
C1L C 0.9803(6) 0.4715(5) 0.6439(4) 0.0532(13) Uani 1 1 d . . . . .
H1L H 0.898556 0.415087 0.583003 0.064 Uiso 1 1 calc R U . . .
Cl1 Cl 1.0033(2) 0.37810(16) 0.73170(12) 0.0785(5) Uani 1 1 d . . . . .
Cl2 Cl 1.16424(16) 0.49420(16) 0.60462(10) 0.0662(4) Uani 1 1 d . . . . .
Cl3 Cl 0.90850(17) 0.63066(13) 0.69344(10) 0.0608(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
B1 C1 1.561(7) . ?
B1 C11 1.569(6) 2_667 ?
B1 C21 1.585(7) . ?
S2 C17 1.720(5) . ?
S2 C14 1.734(5) . ?
S1 C7 1.729(5) . ?
S1 C4 1.735(5) . ?
C1 C2 1.396(6) . ?
C1 C11 1.440(6) . ?
C11 C12 1.378(6) . ?
C12 C13 1.420(6) . ?
C12 H12 0.9500 . ?
C13 C3 1.406(6) . ?
C13 C14 1.439(6) . ?
C14 C15 1.406(6) . ?
C15 C16 1.422(7) . ?
C15 C5 1.429(7) . ?
C5 C4 1.396(6) . ?
C5 C6 1.429(6) . ?
C4 C3 1.447(6) . ?
C3 C2 1.418(6) . ?
C2 H2 0.9500 . ?
C17 C16 1.355(7) . ?
C17 H17 0.9500 . ?
C16 H16 0.9500 . ?
C6 C7 1.340(7) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C21 C22 1.396(7) . ?
C21 C26 1.405(6) . ?
C22 C23 1.424(8) . ?
C22 C28 1.515(8) . ?
C23 C24 1.395(9) . ?
C23 H23 0.9500 . ?
C24 C25 1.362(8) . ?
C24 C29 1.530(8) . ?
C25 C26 1.401(7) . ?
C25 H25 0.9500 . ?
C26 C27 1.515(7) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C1L Cl3 1.748(5) . ?
C1L Cl1 1.757(5) . ?
C1L Cl2 1.770(5) . ?
C1L H1L 1.0000 . ?

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 B1 C11 119.1(4) . 2_667 ?
C1 B1 C21 121.4(4) . . ?
C11 B1 C21 119.3(4) 2_667 . ?
C17 S2 C14 91.1(2) . . ?
C7 S1 C4 91.6(2) . . ?
C2 C1 C11 119.1(4) . . ?
C2 C1 B1 120.5(4) . . ?
C11 C1 B1 120.3(4) . . ?
C12 C11 C1 118.9(4) . . ?
C12 C11 B1 120.9(4) . 2_667 ?
C1 C11 B1 120.3(4) . 2_667 ?
C11 C12 C13 122.4(4) . . ?
C11 C12 H12 118.8 . . ?
C13 C12 H12 118.8 . . ?
C3 C13 C12 118.6(4) . . ?
C3 C13 C14 118.4(4) . . ?
C12 C13 C14 122.9(4) . . ?
C15 C14 C13 122.7(4) . . ?
C15 C14 S2 111.3(3) . . ?
C13 C14 S2 126.0(3) . . ?
C14 C15 C16 111.6(5) . . ?
C14 C15 C5 118.9(4) . . ?
C16 C15 C5 129.5(4) . . ?
C4 C5 C15 118.7(4) . . ?
C4 C5 C6 111.6(4) . . ?
C15 C5 C6 129.6(4) . . ?
C5 C4 C3 122.8(4) . . ?
C5 C4 S1 110.8(3) . . ?
C3 C4 S1 126.2(3) . . ?
C13 C3 C2 119.5(4) . . ?
C13 C3 C4 118.4(4) . . ?
C2 C3 C4 122.1(4) . . ?
C1 C2 C3 121.3(4) . . ?
C1 C2 H2 119.4 . . ?
C3 C2 H2 119.4 . . ?
C16 C17 S2 113.1(4) . . ?
C16 C17 H17 123.4 . . ?
S2 C17 H17 123.4 . . ?
C17 C16 C15 112.9(4) . . ?
C17 C16 H16 123.6 . . ?
C15 C16 H16 123.6 . . ?
C7 C6 C5 113.8(4) . . ?
C7 C6 H6 123.1 . . ?
C5 C6 H6 123.1 . . ?
C6 C7 S1 112.1(4) . . ?
C6 C7 H7 123.9 . . ?
S1 C7 H7 123.9 . . ?
C22 C21 C26 118.7(5) . . ?
C22 C21 B1 121.6(4) . . ?
C26 C21 B1 119.7(4) . . ?
C21 C22 C23 119.2(5) . . ?
C21 C22 C28 118.6(5) . . ?
C23 C22 C28 122.2(5) . . ?
C24 C23 C22 121.6(5) . . ?
C24 C23 H23 119.2 . . ?
C22 C23 H23 119.2 . . ?
C25 C24 C23 118.2(5) . . ?
C25 C24 C29 121.3(6) . . ?
C23 C24 C29 120.6(6) . . ?
C24 C25 C26 122.1(5) . . ?
C24 C25 H25 119.0 . . ?
C26 C25 H25 119.0 . . ?
C25 C26 C21 120.3(5) . . ?
C25 C26 C27 119.6(4) . . ?
C21 C26 C27 120.1(4) . . ?
C22 C28 H28A 109.5 . . ?
C22 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C22 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C24 C29 H29A 109.5 . . ?
C24 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C24 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
Cl3 C1L Cl1 111.2(3) . . ?
Cl3 C1L Cl2 111.6(3) . . ?
Cl1 C1L Cl2 110.2(3) . . ?
Cl3 C1L H1L 107.9 . . ?
Cl1 C1L H1L 107.9 . . ?
Cl2 C1L H1L 107.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C11 B1 C1 C2 -176.5(4) 2_667 . . . ?
C21 B1 C1 C2 8.9(6) . . . . ?
C11 B1 C1 C11 6.1(7) 2_667 . . . ?
C21 B1 C1 C11 -168.5(4) . . . . ?
C2 C1 C11 C12 -3.9(6) . . . . ?
B1 C1 C11 C12 173.5(4) . . . . ?
C2 C1 C11 B1 176.4(4) . . . 2_667 ?
B1 C1 C11 B1 -6.2(7) . . . 2_667 ?
C1 C11 C12 C13 1.3(7) . . . . ?
B1 C11 C12 C13 -179.0(4) 2_667 . . . ?
C11 C12 C13 C3 2.8(6) . . . . ?
C11 C12 C13 C14 -175.8(4) . . . . ?
C3 C13 C14 C15 0.7(6) . . . . ?
C12 C13 C14 C15 179.3(4) . . . . ?
C3 C13 C14 S2 -176.3(3) . . . . ?
C12 C13 C14 S2 2.3(6) . . . . ?
C17 S2 C14 C15 0.1(3) . . . . ?
C17 S2 C14 C13 177.4(4) . . . . ?
C13 C14 C15 C16 -177.9(4) . . . . ?
S2 C14 C15 C16 -0.5(5) . . . . ?
C13 C14 C15 C5 1.0(6) . . . . ?
S2 C14 C15 C5 178.4(3) . . . . ?
C14 C15 C5 C4 -1.0(6) . . . . ?
C16 C15 C5 C4 177.8(4) . . . . ?
C14 C15 C5 C6 -177.8(4) . . . . ?
C16 C15 C5 C6 1.0(8) . . . . ?
C15 C5 C4 C3 -0.8(6) . . . . ?
C6 C5 C4 C3 176.6(4) . . . . ?
C15 C5 C4 S1 -177.0(3) . . . . ?
C6 C5 C4 S1 0.4(5) . . . . ?
C7 S1 C4 C5 -0.3(3) . . . . ?
C7 S1 C4 C3 -176.3(4) . . . . ?
C12 C13 C3 C2 -4.3(6) . . . . ?
C14 C13 C3 C2 174.4(4) . . . . ?
C12 C13 C3 C4 178.9(4) . . . . ?
C14 C13 C3 C4 -2.4(6) . . . . ?
C5 C4 C3 C13 2.6(6) . . . . ?
S1 C4 C3 C13 178.1(3) . . . . ?
C5 C4 C3 C2 -174.1(4) . . . . ?
S1 C4 C3 C2 1.4(6) . . . . ?
C11 C1 C2 C3 2.5(6) . . . . ?
B1 C1 C2 C3 -175.0(4) . . . . ?
C13 C3 C2 C1 1.7(6) . . . . ?
C4 C3 C2 C1 178.3(4) . . . . ?
C14 S2 C17 C16 0.4(4) . . . . ?
S2 C17 C16 C15 -0.8(6) . . . . ?
C14 C15 C16 C17 0.9(6) . . . . ?
C5 C15 C16 C17 -178.0(4) . . . . ?
C4 C5 C6 C7 -0.3(6) . . . . ?
C15 C5 C6 C7 176.7(5) . . . . ?
C5 C6 C7 S1 0.1(6) . . . . ?
C4 S1 C7 C6 0.1(4) . . . . ?
C1 B1 C21 C22 -97.0(5) . . . . ?
C11 B1 C21 C22 88.4(5) 2_667 . . . ?
C1 B1 C21 C26 84.4(5) . . . . ?
C11 B1 C21 C26 -90.2(5) 2_667 . . . ?
C26 C21 C22 C23 1.9(6) . . . . ?
B1 C21 C22 C23 -176.8(4) . . . . ?
C26 C21 C22 C28 -177.6(4) . . . . ?
B1 C21 C22 C28 3.8(6) . . . . ?
C21 C22 C23 C24 -1.1(7) . . . . ?
C28 C22 C23 C24 178.3(4) . . . . ?
C22 C23 C24 C25 -0.3(7) . . . . ?
C22 C23 C24 C29 178.3(4) . . . . ?
C23 C24 C25 C26 0.9(7) . . . . ?
C29 C24 C25 C26 -177.7(5) . . . . ?
C24 C25 C26 C21 -0.1(7) . . . . ?
C24 C25 C26 C27 177.0(4) . . . . ?
C22 C21 C26 C25 -1.3(6) . . . . ?
B1 C21 C26 C25 177.3(4) . . . . ?
C22 C21 C26 C27 -178.4(4) . . . . ?
B1 C21 C26 C27 0.3(6) . . . . ?

_refine_diff_density_max         0.466
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.065

