# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 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_exp_3036
_database_code_depnum_ccdc_archive 'CCDC 1523638'
_audit_update_record             
;
2016-12-20 deposited with the CCDC.
2018-06-22 downloaded from the CCDC.
;
_audit_creation_date             2016-11-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C21 H31 B2 N O4'
_chemical_formula_sum            'C21 H31 B2 N O4'
_chemical_formula_weight         383.09
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.6906(9)
_cell_length_b                   10.9669(11)
_cell_length_c                   11.5436(13)
_cell_angle_alpha                70.045(10)
_cell_angle_beta                 86.183(8)
_cell_angle_gamma                84.832(8)
_cell_volume                     1147.6(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1764
_cell_measurement_temperature    295.1(2)
_cell_measurement_theta_max      26.2330
_cell_measurement_theta_min      3.1940
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       grism
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.846
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8809
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.846
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.172
_diffrn_reflns_theta_min         2.880
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.1(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1213
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.846
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0329730000
_diffrn_orient_matrix_UB_12      -0.0031371000
_diffrn_orient_matrix_UB_13      0.0540922000
_diffrn_orient_matrix_UB_21      0.0653069000
_diffrn_orient_matrix_UB_22      0.0039577000
_diffrn_orient_matrix_UB_23      -0.0321901000
_diffrn_orient_matrix_UB_31      -0.0075497000
_diffrn_orient_matrix_UB_32      0.0688010000
_diffrn_orient_matrix_UB_33      -0.0178140000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2923
_reflns_number_total             5241
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         5241
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1265
_refine_ls_R_factor_gt           0.0724
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0781P)²+0.3922P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1726
_refine_ls_wR_factor_ref         0.2056
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C3(H3), C2(H2)
2.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C11(H11A,H11B,H11C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C15(H15A,H15B,H15C), C24(H24A,H24B,H24C), C17(H17A,H17B,H17C), C18(H18A,
 H18B,H18C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O13 O 0.78266(18) 0.79837(16) 0.50310(16) 0.0568(5) Uani 1 1 d . . . . .
O12 O 0.8142(2) 0.58139(16) 0.54552(15) 0.0589(5) Uani 1 1 d . . . . .
C10 C 0.9695(2) 0.7219(2) 0.36903(19) 0.0423(5) Uani 1 1 d . . . . .
H10 H 1.0215 0.6383 0.3786 0.051 Uiso 1 1 calc R . . . .
O22 O 0.8734(2) 0.89006(19) 0.16884(17) 0.0742(6) Uani 1 1 d . . . . .
C4 C 1.1287(2) 0.7909(2) 0.5013(2) 0.0422(5) Uani 1 1 d . . . . .
C5 C 1.1563(3) 0.6642(2) 0.5803(2) 0.0521(6) Uani 1 1 d . . . . .
H5 H 1.1420 0.5949 0.5545 0.062 Uiso 1 1 calc R . . . .
C9 C 1.0720(3) 0.8183(2) 0.3758(2) 0.0491(6) Uani 1 1 d . . . . .
H9A H 1.1492 0.8178 0.3178 0.059 Uiso 1 1 calc R . . . .
H9B H 1.0259 0.9050 0.3495 0.059 Uiso 1 1 calc R . . . .
C6 C 1.2046(3) 0.6399(3) 0.6962(2) 0.0561(7) Uani 1 1 d . . . . .
H6 H 1.2222 0.5546 0.7480 0.067 Uiso 1 1 calc R . . . .
O21 O 0.8330(3) 0.68210(19) 0.20587(18) 0.0836(7) Uani 1 1 d . . . . .
C3 C 1.1542(3) 0.8910(2) 0.5425(2) 0.0529(6) Uani 1 1 d . . . . .
H3 H 1.1383 0.9764 0.4903 0.063 Uiso 1 1 calc R . . . .
C1 C 1.2270(2) 0.7416(3) 0.7358(2) 0.0529(6) Uani 1 1 d . . . . .
B11 B 0.8547(3) 0.6993(2) 0.4747(2) 0.0399(6) Uani 1 1 d . . . . .
C2 C 1.2020(3) 0.8685(3) 0.6577(3) 0.0590(7) Uani 1 1 d . . . . .
H2 H 1.2175 0.9378 0.6831 0.071 Uiso 1 1 calc R . . . .
B20 B 0.8927(3) 0.7653(3) 0.2453(2) 0.0450(6) Uani 1 1 d . . . . .
C7 C 1.2785(3) 0.7153(3) 0.8564(3) 0.0706(8) Uani 1 1 d . . . . .
C16 C 0.7193(3) 0.6001(3) 0.6426(2) 0.0646(8) Uani 1 1 d . . . . .
C8 C 0.6672(3) 0.7433(3) 0.5868(2) 0.0632(7) Uani 1 1 d . . . . .
N8 N 1.3208(4) 0.6943(4) 0.9511(3) 0.1080(11) Uani 1 1 d . . . . .
C19 C 0.7710(4) 0.8910(3) 0.0809(3) 0.0888(11) Uani 1 1 d . . . . .
C23 C 0.7878(4) 0.7557(4) 0.0805(3) 0.0952(12) Uani 1 1 d . . . . .
C25 C 0.6687(4) 0.6930(4) 0.0541(3) 0.0995(12) Uani 1 1 d . . . . .
H25A H 0.7005 0.6096 0.0486 0.149 Uiso 1 1 calc GR . . . .
H25B H 0.6300 0.7471 -0.0225 0.149 Uiso 1 1 calc GR . . . .
H25C H 0.5992 0.6820 0.1194 0.149 Uiso 1 1 calc GR . . . .
C11 C 0.8084(4) 0.5756(4) 0.7551(3) 0.1038(14) Uani 1 1 d . . . . .
H11A H 0.8598 0.4927 0.7730 0.156 Uiso 1 1 calc GR . . . .
H11B H 0.7493 0.5761 0.8251 0.156 Uiso 1 1 calc GR . . . .
H11C H 0.8716 0.6428 0.7373 0.156 Uiso 1 1 calc GR . . . .
C26 C 0.7883(4) 1.0017(4) -0.0352(3) 0.0937(11) Uani 1 1 d . . . . .
H26A H 0.7685 1.0819 -0.0192 0.141 Uiso 1 1 calc GR . . . .
H26B H 0.7257 0.9973 -0.0945 0.141 Uiso 1 1 calc GR . . . .
H26C H 0.8820 0.9976 -0.0672 0.141 Uiso 1 1 calc GR . . . .
C27 C 0.6206(4) 0.9083(5) 0.1434(4) 0.1309(19) Uani 1 1 d . . . . .
H27A H 0.6041 0.8313 0.2124 0.196 Uiso 1 1 calc GR . . . .
H27B H 0.5509 0.9223 0.0840 0.196 Uiso 1 1 calc GR . . . .
H27C H 0.6171 0.9817 0.1712 0.196 Uiso 1 1 calc GR . . . .
C15 C 0.6371(4) 0.8167(4) 0.6755(3) 0.0988(12) Uani 1 1 d . . . . .
H15A H 0.7210 0.8195 0.7140 0.148 Uiso 1 1 calc GR . . . .
H15B H 0.5699 0.7736 0.7374 0.148 Uiso 1 1 calc GR . . . .
H15C H 0.6012 0.9036 0.6316 0.148 Uiso 1 1 calc GR . . . .
C24 C 0.9173(5) 0.7504(5) -0.0138(3) 0.1318(19) Uani 1 1 d . . . . .
H24A H 0.9910 0.7961 0.0002 0.198 Uiso 1 1 calc GR . . . .
H24B H 0.8885 0.7906 -0.0971 0.198 Uiso 1 1 calc GR . . . .
H24C H 0.9494 0.6615 -0.0005 0.198 Uiso 1 1 calc GR . . . .
C17 C 0.5435(3) 0.7616(5) 0.5047(3) 0.1091(14) Uani 1 1 d . . . . .
H17A H 0.5327 0.8506 0.4517 0.164 Uiso 1 1 calc GR . . . .
H17B H 0.4607 0.7393 0.5555 0.164 Uiso 1 1 calc GR . . . .
H17C H 0.5596 0.7062 0.4555 0.164 Uiso 1 1 calc GR . . . .
C18 C 0.6127(5) 0.5016(4) 0.6746(4) 0.1226(16) Uani 1 1 d . . . . .
H18A H 0.5659 0.5084 0.6017 0.184 Uiso 1 1 calc GR . . . .
H18B H 0.5466 0.5173 0.7345 0.184 Uiso 1 1 calc GR . . . .
H18C H 0.6574 0.4158 0.7081 0.184 Uiso 1 1 calc GR . . . .


_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
O13 B11 1.360(3) . ?
O13 C8 1.459(3) . ?
O12 B11 1.350(3) . ?
O12 C16 1.459(3) . ?
C10 C9 1.539(3) . ?
C10 B11 1.565(3) . ?
C10 B20 1.560(3) . ?
O22 B20 1.356(3) . ?
O22 C19 1.463(3) . ?
C4 C5 1.391(3) . ?
C4 C9 1.507(3) . ?
C4 C3 1.383(3) . ?
C5 C6 1.378(3) . ?
C6 C1 1.380(4) . ?
O21 B20 1.337(3) . ?
O21 C23 1.470(3) . ?
C3 C2 1.372(3) . ?
C1 C2 1.385(4) . ?
C1 C7 1.436(4) . ?
C7 N8 1.135(4) . ?
C16 C8 1.531(4) . ?
C16 C11 1.541(5) . ?
C16 C18 1.499(5) . ?
C8 C15 1.504(4) . ?
C8 C17 1.535(5) . ?
C19 C23 1.480(5) . ?
C19 C26 1.481(4) . ?
C19 C27 1.607(5) . ?
C23 C25 1.493(5) . ?
C23 C24 1.616(6) . ?

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
B11 O13 C8 107.33(19) . . ?
B11 O12 C16 107.57(19) . . ?
C9 C10 B11 111.70(18) . . ?
C9 C10 B20 113.99(19) . . ?
B20 C10 B11 106.66(18) . . ?
B20 O22 C19 106.6(2) . . ?
C5 C4 C9 121.3(2) . . ?
C3 C4 C5 117.6(2) . . ?
C3 C4 C9 121.1(2) . . ?
C6 C5 C4 121.0(2) . . ?
C4 C9 C10 115.00(19) . . ?
C5 C6 C1 120.3(2) . . ?
B20 O21 C23 106.7(2) . . ?
C2 C3 C4 122.2(2) . . ?
C6 C1 C2 119.6(2) . . ?
C6 C1 C7 119.8(3) . . ?
C2 C1 C7 120.6(3) . . ?
O13 B11 C10 123.0(2) . . ?
O12 B11 O13 112.7(2) . . ?
O12 B11 C10 124.3(2) . . ?
C3 C2 C1 119.4(2) . . ?
O22 B20 C10 124.7(2) . . ?
O21 B20 C10 122.8(2) . . ?
O21 B20 O22 112.4(2) . . ?
N8 C7 C1 179.1(3) . . ?
O12 C16 C8 102.47(19) . . ?
O12 C16 C11 105.9(2) . . ?
O12 C16 C18 109.4(3) . . ?
C8 C16 C11 112.0(3) . . ?
C18 C16 C8 117.0(3) . . ?
C18 C16 C11 109.2(3) . . ?
O13 C8 C16 102.2(2) . . ?
O13 C8 C15 109.2(3) . . ?
O13 C8 C17 105.7(2) . . ?
C16 C8 C17 112.1(3) . . ?
C15 C8 C16 116.4(3) . . ?
C15 C8 C17 110.4(3) . . ?
O22 C19 C23 102.4(3) . . ?
O22 C19 C26 110.2(3) . . ?
O22 C19 C27 106.9(3) . . ?
C23 C19 C26 120.5(3) . . ?
C23 C19 C27 106.7(3) . . ?
C26 C19 C27 109.3(3) . . ?
O21 C23 C19 102.6(3) . . ?
O21 C23 C25 108.9(3) . . ?
O21 C23 C24 107.5(3) . . ?
C19 C23 C25 120.7(4) . . ?
C19 C23 C24 106.2(3) . . ?
C25 C23 C24 110.1(3) . . ?

_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.769
_oxdiff_exptl_absorpt_empirical_full_min 0.695
####################################################################### 
# 
# 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_exp_4142
_database_code_depnum_ccdc_archive 'CCDC 1570208'
_audit_update_record             
;
2017-08-22 deposited with the CCDC.
2018-06-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H84 B4 N0 O10'
_chemical_formula_weight         1008.51

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.0513(14)
_cell_length_b                   15.5408(16)
_cell_length_c                   19.0622(18)
_cell_angle_alpha                88.904(8)
_cell_angle_beta                 83.300(10)
_cell_angle_gamma                87.795(10)
_cell_volume                     2954.8(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4291
_cell_measurement_theta_min      0.66044
_cell_measurement_theta_max      1.00000

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1088
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9919
_exptl_absorpt_correction_T_max  0.9941
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'four-circle diffractometer'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            24617
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0871
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         29.45
_reflns_number_total             13325
_reflns_number_gt                5997
_reflns_threshold_expression     >2sigma(I)

_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_special_details          
; Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1730P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         13325
_refine_ls_number_parameters     683
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1816
_refine_ls_R_factor_gt           0.0933
_refine_ls_wR_factor_ref         0.3251
_refine_ls_wR_factor_gt          0.2566
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O2 O 0.6015(2) 0.16206(15) 0.84284(12) 0.0648(7) Uani 1 1 d . . .
O5 O 0.5205(2) 0.13155(14) 0.66714(13) 0.0666(7) Uani 1 1 d . . .
O3 O 0.7373(2) 0.23939(14) 0.76501(13) 0.0652(7) Uani 1 1 d . . .
O7 O 0.9761(3) 0.36939(14) 0.33308(13) 0.0706(7) Uani 1 1 d . . .
O10 O 0.8449(2) 0.31930(16) 0.15234(13) 0.0730(7) Uani 1 1 d . . .
O9 O 0.7321(2) 0.25012(16) 0.24368(12) 0.0678(7) Uani 1 1 d . . .
O6 O 0.9519(2) 0.12595(17) 0.14223(14) 0.0777(8) Uani 1 1 d . . .
O4 O 0.3164(2) 0.13870(14) 0.72896(15) 0.0812(9) Uani 1 1 d . . .
O8 O 1.1103(3) 0.39597(14) 0.23396(13) 0.0819(9) Uani 1 1 d . . .
O1 O 0.5258(3) 0.36139(19) 0.86491(16) 0.0903(9) Uani 1 1 d . . .
C9 C 0.4799(3) 0.25514(16) 0.75525(14) 0.0394(7) Uani 1 1 d . . .
C42 C 0.9937(3) 0.25115(16) 0.24041(14) 0.0390(6) Uani 1 1 d . . .
C8 C 0.3681(3) 0.28244(17) 0.81324(15) 0.0432(7) Uani 1 1 d . . .
H8A H 0.2971 0.3125 0.7912 0.052 Uiso 1 1 calc R . .
H8B H 0.3309 0.2310 0.8362 0.052 Uiso 1 1 calc R . .
C43 C 1.0991(3) 0.22655(17) 0.17803(15) 0.0450(7) Uani 1 1 d . . .
H43A H 1.1219 0.2784 0.1508 0.054 Uiso 1 1 calc R . .
H43B H 1.1797 0.2048 0.1969 0.054 Uiso 1 1 calc R . .
C44 C 1.0583(3) 0.16105(17) 0.12913(16) 0.0467(7) Uani 1 1 d . . .
C41 C 0.9812(3) 0.18096(17) 0.29999(15) 0.0446(7) Uani 1 1 d . . .
H41A H 0.9142 0.2008 0.3375 0.053 Uiso 1 1 calc R . .
H41B H 0.9490 0.1292 0.2811 0.053 Uiso 1 1 calc R . .
C45 C 1.1492(3) 0.13970(17) 0.06395(15) 0.0459(7) Uani 1 1 d . . .
C10 C 0.5173(3) 0.32728(18) 0.69993(16) 0.0462(7) Uani 1 1 d . . .
H10A H 0.5605 0.3720 0.7228 0.055 Uiso 1 1 calc R . .
H10B H 0.5826 0.3034 0.6633 0.055 Uiso 1 1 calc R . .
C7 C 0.4110(3) 0.33896(18) 0.86848(18) 0.0515(8) Uani 1 1 d . . .
C1 C 0.3109(3) 0.36564(17) 0.92888(17) 0.0507(8) Uani 1 1 d . . .
C46 C 1.0977(4) 0.09708(19) 0.01045(17) 0.0589(9) Uani 1 1 d . . .
H46 H 1.0076 0.0838 0.0155 0.071 Uiso 1 1 calc R . .
C33 C 1.0239(3) 0.1431(2) 0.46288(18) 0.0556(9) Uani 1 1 d . . .
C11 C 0.4022(3) 0.3686(2) 0.66514(17) 0.0562(8) Uani 1 1 d . . .
H11A H 0.3450 0.4020 0.6999 0.067 Uiso 1 1 calc R . .
H11B H 0.3492 0.3237 0.6490 0.067 Uiso 1 1 calc R . .
B26 B 0.6097(4) 0.2216(2) 0.78900(17) 0.0431(8) Uani 1 1 d . . .
B19 B 0.4380(3) 0.1739(2) 0.71676(18) 0.0413(8) Uani 1 1 d . . .
C40 C 1.1099(3) 0.1577(2) 0.33172(17) 0.0587(9) Uani 1 1 d . . .
H40A H 1.1499 0.2103 0.3442 0.070 Uiso 1 1 calc R . .
H40B H 1.1724 0.1291 0.2963 0.070 Uiso 1 1 calc R . .
C13 C 0.5075(4) 0.3793(2) 0.53794(19) 0.0610(9) Uani 1 1 d . . .
B51 B 1.0283(3) 0.3392(2) 0.27022(18) 0.0422(8) Uani 1 1 d . . .
B58 B 0.8550(4) 0.2708(2) 0.21142(18) 0.0440(8) Uani 1 1 d . . .
C50 C 1.2811(4) 0.1616(2) 0.0534(2) 0.0679(10) Uani 1 1 d . . .
H50 H 1.3169 0.1919 0.0880 0.081 Uiso 1 1 calc R . .
C2 C 0.3563(4) 0.4065(2) 0.9853(2) 0.0728(11) Uani 1 1 d . . .
H2 H 0.4468 0.4175 0.9842 0.087 Uiso 1 1 calc R . .
C12 C 0.4488(4) 0.4276(2) 0.60218(19) 0.0672(10) Uani 1 1 d . . .
H12A H 0.3730 0.4633 0.5903 0.081 Uiso 1 1 calc R . .
H12B H 0.5153 0.4655 0.6160 0.081 Uiso 1 1 calc R . .
C47 C 1.1791(5) 0.0742(2) -0.05047(19) 0.0734(11) Uani 1 1 d . . .
H47 H 1.1442 0.0443 -0.0855 0.088 Uiso 1 1 calc R . .
C14 C 0.6423(4) 0.3708(3) 0.5169(2) 0.0803(12) Uani 1 1 d . . .
H14 H 0.7009 0.3969 0.5436 0.096 Uiso 1 1 calc R . .
C6 C 0.1769(4) 0.3493(2) 0.9330(2) 0.0717(10) Uani 1 1 d . . .
H6 H 0.1448 0.3215 0.8959 0.086 Uiso 1 1 calc R . .
C39 C 1.0897(4) 0.0993(2) 0.39731(19) 0.0683(10) Uani 1 1 d . . .
H39A H 1.0354 0.0519 0.3871 0.082 Uiso 1 1 calc R . .
H39B H 1.1763 0.0753 0.4068 0.082 Uiso 1 1 calc R . .
C48 C 1.3113(5) 0.0957(2) -0.0593(2) 0.0779(12) Uani 1 1 d . . .
H48 H 1.3661 0.0804 -0.1002 0.094 Uiso 1 1 calc R . .
C20 C 0.4449(4) 0.0672(2) 0.6373(2) 0.0695(10) Uani 1 1 d . . .
C34 C 1.0869(4) 0.2064(3) 0.4928(2) 0.0833(12) Uani 1 1 d . . .
H34 H 1.1701 0.2234 0.4717 0.100 Uiso 1 1 calc R . .
C49 C 1.3614(4) 0.1393(3) -0.0079(2) 0.0844(12) Uani 1 1 d . . .
H49 H 1.4506 0.1544 -0.0140 0.101 Uiso 1 1 calc R . .
C23 C 0.3262(4) 0.0569(2) 0.6914(2) 0.0845(13) Uani 1 1 d . . .
C55 C 1.0413(4) 0.4485(2) 0.3458(2) 0.0727(11) Uani 1 1 d . . .
C38 C 0.9039(4) 0.1191(3) 0.4972(3) 0.0863(13) Uani 1 1 d . . .
H38 H 0.8600 0.0744 0.4792 0.104 Uiso 1 1 calc R . .
C3 C 0.2667(7) 0.4310(3) 1.0435(2) 0.0977(15) Uani 1 1 d . . .
H3 H 0.2975 0.4588 1.0809 0.117 Uiso 1 1 calc R . .
C15 C 0.6946(5) 0.3259(3) 0.4588(3) 0.0937(14) Uani 1 1 d . . .
H15 H 0.7868 0.3223 0.4461 0.112 Uiso 1 1 calc R . .
C5 C 0.0881(5) 0.3732(3) 0.9914(3) 0.0932(14) Uani 1 1 d . . .
H5 H -0.0021 0.3611 0.9930 0.112 Uiso 1 1 calc R . .
C4 C 0.1324(6) 0.4141(3) 1.0458(3) 0.0963(15) Uani 1 1 d . . .
H4 H 0.0726 0.4307 1.0846 0.116 Uiso 1 1 calc R . .
C18 C 0.4264(5) 0.3406(3) 0.4972(2) 0.0953(14) Uani 1 1 d . . .
H18 H 0.3341 0.3446 0.5096 0.114 Uiso 1 1 calc R . .
C31 C 0.7501(5) 0.0930(3) 0.9176(2) 0.1023(16) Uani 1 1 d . . .
H31A H 0.7302 0.1362 0.9530 0.153 Uiso 1 1 calc R . .
H31B H 0.8400 0.0704 0.9189 0.153 Uiso 1 1 calc R . .
H31C H 0.6885 0.0473 0.9266 0.153 Uiso 1 1 calc R . .
C35 C 1.0298(6) 0.2460(3) 0.5537(3) 0.1062(16) Uani 1 1 d . . .
H35 H 1.0744 0.2896 0.5730 0.127 Uiso 1 1 calc R . .
C30 C 0.7374(4) 0.1303(4) 0.8498(2) 0.1063(17) Uani 1 1 d . . .
C36 C 0.9104(7) 0.2222(4) 0.5854(3) 0.1064(17) Uani 1 1 d . . .
H36 H 0.8722 0.2493 0.6264 0.128 Uiso 1 1 calc R . .
C52 C 1.0973(5) 0.4771(2) 0.2728(3) 0.0894(14) Uani 1 1 d . . .
C63 C 0.5017(4) 0.2702(3) 0.2254(3) 0.1072(16) Uani 1 1 d . . .
H63A H 0.4987 0.2092 0.2340 0.161 Uiso 1 1 calc R . .
H63B H 0.4455 0.2864 0.1896 0.161 Uiso 1 1 calc R . .
H63C H 0.4705 0.2999 0.2682 0.161 Uiso 1 1 calc R . .
C16 C 0.6107(6) 0.2860(4) 0.4193(3) 0.1063(16) Uani 1 1 d . . .
H16 H 0.6446 0.2532 0.3805 0.128 Uiso 1 1 calc R . .
C27 C 0.8226(4) 0.1949(3) 0.8130(3) 0.1067(19) Uani 1 1 d . . .
C60 C 0.7040(5) 0.3285(4) 0.1432(3) 0.116(2) Uani 1 1 d . . .
C37 C 0.8458(5) 0.1589(4) 0.5577(3) 0.1050(15) Uani 1 1 d . . .
H37 H 0.7627 0.1423 0.5793 0.126 Uiso 1 1 calc R . .
C25 C 0.1931(5) 0.0417(4) 0.6639(4) 0.171(3) Uani 1 1 d . . .
H25A H 0.1250 0.0343 0.7030 0.256 Uiso 1 1 calc R . .
H25B H 0.2014 -0.0091 0.6356 0.256 Uiso 1 1 calc R . .
H25C H 0.1689 0.0904 0.6357 0.256 Uiso 1 1 calc R . .
C17 C 0.4770(6) 0.2956(4) 0.4381(3) 0.123(2) Uani 1 1 d . . .
H17 H 0.4183 0.2713 0.4105 0.148 Uiso 1 1 calc R . .
C22 C 0.5303(5) -0.0105(3) 0.6189(4) 0.140(3) Uani 1 1 d . . .
H22A H 0.5997 0.0035 0.5819 0.210 Uiso 1 1 calc R . .
H22B H 0.4766 -0.0544 0.6031 0.210 Uiso 1 1 calc R . .
H22C H 0.5700 -0.0311 0.6598 0.210 Uiso 1 1 calc R . .
C54 C 1.2224(6) 0.5226(3) 0.2593(3) 0.138(2) Uani 1 1 d . . .
H54A H 1.2945 0.4872 0.2743 0.207 Uiso 1 1 calc R . .
H54B H 1.2144 0.5755 0.2849 0.207 Uiso 1 1 calc R . .
H54C H 1.2406 0.5350 0.2096 0.207 Uiso 1 1 calc R . .
C29 C 0.9600(4) 0.1905(4) 0.7818(3) 0.125(2) Uani 1 1 d . . .
H29A H 0.9679 0.1553 0.7406 0.188 Uiso 1 1 calc R . .
H29B H 1.0153 0.1659 0.8153 0.188 Uiso 1 1 calc R . .
H29C H 0.9885 0.2475 0.7686 0.188 Uiso 1 1 calc R . .
C62 C 0.6353(4) 0.2924(5) 0.2025(3) 0.147(3) Uani 1 1 d . . .
C28 C 0.8245(6) 0.2644(3) 0.8801(3) 0.143(3) Uani 1 1 d . . .
H28A H 0.8279 0.3223 0.8616 0.214 Uiso 1 1 calc R . .
H28B H 0.9019 0.2517 0.9041 0.214 Uiso 1 1 calc R . .
H28C H 0.7449 0.2587 0.9126 0.214 Uiso 1 1 calc R . .
C61 C 0.6791(6) 0.3808(5) 0.0868(3) 0.168(3) Uani 1 1 d . . .
H61A H 0.7167 0.4359 0.0917 0.253 Uiso 1 1 calc R . .
H61B H 0.5841 0.3880 0.0857 0.253 Uiso 1 1 calc R . .
H61C H 0.7191 0.3549 0.0437 0.253 Uiso 1 1 calc R . .
C21 C 0.4039(7) 0.1100(4) 0.5683(3) 0.150(3) Uani 1 1 d . . .
H21A H 0.3354 0.1538 0.5799 0.225 Uiso 1 1 calc R . .
H21B H 0.3704 0.0672 0.5400 0.225 Uiso 1 1 calc R . .
H21C H 0.4806 0.1354 0.5424 0.225 Uiso 1 1 calc R . .
C53 C 0.9853(7) 0.5330(3) 0.2383(4) 0.158(3) Uani 1 1 d . . .
H53A H 0.9966 0.5252 0.1881 0.236 Uiso 1 1 calc R . .
H53B H 0.9937 0.5927 0.2484 0.236 Uiso 1 1 calc R . .
H53C H 0.8982 0.5149 0.2576 0.236 Uiso 1 1 calc R . .
C57 C 0.9475(7) 0.5071(4) 0.3872(4) 0.176(4) Uani 1 1 d . . .
H57A H 0.8668 0.5144 0.3649 0.264 Uiso 1 1 calc R . .
H57B H 0.9873 0.5619 0.3899 0.264 Uiso 1 1 calc R . .
H57C H 0.9266 0.4836 0.4339 0.264 Uiso 1 1 calc R . .
C24 C 0.3483(9) -0.0112(3) 0.7476(3) 0.184(4) Uani 1 1 d . . .
H24A H 0.4388 -0.0098 0.7588 0.276 Uiso 1 1 calc R . .
H24B H 0.3327 -0.0670 0.7301 0.276 Uiso 1 1 calc R . .
H24C H 0.2874 0.0001 0.7893 0.276 Uiso 1 1 calc R . .
C32 C 0.7739(9) 0.0520(4) 0.7892(4) 0.236(6) Uani 1 1 d . . .
H32A H 0.6937 0.0227 0.7831 0.354 Uiso 1 1 calc R . .
H32B H 0.8389 0.0116 0.8052 0.354 Uiso 1 1 calc R . .
H32C H 0.8096 0.0773 0.7450 0.354 Uiso 1 1 calc R . .
C56 C 1.1573(8) 0.4210(4) 0.3890(4) 0.193(4) Uani 1 1 d . . .
H56A H 1.1297 0.3747 0.4208 0.290 Uiso 1 1 calc R . .
H56B H 1.1803 0.4691 0.4155 0.290 Uiso 1 1 calc R . .
H56C H 1.2340 0.4022 0.3575 0.290 Uiso 1 1 calc R . .
C64 C 0.6355(8) 0.4120(5) 0.2271(6) 0.281(7) Uani 1 1 d . . .
H64A H 0.5479 0.4300 0.2485 0.421 Uiso 1 1 calc R . .
H64B H 0.6589 0.4460 0.1853 0.421 Uiso 1 1 calc R . .
H64C H 0.6997 0.4195 0.2598 0.421 Uiso 1 1 calc R . .
C59 C 0.6639(8) 0.2138(6) 0.1125(5) 0.291(7) Uani 1 1 d . . .
H59A H 0.7377 0.1917 0.0805 0.436 Uiso 1 1 calc R . .
H59B H 0.5844 0.2175 0.0890 0.436 Uiso 1 1 calc R . .
H59C H 0.6499 0.1760 0.1528 0.436 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O2 B26 1.366(4) . ?
O2 C30 1.454(5) . ?
O5 B19 1.347(4) . ?
O5 C20 1.443(4) . ?
O3 B26 1.348(4) . ?
O3 C27 1.470(4) . ?
O7 B51 1.337(4) . ?
O7 C55 1.453(4) . ?
O10 B58 1.354(4) . ?
O10 C60 1.449(5) . ?
O9 B58 1.361(4) . ?
O9 C62 1.451(4) . ?
O6 C44 1.217(4) . ?
O4 B19 1.352(4) . ?
O4 C23 1.465(4) . ?
O8 B51 1.355(4) . ?
O8 C52 1.468(4) . ?
O1 C7 1.213(4) . ?
C9 C8 1.535(4) . ?
C9 C10 1.551(4) . ?
C9 B19 1.568(4) . ?
C9 B26 1.587(4) . ?
C42 C43 1.541(4) . ?
C42 C41 1.557(4) . ?
C42 B51 1.558(4) . ?
C42 B58 1.576(4) . ?
C8 C7 1.495(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C43 C44 1.494(4) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 C45 1.489(4) . ?
C41 C40 1.518(4) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C45 C50 1.372(4) . ?
C45 C46 1.387(4) . ?
C10 C11 1.515(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C7 C1 1.492(4) . ?
C1 C6 1.374(5) . ?
C1 C2 1.390(4) . ?
C46 C47 1.384(5) . ?
C46 H46 0.9300 . ?
C33 C34 1.360(5) . ?
C33 C38 1.365(5) . ?
C33 C39 1.505(5) . ?
C11 C12 1.536(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C40 C39 1.529(4) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C13 C18 1.353(5) . ?
C13 C14 1.369(5) . ?
C13 C12 1.499(5) . ?
C50 C49 1.383(5) . ?
C50 H50 0.9300 . ?
C2 C3 1.394(6) . ?
C2 H2 0.9300 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C47 C48 1.373(6) . ?
C47 H47 0.9300 . ?
C14 C15 1.362(6) . ?
C14 H14 0.9300 . ?
C6 C5 1.390(5) . ?
C6 H6 0.9300 . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C48 C49 1.356(5) . ?
C48 H48 0.9300 . ?
C20 C22 1.479(6) . ?
C20 C23 1.495(6) . ?
C20 C21 1.553(7) . ?
C34 C35 1.379(6) . ?
C34 H34 0.9300 . ?
C49 H49 0.9300 . ?
C23 C24 1.520(7) . ?
C23 C25 1.521(7) . ?
C55 C57 1.459(6) . ?
C55 C52 1.503(6) . ?
C55 C56 1.548(7) . ?
C38 C37 1.377(6) . ?
C38 H38 0.9300 . ?
C3 C4 1.380(7) . ?
C3 H3 0.9300 . ?
C15 C16 1.367(7) . ?
C15 H15 0.9300 . ?
C5 C4 1.354(6) . ?
C5 H5 0.9300 . ?
C4 H4 0.9300 . ?
C18 C17 1.373(7) . ?
C18 H18 0.9300 . ?
C31 C30 1.423(5) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C35 C36 1.342(7) . ?
C35 H35 0.9300 . ?
C30 C27 1.461(6) . ?
C30 C32 1.694(7) . ?
C36 C37 1.347(7) . ?
C36 H36 0.9300 . ?
C52 C54 1.461(6) . ?
C52 C53 1.591(7) . ?
C63 C62 1.416(6) . ?
C63 H63A 0.9600 . ?
C63 H63B 0.9600 . ?
C63 H63C 0.9600 . ?
C16 C17 1.353(7) . ?
C16 H16 0.9300 . ?
C27 C29 1.438(6) . ?
C27 C28 1.692(7) . ?
C60 C61 1.375(6) . ?
C60 C62 1.376(6) . ?
C60 C59 1.957(9) . ?
C37 H37 0.9300 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C17 H17 0.9300 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C62 C64 1.925(10) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C61 H61A 0.9600 . ?
C61 H61B 0.9600 . ?
C61 H61C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C57 H57A 0.9600 . ?
C57 H57B 0.9600 . ?
C57 H57C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C59 H59A 0.9600 . ?
C59 H59B 0.9600 . ?
C59 H59C 0.9600 . ?

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
B26 O2 C30 107.1(3) . . ?
B19 O5 C20 108.2(3) . . ?
B26 O3 C27 106.6(3) . . ?
B51 O7 C55 108.5(3) . . ?
B58 O10 C60 107.5(3) . . ?
B58 O9 C62 106.0(3) . . ?
B19 O4 C23 106.8(3) . . ?
B51 O8 C52 107.7(3) . . ?
C8 C9 C10 113.6(2) . . ?
C8 C9 B19 109.8(2) . . ?
C10 C9 B19 109.4(2) . . ?
C8 C9 B26 110.5(2) . . ?
C10 C9 B26 109.8(2) . . ?
B19 C9 B26 103.2(2) . . ?
C43 C42 C41 112.9(2) . . ?
C43 C42 B51 109.3(2) . . ?
C41 C42 B51 110.7(2) . . ?
C43 C42 B58 108.8(2) . . ?
C41 C42 B58 111.2(2) . . ?
B51 C42 B58 103.6(2) . . ?
C7 C8 C9 114.9(2) . . ?
C7 C8 H8A 108.5 . . ?
C9 C8 H8A 108.5 . . ?
C7 C8 H8B 108.5 . . ?
C9 C8 H8B 108.5 . . ?
H8A C8 H8B 107.5 . . ?
C44 C43 C42 115.7(2) . . ?
C44 C43 H43A 108.4 . . ?
C42 C43 H43A 108.4 . . ?
C44 C43 H43B 108.4 . . ?
C42 C43 H43B 108.4 . . ?
H43A C43 H43B 107.4 . . ?
O6 C44 C45 120.5(3) . . ?
O6 C44 C43 120.5(3) . . ?
C45 C44 C43 119.0(2) . . ?
C40 C41 C42 115.2(2) . . ?
C40 C41 H41A 108.5 . . ?
C42 C41 H41A 108.5 . . ?
C40 C41 H41B 108.5 . . ?
C42 C41 H41B 108.5 . . ?
H41A C41 H41B 107.5 . . ?
C50 C45 C46 118.2(3) . . ?
C50 C45 C44 123.3(3) . . ?
C46 C45 C44 118.5(3) . . ?
C11 C10 C9 116.0(2) . . ?
C11 C10 H10A 108.3 . . ?
C9 C10 H10A 108.3 . . ?
C11 C10 H10B 108.3 . . ?
C9 C10 H10B 108.3 . . ?
H10A C10 H10B 107.4 . . ?
O1 C7 C1 120.6(3) . . ?
O1 C7 C8 120.5(3) . . ?
C1 C7 C8 118.9(3) . . ?
C6 C1 C2 118.1(3) . . ?
C6 C1 C7 123.5(3) . . ?
C2 C1 C7 118.3(3) . . ?
C47 C46 C45 120.6(3) . . ?
C47 C46 H46 119.7 . . ?
C45 C46 H46 119.7 . . ?
C34 C33 C38 116.8(4) . . ?
C34 C33 C39 120.3(3) . . ?
C38 C33 C39 122.8(4) . . ?
C10 C11 C12 113.1(3) . . ?
C10 C11 H11A 109.0 . . ?
C12 C11 H11A 109.0 . . ?
C10 C11 H11B 109.0 . . ?
C12 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
O3 B26 O2 112.6(3) . . ?
O3 B26 C9 126.0(3) . . ?
O2 B26 C9 121.1(3) . . ?
O5 B19 O4 112.5(3) . . ?
O5 B19 C9 123.1(3) . . ?
O4 B19 C9 124.4(3) . . ?
C41 C40 C39 113.7(3) . . ?
C41 C40 H40A 108.8 . . ?
C39 C40 H40A 108.8 . . ?
C41 C40 H40B 108.8 . . ?
C39 C40 H40B 108.8 . . ?
H40A C40 H40B 107.7 . . ?
C18 C13 C14 116.3(4) . . ?
C18 C13 C12 120.2(4) . . ?
C14 C13 C12 123.6(4) . . ?
O7 B51 O8 112.0(3) . . ?
O7 B51 C42 124.2(3) . . ?
O8 B51 C42 123.8(3) . . ?
O10 B58 O9 111.4(3) . . ?
O10 B58 C42 121.9(3) . . ?
O9 B58 C42 126.4(3) . . ?
C45 C50 C49 120.8(3) . . ?
C45 C50 H50 119.6 . . ?
C49 C50 H50 119.6 . . ?
C1 C2 C3 120.2(4) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 H2 119.9 . . ?
C13 C12 C11 113.3(3) . . ?
C13 C12 H12A 108.9 . . ?
C11 C12 H12A 108.9 . . ?
C13 C12 H12B 108.9 . . ?
C11 C12 H12B 108.9 . . ?
H12A C12 H12B 107.7 . . ?
C48 C47 C46 120.2(3) . . ?
C48 C47 H47 119.9 . . ?
C46 C47 H47 119.9 . . ?
C15 C14 C13 123.0(4) . . ?
C15 C14 H14 118.5 . . ?
C13 C14 H14 118.5 . . ?
C1 C6 C5 121.4(4) . . ?
C1 C6 H6 119.3 . . ?
C5 C6 H6 119.3 . . ?
C33 C39 C40 114.8(3) . . ?
C33 C39 H39A 108.6 . . ?
C40 C39 H39A 108.6 . . ?
C33 C39 H39B 108.6 . . ?
C40 C39 H39B 108.6 . . ?
H39A C39 H39B 107.5 . . ?
C49 C48 C47 119.5(4) . . ?
C49 C48 H48 120.2 . . ?
C47 C48 H48 120.2 . . ?
O5 C20 C22 110.6(3) . . ?
O5 C20 C23 103.4(3) . . ?
C22 C20 C23 117.3(4) . . ?
O5 C20 C21 104.3(3) . . ?
C22 C20 C21 108.9(5) . . ?
C23 C20 C21 111.5(4) . . ?
C33 C34 C35 121.3(4) . . ?
C33 C34 H34 119.4 . . ?
C35 C34 H34 119.4 . . ?
C48 C49 C50 120.7(4) . . ?
C48 C49 H49 119.6 . . ?
C50 C49 H49 119.6 . . ?
O4 C23 C20 103.3(3) . . ?
O4 C23 C24 104.8(4) . . ?
C20 C23 C24 113.6(5) . . ?
O4 C23 C25 109.1(4) . . ?
C20 C23 C25 116.7(4) . . ?
C24 C23 C25 108.4(5) . . ?
O7 C55 C57 110.1(4) . . ?
O7 C55 C52 103.1(3) . . ?
C57 C55 C52 118.1(5) . . ?
O7 C55 C56 105.4(3) . . ?
C57 C55 C56 109.6(5) . . ?
C52 C55 C56 109.7(5) . . ?
C33 C38 C37 122.2(4) . . ?
C33 C38 H38 118.9 . . ?
C37 C38 H38 118.9 . . ?
C4 C3 C2 120.3(4) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C14 C15 C16 119.6(5) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C4 C5 C6 120.3(5) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C5 C4 C3 119.6(4) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C13 C18 C17 121.6(5) . . ?
C13 C18 H18 119.2 . . ?
C17 C18 H18 119.2 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C36 C35 C34 120.5(5) . . ?
C36 C35 H35 119.8 . . ?
C34 C35 H35 119.8 . . ?
C31 C30 O2 112.5(4) . . ?
C31 C30 C27 126.7(4) . . ?
O2 C30 C27 104.4(3) . . ?
C31 C30 C32 107.8(5) . . ?
O2 C30 C32 106.7(4) . . ?
C27 C30 C32 96.4(5) . . ?
C35 C36 C37 119.9(5) . . ?
C35 C36 H36 120.1 . . ?
C37 C36 H36 120.1 . . ?
C54 C52 O8 109.3(4) . . ?
C54 C52 C55 122.4(4) . . ?
O8 C52 C55 102.5(3) . . ?
C54 C52 C53 107.4(5) . . ?
O8 C52 C53 105.0(4) . . ?
C55 C52 C53 109.0(4) . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C17 C16 C15 118.2(5) . . ?
C17 C16 H16 120.9 . . ?
C15 C16 H16 120.9 . . ?
C29 C27 C30 131.8(5) . . ?
C29 C27 O3 110.6(4) . . ?
C30 C27 O3 104.7(3) . . ?
C29 C27 C28 103.3(5) . . ?
C30 C27 C28 98.8(5) . . ?
O3 C27 C28 104.1(3) . . ?
C61 C60 C62 139.1(5) . . ?
C61 C60 O10 113.4(4) . . ?
C62 C60 O10 106.3(3) . . ?
C61 C60 C59 103.3(5) . . ?
C62 C60 C59 76.4(6) . . ?
O10 C60 C59 102.7(4) . . ?
C36 C37 C38 119.4(5) . . ?
C36 C37 H37 120.3 . . ?
C38 C37 H37 120.3 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C16 C17 C18 121.2(5) . . ?
C16 C17 H17 119.4 . . ?
C18 C17 H17 119.4 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C52 C54 H54A 109.5 . . ?
C52 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C52 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 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 . . ?
C60 C62 C63 137.2(4) . . ?
C60 C62 O9 108.2(3) . . ?
C63 C62 O9 112.9(4) . . ?
C60 C62 C64 77.7(6) . . ?
C63 C62 C64 102.6(5) . . ?
O9 C62 C64 104.6(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 . . ?
C60 C61 H61A 109.5 . . ?
C60 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C60 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C55 C57 H57A 109.5 . . ?
C55 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C55 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C62 C64 H64A 109.5 . . ?
C62 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C62 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C60 C59 H59A 109.5 . . ?
C60 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C60 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.813
_diffrn_reflns_theta_full        29.45
_diffrn_measured_fraction_theta_full 0.813
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.048
