# Electronic Supplementary Material (ESI) for Chemical Science.
# 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_1a
_database_code_depnum_ccdc_archive 'CCDC 1583775'
_audit_update_record             
;
2017-11-03 deposited with the CCDC.
2018-03-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H19 B10 N'
_chemical_formula_weight         249.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.3461(17)
_cell_length_b                   7.8073(19)
_cell_length_c                   12.765(3)
_cell_angle_alpha                81.469(4)
_cell_angle_beta                 78.051(4)
_cell_angle_gamma                86.599(4)
_cell_volume                     708.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2763
_cell_measurement_theta_min      0.994
_cell_measurement_theta_max      25.990

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             260
_exptl_absorpt_coefficient_mu    0.057
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5162
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0698
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.65
_diffrn_reflns_theta_max         25.99
_reflns_number_total             2763
_reflns_number_gt                1768
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0973P)²+0.0407P] 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         2763
_refine_ls_number_parameters     189
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0607
_refine_ls_wR_factor_ref         0.1751
_refine_ls_wR_factor_gt          0.1541
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_restrained_S_all      0.990
_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
C2 C 0.2186(3) 0.7689(3) 0.22318(16) 0.0207(5) Uani 1 1 d . . .
C13 C 0.1251(3) 0.9315(3) 0.17632(17) 0.0214(5) Uani 1 1 d . . .
C1 C 0.3092(3) 0.7701(3) 0.33608(17) 0.0234(5) Uani 1 1 d . . .
C18 C 0.2111(3) 1.0219(3) 0.07901(18) 0.0272(5) Uani 1 1 d . . .
H18 H 0.3268 0.9832 0.0441 0.033 Uiso 1 1 calc R . .
B9 B 0.1887(4) 0.4388(3) 0.3410(2) 0.0286(6) Uani 1 1 d . . .
H9 H 0.1006 0.3304 0.3830 0.034 Uiso 1 1 calc R . .
B12 B 0.3410(4) 0.4273(3) 0.2145(2) 0.0299(6) Uani 1 1 d . . .
H12 H 0.3527 0.3109 0.1741 0.036 Uiso 1 1 calc R . .
B4 B 0.2919(4) 0.5723(3) 0.4123(2) 0.0279(6) Uani 1 1 d . . .
H4 H 0.2704 0.5520 0.5011 0.034 Uiso 1 1 calc R . .
C14 C -0.0485(3) 0.9910(3) 0.22757(19) 0.0307(6) Uani 1 1 d . . .
H14 H -0.1090 0.9308 0.2927 0.037 Uiso 1 1 calc R . .
C16 C -0.0435(3) 1.2293(3) 0.08452(19) 0.0308(6) Uani 1 1 d . . .
H16 H -0.0993 1.3292 0.0542 0.037 Uiso 1 1 calc R . .
B11 B 0.3558(4) 0.6390(3) 0.1402(2) 0.0263(6) Uani 1 1 d . . .
H11 H 0.3766 0.6619 0.0514 0.032 Uiso 1 1 calc R . .
C17 C 0.1270(3) 1.1697(3) 0.03267(19) 0.0306(6) Uani 1 1 d . . .
H17 H 0.1857 1.2286 -0.0333 0.037 Uiso 1 1 calc R . .
B6 B 0.4570(3) 0.7726(3) 0.2128(2) 0.0248(6) Uani 1 1 d . . .
H6 H 0.5413 0.8842 0.1718 0.030 Uiso 1 1 calc R . .
B5 B 0.5061(4) 0.6428(3) 0.3307(2) 0.0297(6) Uani 1 1 d . . .
H5 H 0.6245 0.6681 0.3661 0.036 Uiso 1 1 calc R . .
C15 C -0.1308(3) 1.1400(3) 0.1814(2) 0.0353(6) Uani 1 1 d . . .
H15 H -0.2460 1.1798 0.2163 0.042 Uiso 1 1 calc R . .
B10 B 0.1413(4) 0.5669(3) 0.2224(2) 0.0269(6) Uani 1 1 d . . .
H10 H 0.0223 0.5428 0.1872 0.032 Uiso 1 1 calc R . .
B3 B 0.1116(3) 0.6570(3) 0.3451(2) 0.0257(6) Uani 1 1 d . . .
H3 H -0.0265 0.6941 0.3896 0.031 Uiso 1 1 calc R . .
B7 B 0.5373(4) 0.5555(3) 0.2081(2) 0.0296(6) Uani 1 1 d . . .
H7 H 0.6768 0.5233 0.1633 0.036 Uiso 1 1 calc R . .
B8 B 0.4341(4) 0.4306(3) 0.3318(2) 0.0295(6) Uani 1 1 d . . .
H8 H 0.5061 0.3162 0.3676 0.035 Uiso 1 1 calc R . .
C19 C 0.2917(4) 0.9404(3) 0.38509(19) 0.0380(6) Uani 1 1 d D . .
H19A H 0.4130 0.9923 0.3668 0.046 Uiso 1 1 calc RD . .
H19B H 0.2081 1.0187 0.3499 0.046 Uiso 1 1 calc R . .
N1 N 0.2283(6) 0.9311(4) 0.4973(2) 0.0897(12) Uani 1 1 d D . .
H1A H 0.311(5) 0.969(10) 0.5300(10) 0.50(8) Uiso 1 1 d D . .
H2A H 0.207(9) 0.827(3) 0.529(4) 0.21(3) Uiso 1 1 d 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
C2 C13 1.511(3) . ?
C2 C1 1.710(3) . ?
C2 B11 1.709(3) . ?
C2 B10 1.709(3) . ?
C2 B3 1.725(3) . ?
C2 B6 1.731(3) . ?
C13 C18 1.381(3) . ?
C13 C14 1.394(3) . ?
C1 C19 1.539(3) . ?
C1 B4 1.695(3) . ?
C1 B5 1.701(3) . ?
C1 B6 1.715(3) . ?
C1 B3 1.718(3) . ?
C18 C17 1.389(3) . ?
C18 H18 0.9300 . ?
B9 B3 1.768(4) . ?
B9 B10 1.772(4) . ?
B9 B4 1.775(4) . ?
B9 B12 1.775(4) . ?
B9 B8 1.780(4) . ?
B9 H9 1.1000 . ?
B12 B10 1.769(4) . ?
B12 B8 1.775(4) . ?
B12 B11 1.776(4) . ?
B12 B7 1.785(4) . ?
B12 H12 1.1000 . ?
B4 B5 1.765(4) . ?
B4 B3 1.767(4) . ?
B4 B8 1.768(4) . ?
B4 H4 1.1000 . ?
C14 C15 1.388(3) . ?
C14 H14 0.9300 . ?
C16 C15 1.377(3) . ?
C16 C17 1.379(3) . ?
C16 H16 0.9300 . ?
B11 B10 1.774(4) . ?
B11 B7 1.779(4) . ?
B11 B6 1.779(4) . ?
B11 H11 1.1000 . ?
C17 H17 0.9300 . ?
B6 B7 1.767(4) . ?
B6 B5 1.776(4) . ?
B6 H6 1.1000 . ?
B5 B8 1.766(4) . ?
B5 B7 1.765(4) . ?
B5 H5 1.1000 . ?
C15 H15 0.9300 . ?
B10 B3 1.779(4) . ?
B10 H10 1.1000 . ?
B3 H3 1.1000 . ?
B7 B8 1.776(4) . ?
B7 H7 1.1000 . ?
B8 H8 1.1000 . ?
C19 N1 1.403(3) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
N1 H1A 0.895(10) . ?
N1 H2A 0.860(10) . ?

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
C13 C2 C1 119.56(16) . . ?
C13 C2 B11 120.55(18) . . ?
C1 C2 B11 109.34(16) . . ?
C13 C2 B10 122.19(17) . . ?
C1 C2 B10 109.54(17) . . ?
B11 C2 B10 62.50(14) . . ?
C13 C2 B3 119.35(17) . . ?
C1 C2 B3 60.05(13) . . ?
B11 C2 B3 113.18(17) . . ?
B10 C2 B3 62.39(14) . . ?
C13 C2 B6 116.84(18) . . ?
C1 C2 B6 59.81(13) . . ?
B11 C2 B6 62.27(14) . . ?
B10 C2 B6 113.10(16) . . ?
B3 C2 B6 111.44(17) . . ?
C18 C13 C14 118.9(2) . . ?
C18 C13 C2 119.42(18) . . ?
C14 C13 C2 121.7(2) . . ?
C19 C1 B4 122.98(19) . . ?
C19 C1 B5 120.91(19) . . ?
B4 C1 B5 62.66(15) . . ?
C19 C1 C2 117.48(17) . . ?
B4 C1 C2 110.37(17) . . ?
B5 C1 C2 110.68(17) . . ?
C19 C1 B6 115.54(19) . . ?
B4 C1 B6 113.88(17) . . ?
B5 C1 B6 62.65(14) . . ?
C2 C1 B6 60.71(13) . . ?
C19 C1 B3 118.77(19) . . ?
B4 C1 B3 62.36(15) . . ?
B5 C1 B3 113.67(18) . . ?
C2 C1 B3 60.42(13) . . ?
B6 C1 B3 112.52(17) . . ?
C13 C18 C17 120.8(2) . . ?
C13 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
B3 B9 B10 60.33(14) . . ?
B3 B9 B4 59.85(14) . . ?
B10 B9 B4 108.11(18) . . ?
B3 B9 B12 107.87(18) . . ?
B10 B9 B12 59.84(15) . . ?
B4 B9 B12 107.64(19) . . ?
B3 B9 B8 107.54(18) . . ?
B10 B9 B8 107.81(19) . . ?
B4 B9 B8 59.66(15) . . ?
B12 B9 B8 59.89(15) . . ?
B3 B9 H9 121.8 . . ?
B10 B9 H9 121.6 . . ?
B4 B9 H9 121.9 . . ?
B12 B9 H9 121.9 . . ?
B8 B9 H9 122.0 . . ?
B10 B12 B8 108.17(18) . . ?
B10 B12 B9 59.99(15) . . ?
B8 B12 B9 60.19(15) . . ?
B10 B12 B11 60.03(14) . . ?
B8 B12 B11 107.98(19) . . ?
B9 B12 B11 108.01(18) . . ?
B10 B12 B7 107.88(18) . . ?
B8 B12 B7 59.84(15) . . ?
B9 B12 B7 107.89(18) . . ?
B11 B12 B7 59.91(15) . . ?
B10 B12 H12 121.7 . . ?
B8 B12 H12 121.6 . . ?
B9 B12 H12 121.7 . . ?
B11 B12 H12 121.7 . . ?
B7 B12 H12 121.9 . . ?
C1 B4 B5 58.83(14) . . ?
C1 B4 B3 59.47(14) . . ?
B5 B4 B3 108.22(19) . . ?
C1 B4 B8 105.50(19) . . ?
B5 B4 B8 59.96(15) . . ?
B3 B4 B8 108.09(19) . . ?
C1 B4 B9 105.97(18) . . ?
B5 B4 B9 108.37(19) . . ?
B3 B4 B9 59.89(15) . . ?
B8 B4 B9 60.32(15) . . ?
C1 B4 H4 123.9 . . ?
B5 B4 H4 121.5 . . ?
B3 B4 H4 121.4 . . ?
B8 B4 H4 122.2 . . ?
B9 B4 H4 121.9 . . ?
C15 C14 C13 120.0(2) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C15 C16 C17 119.7(2) . . ?
C15 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
C2 B11 B10 58.75(13) . . ?
C2 B11 B12 105.44(18) . . ?
B10 B11 B12 59.79(15) . . ?
C2 B11 B7 105.79(18) . . ?
B10 B11 B7 108.00(19) . . ?
B12 B11 B7 60.30(15) . . ?
C2 B11 B6 59.45(13) . . ?
B10 B11 B6 107.80(18) . . ?
B12 B11 B6 107.72(18) . . ?
B7 B11 B6 59.55(15) . . ?
C2 B11 H11 123.8 . . ?
B10 B11 H11 121.8 . . ?
B12 B11 H11 122.3 . . ?
B7 B11 H11 122.1 . . ?
B6 B11 H11 121.7 . . ?
C16 C17 C18 120.0(2) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C1 B6 C2 59.48(12) . . ?
C1 B6 B7 104.94(18) . . ?
C2 B6 B7 105.40(17) . . ?
C1 B6 B5 58.26(14) . . ?
C2 B6 B5 106.23(17) . . ?
B7 B6 B5 59.77(15) . . ?
C1 B6 B11 105.92(17) . . ?
C2 B6 B11 58.28(13) . . ?
B7 B6 B11 60.21(15) . . ?
B5 B6 B11 108.03(19) . . ?
C1 B6 H6 123.6 . . ?
C2 B6 H6 123.3 . . ?
B7 B6 H6 123.0 . . ?
B5 B6 H6 122.1 . . ?
B11 B6 H6 122.1 . . ?
C1 B5 B8 105.37(18) . . ?
C1 B5 B7 105.64(17) . . ?
B8 B5 B7 60.39(16) . . ?
C1 B5 B4 58.51(14) . . ?
B8 B5 B4 60.10(15) . . ?
B7 B5 B4 108.29(19) . . ?
C1 B5 B6 59.08(13) . . ?
B8 B5 B6 108.01(19) . . ?
B7 B5 B6 59.85(15) . . ?
B4 B5 B6 107.61(18) . . ?
C1 B5 H5 124.2 . . ?
B8 B5 H5 122.1 . . ?
B7 B5 H5 121.9 . . ?
B4 B5 H5 121.7 . . ?
B6 B5 H5 121.7 . . ?
C16 C15 C14 120.6(2) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C2 B10 B12 105.74(17) . . ?
C2 B10 B9 105.99(17) . . ?
B12 B10 B9 60.17(15) . . ?
C2 B10 B11 58.75(13) . . ?
B12 B10 B11 60.18(15) . . ?
B9 B10 B11 108.26(18) . . ?
C2 B10 B3 59.23(13) . . ?
B12 B10 B3 107.65(18) . . ?
B9 B10 B3 59.73(15) . . ?
B11 B10 B3 107.61(18) . . ?
C2 B10 H10 123.8 . . ?
B12 B10 H10 122.1 . . ?
B9 B10 H10 122.0 . . ?
B11 B10 H10 121.6 . . ?
B3 B10 H10 121.9 . . ?
C1 B3 C2 59.53(13) . . ?
C1 B3 B4 58.16(14) . . ?
C2 B3 B4 106.32(18) . . ?
C1 B3 B9 105.25(17) . . ?
C2 B3 B9 105.50(17) . . ?
B4 B3 B9 60.27(15) . . ?
C1 B3 B10 105.97(17) . . ?
C2 B3 B10 58.38(13) . . ?
B4 B3 B10 108.14(18) . . ?
B9 B3 B10 59.95(15) . . ?
C1 B3 H3 123.6 . . ?
C2 B3 H3 123.3 . . ?
B4 B3 H3 121.9 . . ?
B9 B3 H3 122.8 . . ?
B10 B3 H3 122.1 . . ?
B5 B7 B6 60.38(15) . . ?
B5 B7 B8 59.82(15) . . ?
B6 B7 B8 107.97(18) . . ?
B5 B7 B11 108.53(17) . . ?
B6 B7 B11 60.23(14) . . ?
B8 B7 B11 107.83(18) . . ?
B5 B7 B12 107.81(19) . . ?
B6 B7 B12 107.85(18) . . ?
B8 B7 B12 59.78(15) . . ?
B11 B7 B12 59.79(15) . . ?
B5 B7 H7 121.5 . . ?
B6 B7 H7 121.6 . . ?
B8 B7 H7 122.0 . . ?
B11 B7 H7 121.6 . . ?
B12 B7 H7 122.0 . . ?
B5 B8 B4 59.94(15) . . ?
B5 B8 B12 108.27(19) . . ?
B4 B8 B12 107.95(18) . . ?
B5 B8 B7 59.79(16) . . ?
B4 B8 B7 107.68(18) . . ?
B12 B8 B7 60.38(15) . . ?
B5 B8 B9 108.12(18) . . ?
B4 B8 B9 60.02(15) . . ?
B12 B8 B9 59.92(15) . . ?
B7 B8 B9 108.10(18) . . ?
B5 B8 H8 121.7 . . ?
B4 B8 H8 121.9 . . ?
B12 B8 H8 121.5 . . ?
B7 B8 H8 121.8 . . ?
B9 B8 H8 121.7 . . ?
N1 C19 C1 117.6(2) . . ?
N1 C19 H19A 107.9 . . ?
C1 C19 H19A 107.9 . . ?
N1 C19 H19B 107.9 . . ?
C1 C19 H19B 107.9 . . ?
H19A C19 H19B 107.2 . . ?
C19 N1 H1A 112.5(8) . . ?
C19 N1 H2A 113(4) . . ?
H1A N1 H2A 104.4(16) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.052
####################################################################### 
# 
# 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_17
_database_code_depnum_ccdc_archive 'CCDC 1583780'
_audit_update_record             
;
2017-11-03 deposited with the CCDC.
2018-03-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H21 B10 Br2 N'
_chemical_formula_weight         555.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   12.4232(5)
_cell_length_b                   14.9794(6)
_cell_length_c                   13.9157(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.5090(10)
_cell_angle_gamma                90.00
_cell_volume                     2440.93(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9775
_cell_measurement_theta_min      3.02
_cell_measurement_theta_max      27.53

_exptl_crystal_description       Block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1096
_exptl_absorpt_coefficient_mu    3.333
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43196
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0176
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         27.55
_reflns_number_total             5596
_reflns_number_gt                4950
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0303P)²+1.8260P] 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         5596
_refine_ls_number_parameters     323
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0257
_refine_ls_wR_factor_ref         0.0653
_refine_ls_wR_factor_gt          0.0619
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.002
_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
Br1 Br -0.494266(16) 0.207792(13) 0.343362(16) 0.02873(6) Uani 1 1 d . . .
Br2 Br -0.437389(17) 0.581382(15) -0.098106(15) 0.03383(7) Uani 1 1 d . . .
C25 C -0.20009(15) 0.47682(13) 0.16240(13) 0.0226(4) Uani 1 1 d . . .
H25 H -0.1911 0.4751 0.2315 0.027 Uiso 1 1 calc R . .
C26 C -0.14191(14) 0.27847(11) 0.30711(13) 0.0177(3) Uani 1 1 d . . .
C19 C 0.28421(16) 0.42215(12) 0.55523(14) 0.0247(4) Uani 1 1 d . . .
H19 H 0.2479 0.3735 0.5726 0.030 Uiso 1 1 calc R . .
C21 C -0.13743(16) 0.43724(12) 0.02393(13) 0.0217(4) Uani 1 1 d . . .
H21 H -0.0849 0.4100 -0.0010 0.026 Uiso 1 1 calc R . .
C29 C -0.35136(15) 0.23621(11) 0.32881(14) 0.0204(3) Uani 1 1 d . . .
C13 C 0.00433(15) 0.46632(11) 0.39069(12) 0.0174(3) Uani 1 1 d . . .
C1 C 0.04640(14) 0.39803(11) 0.32874(12) 0.0143(3) Uani 1 1 d . . .
B4 B -0.01324(16) 0.37941(13) 0.19948(14) 0.0162(4) Uani 1 1 d . . .
C28 C -0.34506(15) 0.24559(12) 0.23188(14) 0.0209(4) Uani 1 1 d . . .
H28 H -0.4095 0.2378 0.1745 0.025 Uiso 1 1 calc R . .
C27 C -0.24037(15) 0.26686(12) 0.22215(13) 0.0202(3) Uani 1 1 d . . .
H27 H -0.2356 0.2736 0.1573 0.024 Uiso 1 1 calc R . .
C14 C 0.26495(14) 0.44175(11) 0.45288(13) 0.0176(3) Uani 1 1 d . . .
C2 C 0.19010(14) 0.38288(11) 0.36885(12) 0.0160(3) Uani 1 1 d . . .
N1 N 0.00898(17) 0.55991(11) 0.36834(14) 0.0261(3) Uani 1 1 d . . .
C20 C -0.11940(14) 0.43417(11) 0.12856(13) 0.0171(3) Uani 1 1 d . . .
C31 C -0.15276(15) 0.26895(13) 0.40353(14) 0.0229(4) Uani 1 1 d . . .
H31 H -0.0888 0.2768 0.4613 0.027 Uiso 1 1 calc R . .
C15 C 0.31990(16) 0.51517(13) 0.42918(14) 0.0241(4) Uani 1 1 d . . .
H15 H 0.3083 0.5290 0.3613 0.029 Uiso 1 1 calc R . .
B6 B 0.10464(16) 0.30387(13) 0.39776(15) 0.0185(4) Uani 1 1 d . . .
H6 H 0.1045 0.2914 0.4756 0.022 Uiso 1 1 calc R . .
B8 B 0.08757(17) 0.21745(13) 0.30757(17) 0.0226(4) Uani 1 1 d . . .
H8 H 0.0763 0.1473 0.3257 0.027 Uiso 1 1 calc R . .
C30 C -0.25701(16) 0.24793(13) 0.41516(14) 0.0247(4) Uani 1 1 d . . .
H30 H -0.2629 0.2419 0.4797 0.030 Uiso 1 1 calc R . .
C24 C -0.29351(16) 0.52174(13) 0.09622(14) 0.0246(4) Uani 1 1 d . . .
H24 H -0.3450 0.5511 0.1207 0.029 Uiso 1 1 calc R . .
B5 B -0.02362(16) 0.29776(13) 0.29092(15) 0.0173(4) Uani 1 1 d . . .
C23 C -0.30826(15) 0.52190(12) -0.00670(13) 0.0218(4) Uani 1 1 d . . .
B3 B 0.12211(16) 0.43297(13) 0.25259(14) 0.0169(4) Uani 1 1 d . . .
H3 H 0.1334 0.5036 0.2365 0.020 Uiso 1 1 calc R . .
B11 B 0.23252(17) 0.35301(14) 0.26912(16) 0.0205(4) Uani 1 1 d . . .
H11 H 0.3156 0.3714 0.2627 0.025 Uiso 1 1 calc R . .
B9 B 0.01616(17) 0.26386(14) 0.18490(16) 0.0211(4) Uani 1 1 d . . .
H9 H -0.0414 0.2235 0.1229 0.025 Uiso 1 1 calc R . .
C22 C -0.23180(16) 0.47988(13) -0.04376(13) 0.0244(4) Uani 1 1 d . . .
H22 H -0.2431 0.4800 -0.1133 0.029 Uiso 1 1 calc R . .
B12 B 0.16670(17) 0.24817(14) 0.22684(17) 0.0242(4) Uani 1 1 d . . .
H12 H 0.2065 0.1978 0.1920 0.029 Uiso 1 1 calc R . .
C17 C 0.41078(17) 0.54783(13) 0.60726(15) 0.0277(4) Uani 1 1 d . . .
H17 H 0.4591 0.5831 0.6586 0.033 Uiso 1 1 calc R . .
C18 C 0.35719(17) 0.47481(14) 0.63139(14) 0.0288(4) Uani 1 1 d . . .
H18 H 0.3701 0.4607 0.6994 0.035 Uiso 1 1 calc R . .
B7 B 0.22183(17) 0.27265(13) 0.35933(17) 0.0215(4) Uani 1 1 d . . .
H7 H 0.2975 0.2389 0.4114 0.026 Uiso 1 1 calc R . .
C16 C 0.39195(18) 0.56808(13) 0.50587(16) 0.0294(4) Uani 1 1 d . . .
H16 H 0.4277 0.6173 0.4890 0.035 Uiso 1 1 calc R . .
B10 B 0.10585(17) 0.34788(14) 0.16117(15) 0.0202(4) Uani 1 1 d . . .
H10 H 0.1067 0.3623 0.0839 0.024 Uiso 1 1 calc R . .
H13A H 0.0479(17) 0.4562(13) 0.4619(16) 0.017(5) Uiso 1 1 d . . .
H13B H -0.0732(19) 0.4507(15) 0.3818(16) 0.024(5) Uiso 1 1 d . . .
H1A H -0.026(2) 0.5694(18) 0.309(2) 0.043(8) Uiso 1 1 d . . .
H1B H 0.082(3) 0.5762(19) 0.382(2) 0.053(8) Uiso 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 C29 1.9011(17) . ?
Br2 C23 1.9033(18) . ?
C25 C24 1.391(2) . ?
C25 C20 1.396(2) . ?
C25 H25 0.9300 . ?
C26 C31 1.400(2) . ?
C26 C27 1.399(2) . ?
C26 B5 1.586(2) . ?
C19 C18 1.388(3) . ?
C19 C14 1.394(2) . ?
C19 H19 0.9300 . ?
C21 C22 1.390(3) . ?
C21 C20 1.398(2) . ?
C21 H21 0.9300 . ?
C29 C30 1.381(3) . ?
C29 C28 1.384(3) . ?
C13 N1 1.441(2) . ?
C13 C1 1.537(2) . ?
C13 H13A 0.97(2) . ?
C13 H13B 0.96(2) . ?
C1 C2 1.698(2) . ?
C1 B3 1.717(2) . ?
C1 B6 1.724(2) . ?
C1 B4 1.724(2) . ?
C1 B5 1.727(2) . ?
B4 C20 1.586(3) . ?
B4 B3 1.785(3) . ?
B4 B9 1.794(3) . ?
B4 B10 1.795(3) . ?
B4 B5 1.800(3) . ?
C28 C27 1.389(2) . ?
C28 H28 0.9300 . ?
C27 H27 0.9300 . ?
C14 C15 1.391(3) . ?
C14 C2 1.511(2) . ?
C2 B11 1.701(3) . ?
C2 B7 1.713(3) . ?
C2 B6 1.725(3) . ?
C2 B3 1.727(2) . ?
N1 H1A 0.80(3) . ?
N1 H1B 0.89(3) . ?
C31 C30 1.394(3) . ?
C31 H31 0.9300 . ?
C15 C16 1.389(3) . ?
C15 H15 0.9300 . ?
B6 B8 1.766(3) . ?
B6 B7 1.773(3) . ?
B6 B5 1.782(3) . ?
B6 H6 1.1000 . ?
B8 B9 1.781(3) . ?
B8 B12 1.783(3) . ?
B8 B7 1.784(3) . ?
B8 B5 1.787(3) . ?
B8 H8 1.1000 . ?
C30 H30 0.9300 . ?
C24 C23 1.382(3) . ?
C24 H24 0.9300 . ?
B5 B9 1.779(3) . ?
C23 C22 1.375(3) . ?
B3 B10 1.764(3) . ?
B3 B11 1.777(3) . ?
B3 H3 1.1000 . ?
B11 B7 1.776(3) . ?
B11 B12 1.778(3) . ?
B11 B10 1.778(3) . ?
B11 H11 1.1000 . ?
B9 B12 1.779(3) . ?
B9 B10 1.783(3) . ?
B9 H9 1.1000 . ?
C22 H22 0.9300 . ?
B12 B7 1.777(3) . ?
B12 B10 1.782(3) . ?
B12 H12 1.1000 . ?
C17 C18 1.379(3) . ?
C17 C16 1.385(3) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
B7 H7 1.1000 . ?
C16 H16 0.9300 . ?
B10 H10 1.1000 . ?

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
C24 C25 C20 122.17(16) . . ?
C24 C25 H25 118.9 . . ?
C20 C25 H25 118.9 . . ?
C31 C26 C27 117.41(16) . . ?
C31 C26 B5 123.04(16) . . ?
C27 C26 B5 119.51(16) . . ?
C18 C19 C14 120.39(18) . . ?
C18 C19 H19 119.8 . . ?
C14 C19 H19 119.8 . . ?
C22 C21 C20 121.77(17) . . ?
C22 C21 H21 119.1 . . ?
C20 C21 H21 119.1 . . ?
C30 C29 C28 121.81(16) . . ?
C30 C29 Br1 119.15(14) . . ?
C28 C29 Br1 119.03(13) . . ?
N1 C13 C1 118.72(15) . . ?
N1 C13 H13A 108.9(12) . . ?
C1 C13 H13A 106.9(12) . . ?
N1 C13 H13B 108.7(13) . . ?
C1 C13 H13B 106.3(13) . . ?
H13A C13 H13B 106.7(17) . . ?
C13 C1 C2 114.93(13) . . ?
C13 C1 B3 120.15(14) . . ?
C2 C1 B3 60.74(10) . . ?
C13 C1 B6 112.95(13) . . ?
C2 C1 B6 60.53(10) . . ?
B3 C1 B6 112.27(13) . . ?
C13 C1 B4 125.77(13) . . ?
C2 C1 B4 111.08(12) . . ?
B3 C1 B4 62.51(10) . . ?
B6 C1 B4 113.78(13) . . ?
C13 C1 B5 121.23(14) . . ?
C2 C1 B5 110.55(12) . . ?
B3 C1 B5 113.64(13) . . ?
B6 C1 B5 62.17(11) . . ?
B4 C1 B5 62.89(11) . . ?
C20 B4 C1 122.94(14) . . ?
C20 B4 B3 119.84(14) . . ?
C1 B4 B3 58.54(10) . . ?
C20 B4 B9 125.92(14) . . ?
C1 B4 B9 103.96(13) . . ?
B3 B4 B9 106.33(13) . . ?
C20 B4 B10 123.21(14) . . ?
C1 B4 B10 104.05(13) . . ?
B3 B4 B10 59.04(10) . . ?
B9 B4 B10 59.58(11) . . ?
C20 B4 B5 123.37(14) . . ?
C1 B4 B5 58.65(10) . . ?
B3 B4 B5 107.01(13) . . ?
B9 B4 B5 59.33(11) . . ?
B10 B4 B5 106.96(14) . . ?
C29 C28 C27 118.55(16) . . ?
C29 C28 H28 120.7 . . ?
C27 C28 H28 120.7 . . ?
C28 C27 C26 121.93(16) . . ?
C28 C27 H27 119.0 . . ?
C26 C27 H27 119.0 . . ?
C15 C14 C19 118.57(16) . . ?
C15 C14 C2 120.12(15) . . ?
C19 C14 C2 121.26(16) . . ?
C14 C2 C1 118.95(13) . . ?
C14 C2 B11 120.44(14) . . ?
C1 C2 B11 110.19(13) . . ?
C14 C2 B7 121.62(14) . . ?
C1 C2 B7 110.32(12) . . ?
B11 C2 B7 62.69(12) . . ?
C14 C2 B6 119.18(14) . . ?
C1 C2 B6 60.47(10) . . ?
B11 C2 B6 113.10(13) . . ?
B7 C2 B6 62.10(11) . . ?
C14 C2 B3 116.97(13) . . ?
C1 C2 B3 60.16(10) . . ?
B11 C2 B3 62.46(11) . . ?
B7 C2 B3 113.55(13) . . ?
B6 C2 B3 111.73(13) . . ?
C13 N1 H1A 110.2(19) . . ?
C13 N1 H1B 109.4(19) . . ?
H1A N1 H1B 110(3) . . ?
C25 C20 C21 116.92(16) . . ?
C25 C20 B4 124.61(15) . . ?
C21 C20 B4 118.40(15) . . ?
C30 C31 C26 121.67(17) . . ?
C30 C31 H31 119.2 . . ?
C26 C31 H31 119.2 . . ?
C16 C15 C14 120.68(17) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C1 B6 C2 59.00(10) . . ?
C1 B6 B8 105.98(14) . . ?
C2 B6 B8 105.93(14) . . ?
C1 B6 B7 106.37(14) . . ?
C2 B6 B7 58.62(11) . . ?
B8 B6 B7 60.54(11) . . ?
C1 B6 B5 59.02(10) . . ?
C2 B6 B5 106.81(13) . . ?
B8 B6 B5 60.50(11) . . ?
B7 B6 B5 109.28(14) . . ?
C1 B6 H6 123.4 . . ?
C2 B6 H6 123.4 . . ?
B8 B6 H6 122.4 . . ?
B7 B6 H6 121.5 . . ?
B5 B6 H6 121.2 . . ?
B6 B8 B9 107.35(14) . . ?
B6 B8 B12 107.34(14) . . ?
B9 B8 B12 59.89(12) . . ?
B6 B8 B7 59.94(11) . . ?
B9 B8 B7 107.77(15) . . ?
B12 B8 B7 59.78(12) . . ?
B6 B8 B5 60.19(11) . . ?
B9 B8 B5 59.81(11) . . ?
B12 B8 B5 108.03(14) . . ?
B7 B8 B5 108.56(13) . . ?
B6 B8 H8 122.1 . . ?
B9 B8 H8 122.1 . . ?
B12 B8 H8 122.0 . . ?
B7 B8 H8 121.6 . . ?
B5 B8 H8 121.4 . . ?
C29 C30 C31 118.63(17) . . ?
C29 C30 H30 120.7 . . ?
C31 C30 H30 120.7 . . ?
C23 C24 C25 118.66(17) . . ?
C23 C24 H24 120.7 . . ?
C25 C24 H24 120.7 . . ?
C26 B5 C1 120.75(14) . . ?
C26 B5 B9 126.37(15) . . ?
C1 B5 B9 104.46(13) . . ?
C26 B5 B6 120.24(15) . . ?
C1 B5 B6 58.81(10) . . ?
B9 B5 B6 106.74(13) . . ?
C26 B5 B8 124.86(14) . . ?
C1 B5 B8 104.89(13) . . ?
B9 B5 B8 59.92(12) . . ?
B6 B5 B8 59.30(11) . . ?
C26 B5 B4 120.84(14) . . ?
C1 B5 B4 58.46(10) . . ?
B9 B5 B4 60.17(11) . . ?
B6 B5 B4 107.44(13) . . ?
B8 B5 B4 108.31(14) . . ?
C22 C23 C24 121.25(17) . . ?
C22 C23 Br2 119.81(13) . . ?
C24 C23 Br2 118.94(14) . . ?
C1 B3 C2 59.10(10) . . ?
C1 B3 B10 105.69(13) . . ?
C2 B3 B10 105.32(13) . . ?
C1 B3 B11 105.84(13) . . ?
C2 B3 B11 58.06(10) . . ?
B10 B3 B11 60.26(11) . . ?
C1 B3 B4 58.94(10) . . ?
C2 B3 B4 106.92(13) . . ?
B10 B3 B4 60.76(11) . . ?
B11 B3 B4 109.28(14) . . ?
C1 B3 H3 123.6 . . ?
C2 B3 H3 123.6 . . ?
B10 B3 H3 122.6 . . ?
B11 B3 H3 121.9 . . ?
B4 B3 H3 121.0 . . ?
C2 B11 B7 58.99(11) . . ?
C2 B11 B3 59.48(10) . . ?
B7 B11 B3 108.16(13) . . ?
C2 B11 B12 105.60(14) . . ?
B7 B11 B12 60.03(12) . . ?
B3 B11 B12 107.62(14) . . ?
C2 B11 B10 105.83(13) . . ?
B7 B11 B10 108.30(14) . . ?
B3 B11 B10 59.51(11) . . ?
B12 B11 B10 60.17(12) . . ?
C2 B11 H11 123.7 . . ?
B7 B11 H11 121.4 . . ?
B3 B11 H11 121.7 . . ?
B12 B11 H11 122.3 . . ?
B10 B11 H11 122.1 . . ?
B12 B9 B5 108.56(14) . . ?
B12 B9 B8 60.10(12) . . ?
B5 B9 B8 60.27(11) . . ?
B12 B9 B10 60.04(12) . . ?
B5 B9 B10 108.42(13) . . ?
B8 B9 B10 108.12(14) . . ?
B12 B9 B4 108.77(14) . . ?
B5 B9 B4 60.51(10) . . ?
B8 B9 B4 108.86(14) . . ?
B10 B9 B4 60.23(11) . . ?
B12 B9 H9 121.4 . . ?
B5 B9 H9 121.3 . . ?
B8 B9 H9 121.5 . . ?
B10 B9 H9 121.7 . . ?
B4 B9 H9 121.1 . . ?
C23 C22 C21 119.21(16) . . ?
C23 C22 H22 120.4 . . ?
C21 C22 H22 120.4 . . ?
B11 B12 B7 59.94(11) . . ?
B11 B12 B9 107.99(14) . . ?
B7 B12 B9 108.17(14) . . ?
B11 B12 B10 59.92(11) . . ?
B7 B12 B10 108.03(14) . . ?
B9 B12 B10 60.10(11) . . ?
B11 B12 B8 108.00(14) . . ?
B7 B12 B8 60.14(12) . . ?
B9 B12 B8 60.02(12) . . ?
B10 B12 B8 108.10(14) . . ?
B11 B12 H12 121.8 . . ?
B7 B12 H12 121.6 . . ?
B9 B12 H12 121.6 . . ?
B10 B12 H12 121.7 . . ?
B8 B12 H12 121.6 . . ?
C18 C17 C16 119.40(17) . . ?
C18 C17 H17 120.3 . . ?
C16 C17 H17 120.3 . . ?
C17 C18 C19 120.69(18) . . ?
C17 C18 H18 119.7 . . ?
C19 C18 H18 119.7 . . ?
C2 B7 B6 59.28(10) . . ?
C2 B7 B11 58.32(11) . . ?
B6 B7 B11 107.29(14) . . ?
C2 B7 B12 105.08(14) . . ?
B6 B7 B12 107.24(14) . . ?
B11 B7 B12 60.04(12) . . ?
C2 B7 B8 105.65(13) . . ?
B6 B7 B8 59.53(11) . . ?
B11 B7 B8 108.02(15) . . ?
B12 B7 B8 60.07(12) . . ?
C2 B7 H7 124.1 . . ?
B6 B7 H7 122.0 . . ?
B11 B7 H7 121.9 . . ?
B12 B7 H7 122.5 . . ?
B8 B7 H7 122.1 . . ?
C17 C16 C15 120.26(18) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
B3 B10 B11 60.23(11) . . ?
B3 B10 B12 108.00(14) . . ?
B11 B10 B12 59.91(12) . . ?
B3 B10 B9 107.73(13) . . ?
B11 B10 B9 107.79(15) . . ?
B12 B10 B9 59.86(12) . . ?
B3 B10 B4 60.20(11) . . ?
B11 B10 B4 108.81(13) . . ?
B12 B10 B4 108.59(14) . . ?
B9 B10 B4 60.19(11) . . ?
B3 B10 H10 121.8 . . ?
B11 B10 H10 121.5 . . ?
B12 B10 H10 121.7 . . ?
B9 B10 H10 122.0 . . ?
B4 B10 H10 121.1 . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.55
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.062
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_6
_database_code_depnum_ccdc_archive 'CCDC 1583778'
_audit_update_record             
;
2017-11-03 deposited with the CCDC.
2018-03-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C23 H26 B10 F3 N O'
_chemical_formula_weight         497.55

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/n  '

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

_cell_length_a                   18.1161(10)
_cell_length_b                   8.1173(5)
_cell_length_c                   18.6508(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.681(2)
_cell_angle_gamma                90.00
_cell_volume                     2511.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4917
_cell_measurement_theta_min      0.990
_cell_measurement_theta_max      26.00

_exptl_crystal_description       Block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1024
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.9886
_exptl_absorpt_correction_T_max  0.9904
_exptl_absorpt_process_details   ?

_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  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43718
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0125
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_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         3.23
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4878
_reflns_number_gt                4335
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.2000P)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         4878
_refine_ls_number_parameters     343
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0518
_refine_ls_wR_factor_ref         0.2324
_refine_ls_wR_factor_gt          0.2127
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_restrained_S_all      1.118
_refine_ls_shift/su_max          0.002
_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
N1 N 0.23357(7) 1.07308(14) 0.07184(7) 0.0241(3) Uani 1 1 d . . .
H1 H 0.2279 1.0438 0.1137 0.029 Uiso 1 1 calc R . .
C25 C 0.28177(8) 0.80700(17) 0.22293(8) 0.0233(3) Uani 1 1 d . . .
H25 H 0.3338 0.8493 0.2460 0.028 Uiso 1 1 calc R . .
C20 C 0.25693(8) 0.72874(16) 0.15006(8) 0.0208(3) Uani 1 1 d . . .
C2 C 0.32457(8) 0.81855(16) -0.03691(8) 0.0216(3) Uani 1 1 d . . .
C27 C 0.48434(9) 0.76406(18) 0.27717(8) 0.0271(4) Uani 1 1 d . . .
H27 H 0.4607 0.6610 0.2736 0.033 Uiso 1 1 calc R . .
C1 C 0.33217(8) 0.87290(16) 0.05639(7) 0.0199(3) Uani 1 1 d . . .
C22 C 0.12663(9) 0.68118(18) 0.15692(9) 0.0290(4) Uani 1 1 d . . .
H22 H 0.0748 0.6377 0.1348 0.035 Uiso 1 1 calc R . .
C14 C 0.29178(8) 0.94271(16) -0.10217(8) 0.0231(3) Uani 1 1 d . . .
B11 B 0.29965(10) 0.61625(18) -0.05398(9) 0.0237(4) Uani 1 1 d . . .
H11 H 0.2628 0.5650 -0.1120 0.028 Uiso 1 1 calc R . .
C21 C 0.17757(9) 0.66735(17) 0.11799(8) 0.0254(4) Uani 1 1 d . . .
H21 H 0.1587 0.6160 0.0693 0.031 Uiso 1 1 calc R . .
C26 C 0.46820(8) 0.85514(18) 0.20850(8) 0.0248(3) Uani 1 1 d . . .
C13 C 0.31105(8) 1.05078(16) 0.06746(8) 0.0230(3) Uani 1 1 d . . .
H13A H 0.3526 1.0935 0.1152 0.028 Uiso 1 1 calc R . .
H13B H 0.3119 1.1162 0.0243 0.028 Uiso 1 1 calc R . .
C18 C 0.17996(9) 1.04131(18) -0.21669(8) 0.0284(4) Uani 1 1 d . . .
H18 H 0.1264 1.0320 -0.2518 0.034 Uiso 1 1 calc R . .
B3 B 0.25786(9) 0.74231(18) -0.00123(8) 0.0204(4) Uani 1 1 d . . .
H3 H 0.1937 0.7768 -0.0260 0.024 Uiso 1 1 calc R . .
C24 C 0.23060(9) 0.82299(18) 0.26168(9) 0.0288(4) Uani 1 1 d . . .
H24 H 0.2484 0.8763 0.3098 0.035 Uiso 1 1 calc R . .
C23 C 0.15307(9) 0.75965(18) 0.22864(9) 0.0290(4) Uani 1 1 d . . .
H23 H 0.1190 0.7699 0.2547 0.035 Uiso 1 1 calc R . .
B4 B 0.31082(9) 0.70580(18) 0.10178(8) 0.0200(3) Uani 1 1 d . . .
B12 B 0.38190(10) 0.5059(2) 0.01631(9) 0.0261(4) Uani 1 1 d . . .
H12 H 0.3988 0.3823 0.0040 0.031 Uiso 1 1 calc R . .
B7 B 0.40030(10) 0.68579(19) -0.02904(9) 0.0246(4) Uani 1 1 d . . .
H7 H 0.4292 0.6809 -0.0708 0.030 Uiso 1 1 calc R . .
B6 B 0.41739(9) 0.85089(19) 0.03894(9) 0.0226(4) Uani 1 1 d . . .
H6 H 0.4562 0.9560 0.0401 0.027 Uiso 1 1 calc R . .
B8 B 0.45576(10) 0.6524(2) 0.07330(9) 0.0247(4) Uani 1 1 d . . .
H8 H 0.5206 0.6248 0.0972 0.030 Uiso 1 1 calc R . .
C31 C 0.50563(8) 1.00880(19) 0.21672(9) 0.0297(4) Uani 1 1 d . . .
H31 H 0.4968 1.0719 0.1724 0.036 Uiso 1 1 calc R . .
C19 C 0.21164(9) 0.92995(17) -0.15568(8) 0.0258(4) Uani 1 1 d . . .
H19 H 0.1793 0.8460 -0.1503 0.031 Uiso 1 1 calc R . .
C28 C 0.53466(9) 0.8239(2) 0.35012(8) 0.0320(4) Uani 1 1 d . . .
H28 H 0.5444 0.7609 0.3947 0.038 Uiso 1 1 calc R . .
C29 C 0.57051(9) 0.9774(2) 0.35693(9) 0.0347(4) Uani 1 1 d . . .
H29 H 0.6039 1.0180 0.4059 0.042 Uiso 1 1 calc R . .
C15 C 0.33965(10) 1.0664(2) -0.11217(9) 0.0327(4) Uani 1 1 d . . .
H15 H 0.3935 1.0749 -0.0778 0.039 Uiso 1 1 calc R . .
C17 C 0.22744(10) 1.1665(2) -0.22574(9) 0.0342(4) Uani 1 1 d . . .
H17 H 0.2060 1.2421 -0.2664 0.041 Uiso 1 1 calc R . .
C30 C 0.55607(9) 1.0694(2) 0.29023(9) 0.0334(4) Uani 1 1 d . . .
H30 H 0.5801 1.1722 0.2944 0.040 Uiso 1 1 calc R . .
B5 B 0.41374(9) 0.77447(19) 0.12761(9) 0.0216(4) Uani 1 1 d . . .
B10 B 0.29263(9) 0.54227(19) 0.03276(9) 0.0237(4) Uani 1 1 d . . .
H10 H 0.2509 0.4420 0.0304 0.028 Uiso 1 1 calc R . .
C16 C 0.30729(11) 1.1777(2) -0.17355(10) 0.0404(4) Uani 1 1 d . . .
H16 H 0.3397 1.2607 -0.1796 0.049 Uiso 1 1 calc R . .
B9 B 0.38926(9) 0.56107(18) 0.11147(9) 0.0237(4) Uani 1 1 d . . .
H9 H 0.4108 0.4724 0.1601 0.028 Uiso 1 1 calc R . .
O1 O 0.16881(8) 1.17807(16) -0.05085(6) 0.0429(4) Uani 1 1 d . . .
C32 C 0.17064(9) 1.13801(17) 0.01246(9) 0.0285(4) Uani 1 1 d . . .
C33 C 0.09668(9) 1.17115(19) 0.03138(11) 0.0376(4) Uani 1 1 d . . .
F1 F 0.09964(6) 1.09323(13) 0.09512(6) 0.0442(3) Uani 1 1 d . . .
F2 F 0.09126(8) 1.33172(13) 0.04274(11) 0.0732(5) Uani 1 1 d . . .
F3 F 0.03025(6) 1.12858(18) -0.02797(8) 0.0711(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
N1 C32 1.3378(19) . ?
N1 C13 1.4498(17) . ?
N1 H1 0.8600 . ?
C25 C24 1.392(2) . ?
C25 C20 1.4007(18) . ?
C25 H25 0.9300 . ?
C20 C21 1.4079(19) . ?
C20 B4 1.5826(19) . ?
C2 C14 1.5065(19) . ?
C2 B11 1.6989(19) . ?
C2 B7 1.704(2) . ?
C2 B3 1.7124(19) . ?
C2 B6 1.728(2) . ?
C2 C1 1.7462(17) . ?
C27 C28 1.386(2) . ?
C27 C26 1.404(2) . ?
C27 H27 0.9300 . ?
C1 C13 1.5288(18) . ?
C1 B6 1.7103(19) . ?
C1 B3 1.7114(18) . ?
C1 B4 1.7231(19) . ?
C1 B5 1.735(2) . ?
C22 C23 1.382(2) . ?
C22 C21 1.389(2) . ?
C22 H22 0.9300 . ?
C14 C15 1.387(2) . ?
C14 C19 1.397(2) . ?
B11 B10 1.778(2) . ?
B11 B3 1.785(2) . ?
B11 B7 1.783(2) . ?
B11 B12 1.781(2) . ?
B11 H11 1.1000 . ?
C21 H21 0.9300 . ?
C26 C31 1.398(2) . ?
C26 B5 1.5755(19) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C18 C19 1.384(2) . ?
C18 C17 1.385(2) . ?
C18 H18 0.9300 . ?
B3 B10 1.765(2) . ?
B3 B4 1.794(2) . ?
B3 H3 1.1000 . ?
C24 C23 1.386(2) . ?
C24 H24 0.9300 . ?
C23 H23 0.9300 . ?
B4 B10 1.785(2) . ?
B4 B9 1.796(2) . ?
B4 B5 1.816(2) . ?
B12 B7 1.784(2) . ?
B12 B9 1.783(2) . ?
B12 B8 1.787(2) . ?
B12 B10 1.788(2) . ?
B12 H12 1.1000 . ?
B7 B6 1.784(2) . ?
B7 B8 1.785(2) . ?
B7 H7 1.1000 . ?
B6 B8 1.769(2) . ?
B6 B5 1.792(2) . ?
B6 H6 1.1000 . ?
B8 B9 1.788(2) . ?
B8 B5 1.790(2) . ?
B8 H8 1.1000 . ?
C31 C30 1.396(2) . ?
C31 H31 0.9300 . ?
C19 H19 0.9300 . ?
C28 C29 1.387(3) . ?
C28 H28 0.9300 . ?
C29 C30 1.383(2) . ?
C29 H29 0.9300 . ?
C15 C16 1.389(2) . ?
C15 H15 0.9300 . ?
C17 C16 1.385(2) . ?
C17 H17 0.9300 . ?
C30 H30 0.9300 . ?
B5 B9 1.783(2) . ?
B10 B9 1.783(2) . ?
B10 H10 1.1000 . ?
C16 H16 0.9300 . ?
B9 H9 1.1000 . ?
O1 C32 1.2123(19) . ?
C32 C33 1.540(2) . ?
C33 F3 1.3125(19) . ?
C33 F2 1.330(2) . ?
C33 F1 1.329(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
C32 N1 C13 121.67(12) . . ?
C32 N1 H1 119.2 . . ?
C13 N1 H1 119.2 . . ?
C24 C25 C20 121.65(13) . . ?
C24 C25 H25 119.2 . . ?
C20 C25 H25 119.2 . . ?
C25 C20 C21 116.61(13) . . ?
C25 C20 B4 125.04(12) . . ?
C21 C20 B4 118.34(12) . . ?
C14 C2 B11 120.42(11) . . ?
C14 C2 B7 122.37(11) . . ?
B11 C2 B7 63.19(9) . . ?
C14 C2 B3 116.41(11) . . ?
B11 C2 B3 63.10(8) . . ?
B7 C2 B3 114.05(11) . . ?
C14 C2 B6 119.87(11) . . ?
B11 C2 B6 113.47(11) . . ?
B7 C2 B6 62.65(9) . . ?
B3 C2 B6 110.08(10) . . ?
C14 C2 C1 118.93(11) . . ?
B11 C2 C1 109.85(10) . . ?
B7 C2 C1 109.60(10) . . ?
B3 C2 C1 59.30(7) . . ?
B6 C2 C1 58.98(8) . . ?
C28 C27 C26 121.64(14) . . ?
C28 C27 H27 119.2 . . ?
C26 C27 H27 119.2 . . ?
C13 C1 B6 114.73(10) . . ?
C13 C1 B3 119.56(10) . . ?
B6 C1 B3 111.00(10) . . ?
C13 C1 B4 124.01(10) . . ?
B6 C1 B4 114.15(10) . . ?
B3 C1 B4 62.99(8) . . ?
C13 C1 B5 120.93(10) . . ?
B6 C1 B5 62.69(8) . . ?
B3 C1 B5 114.13(10) . . ?
B4 C1 B5 63.36(8) . . ?
C13 C1 C2 116.70(10) . . ?
B6 C1 C2 59.99(8) . . ?
B3 C1 C2 59.37(7) . . ?
B4 C1 C2 110.32(9) . . ?
B5 C1 C2 110.40(10) . . ?
C23 C22 C21 119.89(14) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C15 C14 C19 118.95(13) . . ?
C15 C14 C2 121.86(13) . . ?
C19 C14 C2 119.16(12) . . ?
C2 B11 B10 105.47(10) . . ?
C2 B11 B3 58.82(8) . . ?
B10 B11 B3 59.39(8) . . ?
C2 B11 B7 58.54(8) . . ?
B10 B11 B7 108.01(11) . . ?
B3 B11 B7 106.88(10) . . ?
C2 B11 B12 105.50(11) . . ?
B10 B11 B12 60.31(9) . . ?
B3 B11 B12 107.29(11) . . ?
B7 B11 B12 60.10(9) . . ?
C2 B11 H11 124.1 . . ?
B10 B11 H11 122.1 . . ?
B3 B11 H11 122.4 . . ?
B7 B11 H11 121.9 . . ?
B12 B11 H11 122.1 . . ?
C22 C21 C20 121.92(14) . . ?
C22 C21 H21 119.0 . . ?
C20 C21 H21 119.0 . . ?
C27 C26 C31 117.09(13) . . ?
C27 C26 B5 118.39(12) . . ?
C31 C26 B5 124.42(13) . . ?
N1 C13 C1 115.22(10) . . ?
N1 C13 H13A 108.5 . . ?
C1 C13 H13A 108.5 . . ?
N1 C13 H13B 108.5 . . ?
C1 C13 H13B 108.5 . . ?
H13A C13 H13B 107.5 . . ?
C19 C18 C17 120.44(14) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C1 B3 C2 61.33(8) . . ?
C1 B3 B10 105.49(10) . . ?
C2 B3 B10 105.45(11) . . ?
C1 B3 B11 107.48(10) . . ?
C2 B3 B11 58.08(8) . . ?
B10 B3 B11 60.09(9) . . ?
C1 B3 B4 58.83(8) . . ?
C2 B3 B4 108.57(10) . . ?
B10 B3 B4 60.21(8) . . ?
B11 B3 B4 109.44(11) . . ?
C1 B3 H3 122.5 . . ?
C2 B3 H3 122.4 . . ?
B10 B3 H3 123.3 . . ?
B11 B3 H3 121.6 . . ?
B4 B3 H3 120.8 . . ?
C23 C24 C25 120.12(13) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C22 C23 C24 119.78(13) . . ?
C22 C23 H23 120.1 . . ?
C24 C23 H23 120.1 . . ?
C20 B4 C1 119.89(11) . . ?
C20 B4 B10 121.35(11) . . ?
C1 B4 B10 104.12(10) . . ?
C20 B4 B3 113.77(10) . . ?
C1 B4 B3 58.19(7) . . ?
B10 B4 B3 59.08(8) . . ?
C20 B4 B9 131.58(11) . . ?
C1 B4 B9 103.87(10) . . ?
B10 B4 B9 59.71(8) . . ?
B3 B4 B9 106.08(10) . . ?
C20 B4 B5 127.97(11) . . ?
C1 B4 B5 58.64(8) . . ?
B10 B4 B5 106.98(10) . . ?
B3 B4 B5 106.49(10) . . ?
B9 B4 B5 59.17(8) . . ?
B7 B12 B9 108.24(11) . . ?
B7 B12 B11 60.00(9) . . ?
B9 B12 B11 108.21(11) . . ?
B7 B12 B8 59.97(9) . . ?
B9 B12 B8 60.12(9) . . ?
B11 B12 B8 107.97(11) . . ?
B7 B12 B10 107.49(11) . . ?
B9 B12 B10 59.92(9) . . ?
B11 B12 B10 59.75(9) . . ?
B8 B12 B10 107.52(11) . . ?
B7 B12 H12 121.8 . . ?
B9 B12 H12 121.4 . . ?
B11 B12 H12 121.7 . . ?
B8 B12 H12 121.8 . . ?
B10 B12 H12 122.2 . . ?
C2 B7 B6 59.34(8) . . ?
C2 B7 B8 106.02(11) . . ?
B6 B7 B8 59.44(9) . . ?
C2 B7 B12 105.13(11) . . ?
B6 B7 B12 106.85(11) . . ?
B8 B7 B12 60.07(9) . . ?
C2 B7 B11 58.27(8) . . ?
B6 B7 B11 106.89(10) . . ?
B8 B7 B11 107.96(11) . . ?
B12 B7 B11 59.90(9) . . ?
C2 B7 H7 123.9 . . ?
B6 B7 H7 122.3 . . ?
B8 B7 H7 121.9 . . ?
B12 B7 H7 122.6 . . ?
B11 B7 H7 122.1 . . ?
C1 B6 C2 61.04(8) . . ?
C1 B6 B8 106.23(10) . . ?
C2 B6 B8 105.64(11) . . ?
C1 B6 B7 107.54(10) . . ?
C2 B6 B7 58.01(8) . . ?
B8 B6 B7 60.29(9) . . ?
C1 B6 B5 59.32(8) . . ?
C2 B6 B5 108.56(10) . . ?
B8 B6 B5 60.36(9) . . ?
B7 B6 B5 109.60(11) . . ?
C1 B6 H6 122.2 . . ?
C2 B6 H6 122.6 . . ?
B8 B6 H6 123.0 . . ?
B7 B6 H6 121.6 . . ?
B5 B6 H6 120.7 . . ?
B6 B8 B7 60.27(9) . . ?
B6 B8 B12 107.41(11) . . ?
B7 B8 B12 59.96(9) . . ?
B6 B8 B9 107.00(11) . . ?
B7 B8 B9 107.99(11) . . ?
B12 B8 B9 59.83(9) . . ?
B6 B8 B5 60.45(9) . . ?
B7 B8 B5 109.67(11) . . ?
B12 B8 B5 108.54(11) . . ?
B9 B8 B5 59.79(8) . . ?
B6 B8 H8 122.2 . . ?
B7 B8 H8 121.0 . . ?
B12 B8 H8 121.9 . . ?
B9 B8 H8 122.4 . . ?
B5 B8 H8 120.8 . . ?
C30 C31 C26 121.26(14) . . ?
C30 C31 H31 119.4 . . ?
C26 C31 H31 119.4 . . ?
C18 C19 C14 120.51(13) . . ?
C18 C19 H19 119.7 . . ?
C14 C19 H19 119.7 . . ?
C29 C28 C27 120.25(14) . . ?
C29 C28 H28 119.9 . . ?
C27 C28 H28 119.9 . . ?
C30 C29 C28 119.36(13) . . ?
C30 C29 H29 120.3 . . ?
C28 C29 H29 120.3 . . ?
C14 C15 C16 120.10(14) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C16 C17 C18 119.13(14) . . ?
C16 C17 H17 120.4 . . ?
C18 C17 H17 120.4 . . ?
C29 C30 C31 120.39(14) . . ?
C29 C30 H30 119.8 . . ?
C31 C30 H30 119.8 . . ?
C26 B5 C1 123.71(11) . . ?
C26 B5 B9 125.66(12) . . ?
C1 B5 B9 103.92(10) . . ?
C26 B5 B8 121.77(11) . . ?
C1 B5 B8 104.27(10) . . ?
B9 B5 B8 60.04(9) . . ?
C26 B5 B6 119.91(11) . . ?
C1 B5 B6 57.99(8) . . ?
B9 B5 B6 106.22(10) . . ?
B8 B5 B6 59.19(9) . . ?
C26 B5 B4 124.26(12) . . ?
C1 B5 B4 58.01(8) . . ?
B9 B5 B4 59.86(8) . . ?
B8 B5 B4 107.73(10) . . ?
B6 B5 B4 106.02(10) . . ?
B3 B10 B11 60.52(8) . . ?
B3 B10 B9 107.92(10) . . ?
B11 B10 B9 108.35(11) . . ?
B3 B10 B4 60.71(8) . . ?
B11 B10 B4 110.19(10) . . ?
B9 B10 B4 60.45(8) . . ?
B3 B10 B12 107.88(11) . . ?
B11 B10 B12 59.94(9) . . ?
B9 B10 B12 59.90(8) . . ?
B4 B10 B12 109.19(10) . . ?
B3 B10 H10 121.7 . . ?
B11 B10 H10 120.9 . . ?
B9 B10 H10 121.9 . . ?
B4 B10 H10 120.3 . . ?
B12 B10 H10 121.7 . . ?
C17 C16 C15 120.85(15) . . ?
C17 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
B10 B9 B12 60.18(9) . . ?
B10 B9 B5 108.51(11) . . ?
B12 B9 B5 109.03(11) . . ?
B10 B9 B8 107.67(11) . . ?
B12 B9 B8 60.05(9) . . ?
B5 B9 B8 60.18(9) . . ?
B10 B9 B4 59.84(8) . . ?
B12 B9 B4 108.92(10) . . ?
B5 B9 B4 60.97(8) . . ?
B8 B9 B4 108.72(10) . . ?
B10 B9 H9 122.0 . . ?
B12 B9 H9 121.1 . . ?
B5 B9 H9 121.0 . . ?
B8 B9 H9 121.8 . . ?
B4 B9 H9 121.0 . . ?
O1 C32 N1 126.35(15) . . ?
O1 C32 C33 119.37(15) . . ?
N1 C32 C33 114.18(13) . . ?
F3 C33 F2 106.91(14) . . ?
F3 C33 F1 108.85(13) . . ?
F2 C33 F1 107.63(16) . . ?
F3 C33 C32 110.38(16) . . ?
F2 C33 C32 109.53(12) . . ?
F1 C33 C32 113.31(13) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.050
####################################################################### 
# 
# 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_10
_database_code_depnum_ccdc_archive 'CCDC 1583779'
_audit_update_record             
;
2017-11-03 deposited with the CCDC.
2018-03-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H35 B10 N'
_chemical_formula_weight         457.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P2(1)2(1)2(1) '

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

_cell_length_a                   8.0494(7)
_cell_length_b                   15.8108(12)
_cell_length_c                   20.486(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2607.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5069
_cell_measurement_theta_min      0.99
_cell_measurement_theta_max      25.990

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             968
_exptl_absorpt_coefficient_mu    0.061
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12407
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_sigmaI/netI    0.0979
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.84
_diffrn_reflns_theta_max         25.99
_reflns_number_total             5069
_reflns_number_gt                3572
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0822P)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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(4)
_refine_ls_number_reflns         5069
_refine_ls_number_parameters     345
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.0620
_refine_ls_wR_factor_ref         0.1429
_refine_ls_wR_factor_gt          0.1271
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_restrained_S_all      0.953
_refine_ls_shift/su_max          0.092
_refine_ls_shift/su_mean         0.003

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
C29 C -0.0294(3) 0.53543(18) 0.11970(13) 0.0227(6) Uani 1 1 d . . .
H29 H -0.0715 0.5841 0.0981 0.027 Uiso 1 1 calc R . .
C30 C -0.0084(3) 0.53750(18) 0.18711(13) 0.0252(7) Uani 1 1 d . . .
C14 C 0.0746(3) 0.29013(17) -0.13949(13) 0.0202(6) Uani 1 1 d . . .
C28 C 0.0095(3) 0.46389(18) 0.08292(12) 0.0187(6) Uani 1 1 d . . .
C2 C 0.0236(3) 0.37387(17) -0.11035(13) 0.0187(6) Uani 1 1 d . . .
N1 N 0.4145(3) 0.34133(19) -0.05515(13) 0.0281(6) Uani 1 1 d . . .
C15 C 0.0571(4) 0.21471(17) -0.10542(14) 0.0264(7) Uani 1 1 d . . .
H15 H 0.0163 0.2153 -0.0619 0.032 Uiso 1 1 calc R . .
C33 C 0.0649(4) 0.39280(17) 0.11730(13) 0.0232(7) Uani 1 1 d . . .
H33 H 0.0847 0.3419 0.0939 0.028 Uiso 1 1 calc R . .
C16 C 0.0988(4) 0.13845(18) -0.13462(15) 0.0305(8) Uani 1 1 d . . .
H16 H 0.0881 0.0872 -0.1107 0.037 Uiso 1 1 calc R . .
C22 C 0.5165(3) 0.67413(16) -0.03885(15) 0.0241(7) Uani 1 1 d . . .
C19 C 0.1355(4) 0.28756(19) -0.20282(13) 0.0271(7) Uani 1 1 d . . .
H19 H 0.1512 0.3388 -0.2263 0.033 Uiso 1 1 calc R . .
C17 C 0.1559(4) 0.1365(2) -0.19821(16) 0.0364(8) Uani 1 1 d . . .
H17 H 0.1828 0.0842 -0.2183 0.044 Uiso 1 1 calc R . .
C21 C 0.3868(4) 0.62413(16) -0.06084(14) 0.0232(7) Uani 1 1 d . . .
H21 H 0.3564 0.6274 -0.1056 0.028 Uiso 1 1 calc R . .
B5 B -0.0067(4) 0.4668(2) 0.00616(15) 0.0191(7) Uani 1 1 d . . .
C32 C 0.0919(4) 0.39373(17) 0.18430(14) 0.0256(7) Uani 1 1 d . . .
C31 C 0.0552(4) 0.46673(18) 0.21828(13) 0.0266(7) Uani 1 1 d . . .
H31 H 0.0739 0.4685 0.2640 0.032 Uiso 1 1 calc R . .
B8 B -0.2018(4) 0.4653(2) -0.03514(16) 0.0228(7) Uani 1 1 d . . .
H8 H -0.3217 0.4677 -0.0074 0.027 Uiso 1 1 calc R . .
B11 B -0.0374(4) 0.4565(2) -0.15928(15) 0.0221(7) Uani 1 1 d . . .
H11 H -0.0476 0.4522 -0.2137 0.027 Uiso 1 1 calc R . .
C20 C 0.2986(3) 0.56919(16) -0.02024(14) 0.0188(6) Uani 1 1 d . . .
C24 C 0.4778(4) 0.61526(19) 0.06898(14) 0.0261(7) Uani 1 1 d . . .
C25 C 0.3498(3) 0.56551(18) 0.04502(14) 0.0228(7) Uani 1 1 d . . .
H25 H 0.2949 0.5276 0.0739 0.027 Uiso 1 1 calc R . .
B7 B -0.1810(4) 0.4040(2) -0.10749(17) 0.0235(8) Uani 1 1 d . . .
H7 H -0.2856 0.3651 -0.1275 0.028 Uiso 1 1 calc R . .
B3 B 0.1584(4) 0.45873(19) -0.11940(15) 0.0185(7) Uani 1 1 d . . .
H3 H 0.2781 0.4550 -0.1471 0.022 Uiso 1 1 calc R . .
C34 C -0.0525(4) 0.61558(18) 0.22614(14) 0.0352(8) Uani 1 1 d . . .
H34A H -0.1735 0.6215 0.2282 0.053 Uiso 1 1 calc R . .
H34B H -0.0046 0.6656 0.2051 0.053 Uiso 1 1 calc R . .
H34C H -0.0078 0.6102 0.2704 0.053 Uiso 1 1 calc R . .
C18 C 0.1735(4) 0.2112(2) -0.23217(15) 0.0344(8) Uani 1 1 d . . .
H18 H 0.2119 0.2103 -0.2760 0.041 Uiso 1 1 calc R . .
B4 B 0.1415(4) 0.52135(18) -0.04657(15) 0.0189(7) Uani 1 1 d . . .
C1 C 0.1275(3) 0.41146(15) -0.04457(13) 0.0169(6) Uani 1 1 d . . .
B12 B -0.1786(4) 0.5167(2) -0.11190(17) 0.0245(8) Uani 1 1 d . . .
H12 H -0.2828 0.5532 -0.1347 0.029 Uiso 1 1 calc R . .
C13 C 0.2670(4) 0.35677(18) -0.01651(15) 0.0202(7) Uani 1 1 d . . .
B10 B 0.0317(4) 0.5495(2) -0.11989(15) 0.0220(8) Uani 1 1 d . . .
H10 H 0.0665 0.6072 -0.1484 0.026 Uiso 1 1 calc R . .
B6 B -0.0737(4) 0.3745(2) -0.03547(16) 0.0210(7) Uani 1 1 d . . .
H6 H -0.1061 0.3156 -0.0080 0.025 Uiso 1 1 calc R . .
B9 B -0.0706(4) 0.5558(2) -0.04219(16) 0.0222(8) Uani 1 1 d . . .
H9 H -0.1035 0.6178 -0.0191 0.027 Uiso 1 1 calc R . .
C23 C 0.5586(4) 0.66985(18) 0.02708(15) 0.0269(7) Uani 1 1 d . . .
H23 H 0.6444 0.7052 0.0435 0.032 Uiso 1 1 calc R . .
C35 C 0.1585(5) 0.31688(19) 0.21923(16) 0.0412(9) Uani 1 1 d . . .
H35A H 0.2800 0.3200 0.2211 0.062 Uiso 1 1 calc R . .
H35B H 0.1252 0.2657 0.1956 0.062 Uiso 1 1 calc R . .
H35C H 0.1135 0.3150 0.2636 0.062 Uiso 1 1 calc R . .
C27 C 0.5236(4) 0.6111(2) 0.14108(14) 0.0423(9) Uani 1 1 d . . .
H27A H 0.4309 0.5867 0.1658 0.063 Uiso 1 1 calc R . .
H27B H 0.5467 0.6682 0.1572 0.063 Uiso 1 1 calc R . .
H27C H 0.6225 0.5756 0.1466 0.063 Uiso 1 1 calc R . .
C26 C 0.6106(4) 0.73213(18) -0.08414(16) 0.0377(9) Uani 1 1 d . . .
H26A H 0.7254 0.7123 -0.0884 0.056 Uiso 1 1 calc R . .
H26B H 0.6101 0.7897 -0.0663 0.056 Uiso 1 1 calc R . .
H26C H 0.5573 0.7321 -0.1271 0.056 Uiso 1 1 calc R . .
H13B H 0.221(3) 0.2989(17) -0.0044(13) 0.024(8) Uiso 1 1 d . . .
H13A H 0.299(3) 0.3820(16) 0.0229(14) 0.015(7) Uiso 1 1 d . . .
H1A H 0.393(4) 0.3150(19) -0.0919(16) 0.038(10) Uiso 1 1 d . . .
H1B H 0.474(5) 0.389(2) -0.0694(17) 0.065(13) Uiso 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
C29 C30 1.392(4) . ?
C29 C28 1.395(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.386(4) . ?
C30 C34 1.513(4) . ?
C14 C19 1.388(4) . ?
C14 C15 1.389(4) . ?
C14 C2 1.509(4) . ?
C28 C33 1.399(4) . ?
C28 B5 1.578(4) . ?
C2 C1 1.694(4) . ?
C2 B7 1.715(4) . ?
C2 B11 1.718(4) . ?
C2 B6 1.722(4) . ?
C2 B3 1.736(4) . ?
N1 C13 1.448(4) . ?
N1 H1A 0.88(3) . ?
N1 H1B 0.94(4) . ?
C15 C16 1.387(4) . ?
C15 H15 0.9500 . ?
C33 C32 1.390(4) . ?
C33 H33 0.9500 . ?
C16 C17 1.382(4) . ?
C16 H16 0.9500 . ?
C22 C21 1.385(4) . ?
C22 C23 1.394(4) . ?
C22 C26 1.508(4) . ?
C19 C18 1.383(4) . ?
C19 H19 0.9500 . ?
C17 C18 1.378(4) . ?
C17 H17 0.9500 . ?
C21 C20 1.397(4) . ?
C21 H21 0.9500 . ?
B5 C1 1.736(4) . ?
B5 B6 1.774(4) . ?
B5 B8 1.784(4) . ?
B5 B9 1.796(4) . ?
B5 B4 1.826(4) . ?
C32 C31 1.380(4) . ?
C32 C35 1.508(4) . ?
C31 H31 0.9500 . ?
B8 B6 1.768(5) . ?
B8 B7 1.779(5) . ?
B8 B12 1.779(5) . ?
B8 B9 1.783(4) . ?
B8 H8 1.1200 . ?
B11 B10 1.767(4) . ?
B11 B12 1.772(5) . ?
B11 B7 1.775(5) . ?
B11 B3 1.775(4) . ?
B11 H11 1.1200 . ?
C20 C25 1.400(4) . ?
C20 B4 1.569(4) . ?
C24 C23 1.380(4) . ?
C24 C25 1.386(4) . ?
C24 C27 1.524(4) . ?
C25 H25 0.9500 . ?
B7 B6 1.772(5) . ?
B7 B12 1.784(4) . ?
B7 H7 1.1200 . ?
B3 C1 1.724(4) . ?
B3 B10 1.760(4) . ?
B3 B4 1.796(4) . ?
B3 H3 1.1200 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C18 H18 0.9500 . ?
B4 C1 1.742(4) . ?
B4 B9 1.795(4) . ?
B4 B10 1.799(4) . ?
C1 C13 1.530(4) . ?
C1 B6 1.731(4) . ?
B12 B10 1.778(5) . ?
B12 B9 1.782(5) . ?
B12 H12 1.1200 . ?
C13 H13B 1.02(3) . ?
C13 H13A 0.94(3) . ?
B10 B9 1.795(5) . ?
B10 H10 1.1200 . ?
B6 H6 1.1200 . ?
B9 H9 1.1200 . ?
C23 H23 0.9500 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 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
C30 C29 C28 121.9(3) . . ?
C30 C29 H29 119.1 . . ?
C28 C29 H29 119.1 . . ?
C29 C30 C31 118.9(3) . . ?
C29 C30 C34 121.0(3) . . ?
C31 C30 C34 120.1(2) . . ?
C19 C14 C15 118.7(3) . . ?
C19 C14 C2 119.5(2) . . ?
C15 C14 C2 121.8(2) . . ?
C29 C28 C33 116.8(2) . . ?
C29 C28 B5 119.7(3) . . ?
C33 C28 B5 123.4(3) . . ?
C14 C2 C1 119.2(2) . . ?
C14 C2 B7 121.2(2) . . ?
C1 C2 B7 110.5(2) . . ?
C14 C2 B11 120.9(2) . . ?
C1 C2 B11 109.8(2) . . ?
B7 C2 B11 62.27(18) . . ?
C14 C2 B6 118.8(2) . . ?
C1 C2 B6 60.91(16) . . ?
B7 C2 B6 62.06(19) . . ?
B11 C2 B6 112.7(2) . . ?
C14 C2 B3 117.8(2) . . ?
C1 C2 B3 60.33(16) . . ?
B7 C2 B3 112.9(2) . . ?
B11 C2 B3 61.86(17) . . ?
B6 C2 B3 112.0(2) . . ?
C13 N1 H1A 113(2) . . ?
C13 N1 H1B 117(2) . . ?
H1A N1 H1B 102(3) . . ?
C14 C15 C16 120.3(3) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C32 C33 C28 122.6(3) . . ?
C32 C33 H33 118.7 . . ?
C28 C33 H33 118.7 . . ?
C17 C16 C15 120.4(3) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C21 C22 C23 118.1(3) . . ?
C21 C22 C26 121.7(3) . . ?
C23 C22 C26 120.2(3) . . ?
C18 C19 C14 120.7(3) . . ?
C18 C19 H19 119.7 . . ?
C14 C19 H19 119.7 . . ?
C16 C17 C18 119.4(3) . . ?
C16 C17 H17 120.3 . . ?
C18 C17 H17 120.3 . . ?
C22 C21 C20 123.0(3) . . ?
C22 C21 H21 118.5 . . ?
C20 C21 H21 118.5 . . ?
C28 B5 C1 122.0(2) . . ?
C28 B5 B6 118.7(2) . . ?
C1 B5 B6 59.12(16) . . ?
C28 B5 B8 123.0(2) . . ?
C1 B5 B8 104.9(2) . . ?
B6 B5 B8 59.57(18) . . ?
C28 B5 B9 126.6(2) . . ?
C1 B5 B9 104.1(2) . . ?
B6 B5 B9 107.0(2) . . ?
B8 B5 B9 59.75(18) . . ?
C28 B5 B4 123.3(2) . . ?
C1 B5 B4 58.49(15) . . ?
B6 B5 B4 107.6(2) . . ?
B8 B5 B4 107.5(2) . . ?
B9 B5 B4 59.40(17) . . ?
C31 C32 C33 118.3(3) . . ?
C31 C32 C35 120.7(3) . . ?
C33 C32 C35 121.0(3) . . ?
C32 C31 C30 121.5(3) . . ?
C32 C31 H31 119.3 . . ?
C30 C31 H31 119.3 . . ?
B6 B8 B5 59.92(18) . . ?
B6 B8 B7 59.95(18) . . ?
B5 B8 B7 108.6(2) . . ?
B6 B8 B12 107.8(2) . . ?
B5 B8 B12 108.7(2) . . ?
B7 B8 B12 60.17(18) . . ?
B6 B8 B9 107.8(2) . . ?
B5 B8 B9 60.45(18) . . ?
B7 B8 B9 108.3(2) . . ?
B12 B8 B9 60.05(18) . . ?
B6 B8 H8 122.1 . . ?
B5 B8 H8 121.2 . . ?
B7 B8 H8 121.4 . . ?
B12 B8 H8 121.6 . . ?
B9 B8 H8 121.6 . . ?
C2 B11 B10 106.0(2) . . ?
C2 B11 B12 105.8(2) . . ?
B10 B11 B12 60.33(18) . . ?
C2 B11 B7 58.79(17) . . ?
B10 B11 B7 108.7(2) . . ?
B12 B11 B7 60.38(18) . . ?
C2 B11 B3 59.55(17) . . ?
B10 B11 B3 59.60(18) . . ?
B12 B11 B3 107.9(2) . . ?
B7 B11 B3 108.2(2) . . ?
C2 B11 H11 123.8 . . ?
B10 B11 H11 121.9 . . ?
B12 B11 H11 122.1 . . ?
B7 B11 H11 121.3 . . ?
B3 B11 H11 121.6 . . ?
C21 C20 C25 116.4(2) . . ?
C21 C20 B4 120.3(2) . . ?
C25 C20 B4 123.0(2) . . ?
C23 C24 C25 119.0(3) . . ?
C23 C24 C27 121.1(3) . . ?
C25 C24 C27 119.9(3) . . ?
C24 C25 C20 122.2(3) . . ?
C24 C25 H25 118.9 . . ?
C20 C25 H25 118.9 . . ?
C2 B7 B11 58.94(17) . . ?
C2 B7 B6 59.16(18) . . ?
B11 B7 B6 107.6(2) . . ?
C2 B7 B8 105.7(2) . . ?
B11 B7 B8 107.7(2) . . ?
B6 B7 B8 59.70(18) . . ?
C2 B7 B12 105.4(2) . . ?
B11 B7 B12 59.71(19) . . ?
B6 B7 B12 107.4(2) . . ?
B8 B7 B12 59.91(19) . . ?
C2 B7 H7 123.8 . . ?
B11 B7 H7 121.8 . . ?
B6 B7 H7 121.8 . . ?
B8 B7 H7 122.3 . . ?
B12 B7 H7 122.5 . . ?
C1 B3 C2 58.62(16) . . ?
C1 B3 B10 105.9(2) . . ?
C2 B3 B10 105.6(2) . . ?
C1 B3 B11 105.8(2) . . ?
C2 B3 B11 58.59(17) . . ?
B10 B3 B11 59.96(17) . . ?
C1 B3 B4 59.28(16) . . ?
C2 B3 B4 106.9(2) . . ?
B10 B3 B4 60.76(17) . . ?
B11 B3 B4 109.0(2) . . ?
C1 B3 H3 123.5 . . ?
C2 B3 H3 123.5 . . ?
B10 B3 H3 122.6 . . ?
B11 B3 H3 122.0 . . ?
B4 B3 H3 121.0 . . ?
C30 C34 H34A 109.5 . . ?
C30 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C30 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C17 C18 C19 120.4(3) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C20 B4 C1 121.7(2) . . ?
C20 B4 B9 127.1(2) . . ?
C1 B4 B9 103.8(2) . . ?
C20 B4 B3 119.4(2) . . ?
C1 B4 B3 58.29(16) . . ?
B9 B4 B3 106.3(2) . . ?
C20 B4 B10 124.3(2) . . ?
C1 B4 B10 103.5(2) . . ?
B9 B4 B10 59.93(19) . . ?
B3 B4 B10 58.64(17) . . ?
C20 B4 B5 123.4(2) . . ?
C1 B4 B5 58.16(17) . . ?
B9 B4 B5 59.45(17) . . ?
B3 B4 B5 106.3(2) . . ?
B10 B4 B5 106.8(2) . . ?
C13 C1 C2 117.6(2) . . ?
C13 C1 B6 117.1(2) . . ?
C2 C1 B6 60.37(17) . . ?
C13 C1 B3 118.3(2) . . ?
C2 C1 B3 61.04(16) . . ?
B6 C1 B3 112.2(2) . . ?
C13 C1 B5 121.1(2) . . ?
C2 C1 B5 110.3(2) . . ?
B6 C1 B5 61.54(17) . . ?
B3 C1 B5 113.8(2) . . ?
C13 C1 B4 121.7(2) . . ?
C2 C1 B4 111.3(2) . . ?
B6 C1 B4 113.6(2) . . ?
B3 C1 B4 62.43(17) . . ?
B5 C1 B4 63.36(17) . . ?
B11 B12 B10 59.69(18) . . ?
B11 B12 B9 108.2(2) . . ?
B10 B12 B9 60.55(19) . . ?
B11 B12 B8 107.9(2) . . ?
B10 B12 B8 108.3(2) . . ?
B9 B12 B8 60.09(18) . . ?
B11 B12 B7 59.91(19) . . ?
B10 B12 B7 107.8(2) . . ?
B9 B12 B7 108.1(2) . . ?
B8 B12 B7 59.92(19) . . ?
B11 B12 H12 121.9 . . ?
B10 B12 H12 121.6 . . ?
B9 B12 H12 121.4 . . ?
B8 B12 H12 121.7 . . ?
B7 B12 H12 121.8 . . ?
N1 C13 C1 119.5(2) . . ?
N1 C13 H13B 106.3(15) . . ?
C1 C13 H13B 109.4(16) . . ?
N1 C13 H13A 108.7(16) . . ?
C1 C13 H13A 106.5(15) . . ?
H13B C13 H13A 106(2) . . ?
B3 B10 B11 60.44(17) . . ?
B3 B10 B12 108.3(2) . . ?
B11 B10 B12 59.98(19) . . ?
B3 B10 B9 107.8(2) . . ?
B11 B10 B9 107.9(2) . . ?
B12 B10 B9 59.85(19) . . ?
B3 B10 B4 60.60(17) . . ?
B11 B10 B4 109.3(2) . . ?
B12 B10 B4 108.6(2) . . ?
B9 B10 B4 59.92(18) . . ?
B3 B10 H10 121.5 . . ?
B11 B10 H10 121.3 . . ?
B12 B10 H10 121.6 . . ?
B9 B10 H10 122.2 . . ?
B4 B10 H10 120.9 . . ?
C2 B6 C1 58.73(16) . . ?
C2 B6 B8 105.9(2) . . ?
C1 B6 B8 105.8(2) . . ?
C2 B6 B5 107.2(2) . . ?
C1 B6 B5 59.34(17) . . ?
B8 B6 B5 60.50(17) . . ?
C2 B6 B7 58.78(18) . . ?
C1 B6 B7 106.1(2) . . ?
B8 B6 B7 60.36(18) . . ?
B5 B6 B7 109.4(2) . . ?
C2 B6 H6 123.3 . . ?
C1 B6 H6 123.5 . . ?
B8 B6 H6 122.6 . . ?
B5 B6 H6 120.9 . . ?
B7 B6 H6 121.6 . . ?
B12 B9 B8 59.87(18) . . ?
B12 B9 B10 59.61(19) . . ?
B8 B9 B10 107.4(2) . . ?
B12 B9 B4 108.6(2) . . ?
B8 B9 B4 108.9(2) . . ?
B10 B9 B4 60.15(18) . . ?
B12 B9 B5 108.1(2) . . ?
B8 B9 B5 59.80(17) . . ?
B10 B9 B5 108.3(2) . . ?
B4 B9 B5 61.14(17) . . ?
B12 B9 H9 121.8 . . ?
B8 B9 H9 121.9 . . ?
B10 B9 H9 122.1 . . ?
B4 B9 H9 120.7 . . ?
B5 B9 H9 121.3 . . ?
C24 C23 C22 121.2(3) . . ?
C24 C23 H23 119.4 . . ?
C22 C23 H23 119.4 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C22 C26 H26A 109.5 . . ?
C22 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C22 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.225
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.052
####################################################################### 
# 
# 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_34
_database_code_depnum_ccdc_archive 'CCDC 1583782'
_audit_update_record             
;
2017-11-03 deposited with the CCDC.
2018-03-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H28 B10 N2 O2 S'
_chemical_formula_weight         480.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.7385(6)
_cell_length_b                   10.4142(8)
_cell_length_c                   15.9824(11)
_cell_angle_alpha                92.169(3)
_cell_angle_beta                 102.976(2)
_cell_angle_gamma                99.951(3)
_cell_volume                     1232.30(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    4473
_cell_measurement_theta_min      0.991
_cell_measurement_theta_max      25.320

_exptl_crystal_description       Block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             500
_exptl_absorpt_coefficient_mu    0.156
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9903
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_sigmaI/netI    0.0835
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.75
_diffrn_reflns_theta_max         25.32
_reflns_number_total             4473
_reflns_number_gt                3091
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0861P)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         4473
_refine_ls_number_parameters     345
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0530
_refine_ls_wR_factor_ref         0.1362
_refine_ls_wR_factor_gt          0.1212
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_restrained_S_all      0.893
_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
O1 O 1.1202(2) 0.35589(19) 1.03550(11) 0.0263(5) Uani 1 1 d . . .
S1 S 1.20987(8) 0.38260(7) 0.96725(4) 0.01718(19) Uani 1 1 d . . .
O2 O 1.3827(2) 0.34652(19) 0.97538(12) 0.0254(5) Uani 1 1 d . . .
C2 C 0.9055(3) 0.4772(2) 0.69542(16) 0.0150(6) Uani 1 1 d . . .
N1 N 1.0641(3) 0.3104(2) 0.88314(14) 0.0206(6) Uani 1 1 d . . .
C21 C 0.7827(3) 0.0359(3) 0.81987(17) 0.0195(6) Uani 1 1 d . . .
H21 H 0.8328 0.0063 0.7753 0.023 Uiso 1 1 calc R . .
C13 C 1.0918(3) 0.3099(3) 0.79627(16) 0.0160(6) Uani 1 1 d . . .
C18 C 1.1542(4) 0.7969(3) 0.81793(18) 0.0252(7) Uani 1 1 d . . .
H18 H 1.1318 0.8612 0.8559 0.030 Uiso 1 1 calc R . .
C14 C 1.0551(3) 0.5921(3) 0.73127(16) 0.0167(6) Uani 1 1 d . . .
C1 C 0.9213(3) 0.3240(2) 0.72992(16) 0.0146(6) Uani 1 1 d . . .
C29 C 0.9863(4) -0.1600(3) 0.58464(18) 0.0256(7) Uani 1 1 d . . .
H29 H 1.0206 -0.2395 0.5696 0.031 Uiso 1 1 calc R . .
C25 C 0.6248(3) 0.1835(3) 0.87598(17) 0.0204(6) Uani 1 1 d . . .
H25 H 0.5641 0.2557 0.8700 0.024 Uiso 1 1 calc R . .
C22 C 0.7920(3) -0.0312(3) 0.89394(17) 0.0224(6) Uani 1 1 d . . .
H22 H 0.8472 -0.1061 0.8993 0.027 Uiso 1 1 calc R . .
C27 C 0.7594(4) -0.0412(3) 0.60664(17) 0.0216(6) Uani 1 1 d . . .
H27 H 0.6365 -0.0408 0.6061 0.026 Uiso 1 1 calc R . .
C15 C 1.2182(3) 0.6109(3) 0.70702(19) 0.0244(7) Uani 1 1 d . . .
H15 H 1.2410 0.5478 0.6684 0.029 Uiso 1 1 calc R . .
C20 C 0.7012(3) 0.1459(2) 0.80964(16) 0.0161(6) Uani 1 1 d . . .
C26 C 0.8852(3) 0.0750(2) 0.62940(15) 0.0162(6) Uani 1 1 d . . .
C28 C 0.8092(4) -0.1567(3) 0.58480(17) 0.0247(7) Uani 1 1 d . . .
H28 H 0.7206 -0.2344 0.5698 0.030 Uiso 1 1 calc R . .
C24 C 0.6356(4) 0.1178(3) 0.95024(18) 0.0240(7) Uani 1 1 d . . .
H24 H 0.5843 0.1461 0.9947 0.029 Uiso 1 1 calc R . .
C19 C 1.0246(3) 0.6867(3) 0.78757(16) 0.0202(6) Uani 1 1 d . . .
H19 H 0.9139 0.6751 0.8051 0.024 Uiso 1 1 calc R . .
C23 C 0.7209(4) 0.0110(3) 0.95989(18) 0.0267(7) Uani 1 1 d . . .
H23 H 0.7305 -0.0329 1.0113 0.032 Uiso 1 1 calc R . .
C31 C 1.0632(3) 0.0697(3) 0.62813(17) 0.0203(6) Uani 1 1 d . . .
H31 H 1.1520 0.1474 0.6423 0.024 Uiso 1 1 calc R . .
C16 C 1.3478(4) 0.7212(3) 0.7389(2) 0.0324(8) Uani 1 1 d . . .
H16 H 1.4601 0.7325 0.7227 0.039 Uiso 1 1 calc R . .
B4 B 0.7119(4) 0.2372(3) 0.73354(19) 0.0164(7) Uani 1 1 d . . .
B11 B 0.6857(4) 0.4967(3) 0.6752(2) 0.0194(7) Uani 1 1 d . . .
H11 H 0.6434 0.5928 0.6843 0.023 Uiso 1 1 calc R . .
C17 C 1.3159(4) 0.8144(3) 0.79353(19) 0.0298(7) Uani 1 1 d . . .
H17 H 1.4049 0.8905 0.8144 0.036 Uiso 1 1 calc R . .
C30 C 1.1137(4) -0.0459(3) 0.60672(18) 0.0245(7) Uani 1 1 d . . .
H30 H 1.2364 -0.0470 0.6072 0.029 Uiso 1 1 calc R . .
B6 B 0.9414(4) 0.3570(3) 0.62784(18) 0.0160(6) Uani 1 1 d . . .
H6 H 1.0713 0.3613 0.6073 0.019 Uiso 1 1 calc R . .
B5 B 0.8156(4) 0.2046(3) 0.64603(18) 0.0154(6) Uani 1 1 d . . .
B10 B 0.5618(4) 0.3471(3) 0.6978(2) 0.0194(7) Uani 1 1 d . . .
H10 H 0.4366 0.3444 0.7223 0.023 Uiso 1 1 calc R . .
B9 B 0.5837(4) 0.2219(3) 0.6245(2) 0.0193(7) Uani 1 1 d . . .
H9 H 0.4721 0.1362 0.5995 0.023 Uiso 1 1 calc R . .
B3 B 0.7767(4) 0.4109(3) 0.76396(19) 0.0156(6) Uani 1 1 d . . .
H3 H 0.7975 0.4510 0.8322 0.019 Uiso 1 1 calc R . .
B8 B 0.7259(4) 0.2944(3) 0.5585(2) 0.0188(7) Uani 1 1 d . . .
H8 H 0.7098 0.2570 0.4900 0.023 Uiso 1 1 calc R . .
B7 B 0.7890(4) 0.4633(3) 0.59034(19) 0.0195(7) Uani 1 1 d . . .
H7 H 0.8158 0.5369 0.5433 0.023 Uiso 1 1 calc R . .
B12 B 0.5671(4) 0.3792(3) 0.5900(2) 0.0215(7) Uani 1 1 d . . .
H12 H 0.4445 0.3968 0.5427 0.026 Uiso 1 1 calc R . .
N2 N 1.2353(4) 0.5316(2) 0.94531(16) 0.0250(6) Uani 1 1 d . . .
H13A H 1.125(3) 0.225(3) 0.7821(17) 0.019(7) Uiso 1 1 d . . .
H13B H 1.184(3) 0.383(3) 0.7924(15) 0.013(7) Uiso 1 1 d . . .
H2A H 1.147(4) 0.567(3) 0.9492(19) 0.029(9) Uiso 1 1 d . . .
H1A H 1.004(4) 0.250(3) 0.8964(18) 0.023(9) Uiso 1 1 d . . .
H2B H 1.344(5) 0.576(3) 0.964(2) 0.037(9) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 S1 1.4301(19) . ?
S1 O2 1.4305(19) . ?
S1 N2 1.592(3) . ?
S1 N1 1.610(2) . ?
C2 C14 1.507(3) . ?
C2 B11 1.708(4) . ?
C2 B7 1.706(4) . ?
C2 B6 1.722(4) . ?
C2 C1 1.723(4) . ?
C2 B3 1.727(4) . ?
N1 C13 1.452(3) . ?
N1 H1A 0.79(3) . ?
C21 C22 1.392(4) . ?
C21 C20 1.398(4) . ?
C21 H21 0.9500 . ?
C13 C1 1.529(3) . ?
C13 H13A 1.00(3) . ?
C13 H13B 0.96(2) . ?
C18 C19 1.378(4) . ?
C18 C17 1.377(4) . ?
C18 H18 0.9500 . ?
C14 C15 1.386(4) . ?
C14 C19 1.394(4) . ?
C1 B6 1.715(4) . ?
C1 B3 1.718(4) . ?
C1 B4 1.728(3) . ?
C1 B5 1.745(4) . ?
C29 C28 1.378(4) . ?
C29 C30 1.385(4) . ?
C29 H29 0.9500 . ?
C25 C24 1.386(4) . ?
C25 C20 1.399(4) . ?
C25 H25 0.9500 . ?
C22 C23 1.384(4) . ?
C22 H22 0.9500 . ?
C27 C28 1.381(4) . ?
C27 C26 1.395(3) . ?
C27 H27 0.9500 . ?
C15 C16 1.383(4) . ?
C15 H15 0.9500 . ?
C20 B4 1.579(4) . ?
C26 C31 1.392(4) . ?
C26 B5 1.571(4) . ?
C28 H28 0.9500 . ?
C24 C23 1.384(4) . ?
C24 H24 0.9500 . ?
C19 H19 0.9500 . ?
C23 H23 0.9500 . ?
C31 C30 1.382(4) . ?
C31 H31 0.9500 . ?
C16 C17 1.372(4) . ?
C16 H16 0.9500 . ?
B4 B10 1.789(4) . ?
B4 B9 1.788(4) . ?
B4 B3 1.809(4) . ?
B4 B5 1.810(4) . ?
B11 B12 1.766(4) . ?
B11 B7 1.773(4) . ?
B11 B10 1.777(4) . ?
B11 B3 1.781(4) . ?
B11 H11 1.1200 . ?
C17 H17 0.9500 . ?
C30 H30 0.9500 . ?
B6 B7 1.778(4) . ?
B6 B8 1.781(4) . ?
B6 B5 1.783(4) . ?
B6 H6 1.1200 . ?
B5 B9 1.792(4) . ?
B5 B8 1.789(4) . ?
B10 B3 1.761(4) . ?
B10 B9 1.775(4) . ?
B10 B12 1.774(4) . ?
B10 H10 1.1200 . ?
B9 B12 1.764(4) . ?
B9 B8 1.785(4) . ?
B9 H9 1.1200 . ?
B3 H3 1.1200 . ?
B8 B7 1.765(4) . ?
B8 B12 1.779(5) . ?
B8 H8 1.1200 . ?
B7 B12 1.787(4) . ?
B7 H7 1.1200 . ?
B12 H12 1.1200 . ?
N2 H2A 0.84(3) . ?
N2 H2B 0.87(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 S1 O2 117.77(12) . . ?
O1 S1 N2 114.00(14) . . ?
O2 S1 N2 105.89(13) . . ?
O1 S1 N1 103.44(12) . . ?
O2 S1 N1 112.43(12) . . ?
N2 S1 N1 102.37(14) . . ?
C14 C2 B11 120.0(2) . . ?
C14 C2 B7 121.2(2) . . ?
B11 C2 B7 62.59(17) . . ?
C14 C2 B6 119.6(2) . . ?
B11 C2 B6 113.1(2) . . ?
B7 C2 B6 62.48(17) . . ?
C14 C2 C1 120.2(2) . . ?
B11 C2 C1 109.60(18) . . ?
B7 C2 C1 109.70(19) . . ?
B6 C2 C1 59.73(15) . . ?
C14 C2 B3 117.5(2) . . ?
B11 C2 B3 62.48(16) . . ?
B7 C2 B3 113.29(19) . . ?
B6 C2 B3 110.97(19) . . ?
C1 C2 B3 59.75(15) . . ?
C13 N1 S1 124.66(18) . . ?
C13 N1 H1A 119(2) . . ?
S1 N1 H1A 109(2) . . ?
C22 C21 C20 121.5(3) . . ?
C22 C21 H21 119.3 . . ?
C20 C21 H21 119.3 . . ?
N1 C13 C1 111.9(2) . . ?
N1 C13 H13A 108.2(15) . . ?
C1 C13 H13A 108.3(15) . . ?
N1 C13 H13B 109.6(15) . . ?
C1 C13 H13B 106.6(15) . . ?
H13A C13 H13B 112(2) . . ?
C19 C18 C17 120.3(3) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C15 C14 C19 118.7(2) . . ?
C15 C14 C2 122.6(2) . . ?
C19 C14 C2 118.7(2) . . ?
C13 C1 B6 117.9(2) . . ?
C13 C1 B3 117.1(2) . . ?
B6 C1 B3 111.7(2) . . ?
C13 C1 C2 117.7(2) . . ?
B6 C1 C2 60.10(15) . . ?
B3 C1 C2 60.25(15) . . ?
C13 C1 B4 121.3(2) . . ?
B6 C1 B4 113.65(19) . . ?
B3 C1 B4 63.31(16) . . ?
C2 C1 B4 111.10(19) . . ?
C13 C1 B5 122.1(2) . . ?
B6 C1 B5 62.04(16) . . ?
B3 C1 B5 113.98(19) . . ?
C2 C1 B5 110.04(19) . . ?
B4 C1 B5 62.84(16) . . ?
C28 C29 C30 119.0(3) . . ?
C28 C29 H29 120.5 . . ?
C30 C29 H29 120.5 . . ?
C24 C25 C20 121.5(3) . . ?
C24 C25 H25 119.3 . . ?
C20 C25 H25 119.3 . . ?
C23 C22 C21 120.1(3) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C28 C27 C26 121.6(3) . . ?
C28 C27 H27 119.2 . . ?
C26 C27 H27 119.2 . . ?
C16 C15 C14 120.2(3) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C21 C20 C25 117.2(2) . . ?
C21 C20 B4 123.3(2) . . ?
C25 C20 B4 119.1(2) . . ?
C31 C26 C27 117.0(3) . . ?
C31 C26 B5 124.2(2) . . ?
C27 C26 B5 118.5(2) . . ?
C29 C28 C27 120.5(3) . . ?
C29 C28 H28 119.8 . . ?
C27 C28 H28 119.8 . . ?
C23 C24 C25 120.3(3) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
C18 C19 C14 120.4(2) . . ?
C18 C19 H19 119.8 . . ?
C14 C19 H19 119.8 . . ?
C24 C23 C22 119.4(3) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
C30 C31 C26 121.6(2) . . ?
C30 C31 H31 119.2 . . ?
C26 C31 H31 119.2 . . ?
C17 C16 C15 120.7(3) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
C20 B4 C1 117.8(2) . . ?
C20 B4 B10 125.2(2) . . ?
C1 B4 B10 103.8(2) . . ?
C20 B4 B9 131.4(2) . . ?
C1 B4 B9 104.4(2) . . ?
B10 B4 B9 59.52(17) . . ?
C20 B4 B3 116.1(2) . . ?
C1 B4 B3 58.09(15) . . ?
B10 B4 B3 58.61(16) . . ?
B9 B4 B3 105.8(2) . . ?
C20 B4 B5 124.0(2) . . ?
C1 B4 B5 59.03(15) . . ?
B10 B4 B5 107.2(2) . . ?
B9 B4 B5 59.73(16) . . ?
B3 B4 B5 106.72(19) . . ?
C2 B11 B12 106.1(2) . . ?
C2 B11 B7 58.66(16) . . ?
B12 B11 B7 60.64(18) . . ?
C2 B11 B10 105.7(2) . . ?
B12 B11 B10 60.11(17) . . ?
B7 B11 B10 108.3(2) . . ?
C2 B11 B3 59.29(16) . . ?
B12 B11 B3 107.6(2) . . ?
B7 B11 B3 107.6(2) . . ?
B10 B11 B3 59.32(16) . . ?
C2 B11 H11 123.7 . . ?
B12 B11 H11 121.9 . . ?
B7 B11 H11 121.5 . . ?
B10 B11 H11 122.2 . . ?
B3 B11 H11 122.1 . . ?
C16 C17 C18 119.6(3) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 H17 120.2 . . ?
C31 C30 C29 120.3(3) . . ?
C31 C30 H30 119.9 . . ?
C29 C30 H30 119.9 . . ?
C1 B6 C2 60.16(15) . . ?
C1 B6 B7 106.8(2) . . ?
C2 B6 B7 58.33(16) . . ?
C1 B6 B8 106.02(19) . . ?
C2 B6 B8 105.2(2) . . ?
B7 B6 B8 59.47(17) . . ?
C1 B6 B5 59.79(15) . . ?
C2 B6 B5 108.3(2) . . ?
B7 B6 B5 108.8(2) . . ?
B8 B6 B5 60.26(16) . . ?
C1 B6 H6 122.5 . . ?
C2 B6 H6 122.8 . . ?
B7 B6 H6 122.2 . . ?
B8 B6 H6 123.3 . . ?
B5 B6 H6 120.7 . . ?
C26 B5 C1 124.5(2) . . ?
C26 B5 B6 119.2(2) . . ?
C1 B5 B6 58.17(15) . . ?
C26 B5 B9 125.5(2) . . ?
C1 B5 B9 103.6(2) . . ?
B6 B5 B9 106.7(2) . . ?
C26 B5 B8 121.0(2) . . ?
C1 B5 B8 104.4(2) . . ?
B6 B5 B8 59.82(16) . . ?
B9 B5 B8 59.80(16) . . ?
C26 B5 B4 124.8(2) . . ?
C1 B5 B4 58.13(15) . . ?
B6 B5 B4 106.6(2) . . ?
B9 B5 B4 59.51(16) . . ?
B8 B5 B4 107.6(2) . . ?
B3 B10 B9 108.4(2) . . ?
B3 B10 B12 108.1(2) . . ?
B9 B10 B12 59.59(17) . . ?
B3 B10 B11 60.45(16) . . ?
B9 B10 B11 107.7(2) . . ?
B12 B10 B11 59.61(17) . . ?
B3 B10 B4 61.26(16) . . ?
B9 B10 B4 60.22(17) . . ?
B12 B10 B4 108.7(2) . . ?
B11 B10 B4 109.8(2) . . ?
B3 B10 H10 121.1 . . ?
B9 B10 H10 122.1 . . ?
B12 B10 H10 122.0 . . ?
B11 B10 H10 121.4 . . ?
B4 B10 H10 120.4 . . ?
B12 B9 B10 60.18(18) . . ?
B12 B9 B8 60.18(17) . . ?
B10 B9 B8 107.9(2) . . ?
B12 B9 B4 109.2(2) . . ?
B10 B9 B4 60.26(17) . . ?
B8 B9 B4 108.7(2) . . ?
B12 B9 B5 108.9(2) . . ?
B10 B9 B5 108.6(2) . . ?
B8 B9 B5 60.02(16) . . ?
B4 B9 B5 60.75(16) . . ?
B12 B9 H9 121.1 . . ?
B10 B9 H9 121.7 . . ?
B8 B9 H9 121.7 . . ?
B4 B9 H9 120.9 . . ?
B5 B9 H9 121.2 . . ?
C1 B3 C2 60.00(15) . . ?
C1 B3 B10 105.4(2) . . ?
C2 B3 B10 105.6(2) . . ?
C1 B3 B11 106.4(2) . . ?
C2 B3 B11 58.24(15) . . ?
B10 B3 B11 60.23(16) . . ?
C1 B3 B4 58.60(15) . . ?
C2 B3 B4 107.2(2) . . ?
B10 B3 B4 60.13(16) . . ?
B11 B3 B4 108.7(2) . . ?
C1 B3 H3 123.2 . . ?
C2 B3 H3 123.0 . . ?
B10 B3 H3 122.9 . . ?
B11 B3 H3 121.9 . . ?
B4 B3 H3 121.5 . . ?
B7 B8 B6 60.17(17) . . ?
B7 B8 B12 60.53(17) . . ?
B6 B8 B12 107.7(2) . . ?
B7 B8 B9 108.0(2) . . ?
B6 B8 B9 107.1(2) . . ?
B12 B8 B9 59.31(17) . . ?
B7 B8 B5 109.1(2) . . ?
B6 B8 B5 59.92(16) . . ?
B12 B8 B5 108.3(2) . . ?
B9 B8 B5 60.18(16) . . ?
B7 B8 H8 121.0 . . ?
B6 B8 H8 122.2 . . ?
B12 B8 H8 121.8 . . ?
B9 B8 H8 122.3 . . ?
B5 B8 H8 121.1 . . ?
C2 B7 B8 106.6(2) . . ?
C2 B7 B11 58.75(16) . . ?
B8 B7 B11 108.1(2) . . ?
C2 B7 B6 59.19(16) . . ?
B8 B7 B6 60.37(17) . . ?
B11 B7 B6 107.4(2) . . ?
C2 B7 B12 105.2(2) . . ?
B8 B7 B12 60.12(17) . . ?
B11 B7 B12 59.46(17) . . ?
B6 B7 B12 107.5(2) . . ?
C2 B7 H7 123.7 . . ?
B8 B7 H7 121.5 . . ?
B11 B7 H7 122.0 . . ?
B6 B7 H7 121.8 . . ?
B12 B7 H7 122.7 . . ?
B9 B12 B11 108.7(2) . . ?
B9 B12 B10 60.23(17) . . ?
B11 B12 B10 60.28(17) . . ?
B9 B12 B8 60.51(17) . . ?
B11 B12 B8 107.8(2) . . ?
B10 B12 B8 108.2(2) . . ?
B9 B12 B7 108.0(2) . . ?
B11 B12 B7 59.89(16) . . ?
B10 B12 B7 107.8(2) . . ?
B8 B12 B7 59.34(17) . . ?
B9 B12 H12 121.2 . . ?
B11 B12 H12 121.5 . . ?
B10 B12 H12 121.6 . . ?
B8 B12 H12 121.8 . . ?
B7 B12 H12 122.2 . . ?
S1 N2 H2A 113(2) . . ?
S1 N2 H2B 115(2) . . ?
H2A N2 H2B 119(3) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.32
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.060
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4
_database_code_depnum_ccdc_archive 'CCDC 1583777'
_audit_update_record             
;
2017-11-03 deposited with the CCDC.
2018-03-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H35 B10 N O P Pd'
_chemical_formula_weight         719.10

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/c  '

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

_cell_length_a                   10.5093(6)
_cell_length_b                   22.2105(13)
_cell_length_c                   15.7027(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.021(2)
_cell_angle_gamma                90.00
_cell_volume                     3540.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6359
_cell_measurement_theta_min      0.981
_cell_measurement_theta_max      25.350

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1460
_exptl_absorpt_coefficient_mu    0.599
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20949
_diffrn_reflns_av_R_equivalents  0.0762
_diffrn_reflns_av_sigmaI/netI    0.0745
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.79
_diffrn_reflns_theta_max         25.35
_reflns_number_total             6359
_reflns_number_gt                4611
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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. 
;
# SQUEEZE RESULTS (Version = 120716)
# 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 0.500 0.500 0.000 128 46 ' '
2 0.500 0.000 0.500 128 46 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?


_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)+(0.0489P)²+3.1179P] 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         6359
_refine_ls_number_parameters     433
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0481
_refine_ls_wR_factor_ref         0.1090
_refine_ls_wR_factor_gt          0.0984
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.13294(3) 0.376283(16) 0.20445(2) 0.01628(11) Uani 1 1 d . . .
P2 P 0.07398(11) 0.42576(5) 0.31378(7) 0.0175(3) Uani 1 1 d . . .
O1 O -0.0084(3) 0.42198(15) 0.10719(18) 0.0253(7) Uani 1 1 d . . .
N1 N 0.1993(3) 0.33398(16) 0.1071(2) 0.0177(8) Uani 1 1 d . . .
C27 C 0.0627(4) 0.3810(2) 0.4090(3) 0.0206(10) Uani 1 1 d . . .
C21 C 0.0286(4) 0.3716(2) -0.0199(3) 0.0216(10) Uani 1 1 d . . .
C40 C -0.1828(5) 0.4563(2) 0.3290(3) 0.0305(12) Uani 1 1 d . . .
H40 H -0.1697 0.4273 0.3751 0.037 Uiso 1 1 calc R . .
C39 C -0.0864(4) 0.4644(2) 0.2840(3) 0.0220(10) Uani 1 1 d . . .
C14 C 0.6248(4) 0.2866(2) 0.2235(3) 0.0226(10) Uani 1 1 d . . .
B4 B 0.2751(5) 0.3275(2) 0.2909(3) 0.0178(11) Uani 1 1 d . . .
C1 C 0.3631(4) 0.2882(2) 0.2281(3) 0.0188(10) Uani 1 1 d . . .
C26 C -0.0382(4) 0.4125(2) 0.0231(3) 0.0234(11) Uani 1 1 d . . .
C32 C -0.0198(5) 0.3311(2) 0.3935(3) 0.0256(11) Uani 1 1 d . . .
H32 H -0.0676 0.3215 0.3351 0.031 Uiso 1 1 calc R . .
C2 C 0.5253(4) 0.2837(2) 0.2776(3) 0.0198(10) Uani 1 1 d . . .
C15 C 0.6552(5) 0.3403(2) 0.1879(3) 0.0318(12) Uani 1 1 d . . .
H15 H 0.6100 0.3760 0.1960 0.038 Uiso 1 1 calc R . .
C37 C 0.2228(5) 0.5819(2) 0.4388(3) 0.0316(12) Uani 1 1 d . . .
H37 H 0.1965 0.6114 0.4746 0.038 Uiso 1 1 calc R . .
C34 C 0.3009(4) 0.4967(2) 0.3342(3) 0.0219(10) Uani 1 1 d . . .
H34 H 0.3280 0.4675 0.2984 0.026 Uiso 1 1 calc R . .
C33 C 0.1826(4) 0.4892(2) 0.3570(3) 0.0186(10) Uani 1 1 d . . .
C13 C 0.3183(4) 0.2961(2) 0.1291(3) 0.0242(11) Uani 1 1 d . . .
H13A H 0.3890 0.3154 0.1075 0.029 Uiso 1 1 calc R . .
H13B H 0.2988 0.2564 0.1002 0.029 Uiso 1 1 calc R . .
B8 B 0.3906(5) 0.2145(2) 0.3724(4) 0.0250(12) Uani 1 1 d . . .
H8 H 0.3738 0.1697 0.4004 0.030 Uiso 1 1 calc R . .
C35 C 0.3802(5) 0.5468(2) 0.3636(3) 0.0272(11) Uani 1 1 d . . .
H35 H 0.4605 0.5519 0.3473 0.033 Uiso 1 1 calc R . .
C23 C -0.1236(5) 0.3947(2) -0.1615(3) 0.0351(13) Uani 1 1 d . . .
H23 H -0.1540 0.3880 -0.2232 0.042 Uiso 1 1 calc R . .
C31 C -0.0326(5) 0.2949(2) 0.4638(3) 0.0271(11) Uani 1 1 d . . .
H31 H -0.0906 0.2614 0.4537 0.033 Uiso 1 1 calc R . .
C20 C 0.1419(4) 0.3378(2) 0.0233(3) 0.0223(10) Uani 1 1 d . . .
H20 H 0.1811 0.3150 -0.0143 0.027 Uiso 1 1 calc R . .
C36 C 0.3416(5) 0.5889(2) 0.4163(3) 0.0308(12) Uani 1 1 d . . .
H36 H 0.3961 0.6226 0.4374 0.037 Uiso 1 1 calc R . .
C18 C 0.7897(5) 0.2381(2) 0.1652(4) 0.0374(13) Uani 1 1 d . . .
H18 H 0.8380 0.2030 0.1588 0.045 Uiso 1 1 calc R . .
B12 B 0.4709(5) 0.2741(3) 0.4408(3) 0.0237(12) Uani 1 1 d . . .
H12 H 0.5074 0.2690 0.5140 0.028 Uiso 1 1 calc R . .
C42 C -0.3195(5) 0.5323(3) 0.2420(4) 0.0409(14) Uani 1 1 d . . .
H42 H -0.3981 0.5556 0.2282 0.049 Uiso 1 1 calc R . .
C44 C -0.1084(5) 0.5069(2) 0.2167(3) 0.0283(11) Uani 1 1 d . . .
H44 H -0.0441 0.5129 0.1847 0.034 Uiso 1 1 calc R . .
C28 C 0.1351(5) 0.3942(2) 0.4951(3) 0.0268(11) Uani 1 1 d . . .
H28 H 0.1925 0.4280 0.5064 0.032 Uiso 1 1 calc R . .
C38 C 0.1422(5) 0.5328(2) 0.4096(3) 0.0256(11) Uani 1 1 d . . .
B10 B 0.4024(5) 0.3434(2) 0.3904(3) 0.0211(11) Uani 1 1 d . . .
H10 H 0.3954 0.3840 0.4312 0.025 Uiso 1 1 calc R . .
C19 C 0.6923(5) 0.2351(2) 0.2113(3) 0.0326(12) Uani 1 1 d . . .
H19 H 0.6725 0.1977 0.2343 0.039 Uiso 1 1 calc R . .
B11 B 0.5579(5) 0.3180(3) 0.3783(3) 0.0223(12) Uani 1 1 d . . .
H11 H 0.6522 0.3421 0.4094 0.027 Uiso 1 1 calc R . .
C24 C -0.1877(5) 0.4360(3) -0.1195(3) 0.0391(14) Uani 1 1 d . . .
H24 H -0.2609 0.4581 -0.1533 0.047 Uiso 1 1 calc R . .
C30 C 0.0398(5) 0.3087(2) 0.5475(3) 0.0307(12) Uani 1 1 d . . .
H30 H 0.0323 0.2839 0.5953 0.037 Uiso 1 1 calc R . .
C43 C -0.2244(5) 0.5408(2) 0.1959(3) 0.0395(14) Uani 1 1 d . . .
H43 H -0.2384 0.5698 0.1499 0.047 Uiso 1 1 calc R . .
C29 C 0.1224(5) 0.3573(2) 0.5640(3) 0.0287(12) Uani 1 1 d . . .
H29 H 0.1712 0.3659 0.6226 0.034 Uiso 1 1 calc R . .
C22 C -0.0179(5) 0.3644(2) -0.1130(3) 0.0308(12) Uani 1 1 d . . .
H22 H 0.0270 0.3374 -0.1421 0.037 Uiso 1 1 calc R . .
B7 B 0.5511(5) 0.2375(2) 0.3676(3) 0.0250(12) Uani 1 1 d . . .
H7 H 0.6404 0.2086 0.3919 0.030 Uiso 1 1 calc R . .
C41 C -0.2981(5) 0.4900(3) 0.3075(4) 0.0411(14) Uani 1 1 d . . .
H41 H -0.3631 0.4835 0.3388 0.049 Uiso 1 1 calc R . .
B3 B 0.4373(5) 0.3493(2) 0.2866(3) 0.0180(11) Uani 1 1 d . . .
H3 H 0.4524 0.3935 0.2562 0.022 Uiso 1 1 calc R . .
C25 C -0.1464(5) 0.4451(3) -0.0307(3) 0.0371(13) Uani 1 1 d . . .
H25 H -0.1908 0.4738 -0.0040 0.045 Uiso 1 1 calc R . .
B5 B 0.2725(5) 0.2466(2) 0.2809(3) 0.0224(12) Uani 1 1 d . . .
H5 H 0.1784 0.2231 0.2476 0.027 Uiso 1 1 calc R . .
B6 B 0.4287(5) 0.2204(2) 0.2698(4) 0.0253(12) Uani 1 1 d . . .
H6 H 0.4376 0.1802 0.2286 0.030 Uiso 1 1 calc R . .
B9 B 0.2988(5) 0.2797(2) 0.3871(3) 0.0226(12) Uani 1 1 d . . .
H9 H 0.2225 0.2780 0.4253 0.027 Uiso 1 1 calc R . .
C17 C 0.8157(5) 0.2913(2) 0.1293(3) 0.0350(13) Uani 1 1 d . . .
H17 H 0.8795 0.2927 0.0961 0.042 Uiso 1 1 calc R . .
C16 C 0.7496(5) 0.3431(2) 0.1410(3) 0.0374(13) Uani 1 1 d . . .
H16 H 0.7689 0.3803 0.1171 0.045 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
Pd1 B4 2.049(5) . ?
Pd1 N1 2.064(3) . ?
Pd1 O1 2.096(3) . ?
Pd1 P2 2.2560(11) . ?
P2 C27 1.824(4) . ?
P2 C33 1.829(5) . ?
P2 C39 1.841(5) . ?
O1 C26 1.294(5) . ?
N1 C20 1.301(5) . ?
N1 C13 1.472(6) . ?
C27 C32 1.389(6) . ?
C27 C28 1.401(6) . ?
C21 C20 1.422(6) . ?
C21 C26 1.421(6) . ?
C21 C22 1.426(6) . ?
C40 C39 1.389(6) . ?
C40 C41 1.390(7) . ?
C40 H40 0.9500 . ?
C39 C44 1.391(6) . ?
C14 C15 1.389(7) . ?
C14 C19 1.385(7) . ?
C14 C2 1.511(6) . ?
B4 C1 1.751(6) . ?
B4 B3 1.790(7) . ?
B4 B5 1.805(7) . ?
B4 B10 1.809(7) . ?
B4 B9 1.809(7) . ?
C1 C13 1.513(6) . ?
C1 C2 1.683(6) . ?
C1 B5 1.692(6) . ?
C1 B3 1.709(7) . ?
C1 B6 1.715(7) . ?
C26 C25 1.425(7) . ?
C32 C31 1.399(6) . ?
C32 H32 0.9500 . ?
C2 B11 1.708(6) . ?
C2 B7 1.710(7) . ?
C2 B6 1.720(7) . ?
C2 B3 1.751(6) . ?
C15 C16 1.381(6) . ?
C15 H15 0.9500 . ?
C37 C38 1.384(7) . ?
C37 C36 1.391(7) . ?
C37 H37 0.9500 . ?
C34 C33 1.390(6) . ?
C34 C35 1.396(6) . ?
C34 H34 0.9500 . ?
C33 C38 1.409(6) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
B8 B6 1.762(7) . ?
B8 B12 1.775(8) . ?
B8 B9 1.789(7) . ?
B8 B5 1.785(8) . ?
B8 B7 1.782(7) . ?
B8 H8 1.1200 . ?
C35 C36 1.376(6) . ?
C35 H35 0.9500 . ?
C23 C22 1.352(7) . ?
C23 C24 1.400(7) . ?
C23 H23 0.9500 . ?
C31 C30 1.372(7) . ?
C31 H31 0.9500 . ?
C20 H20 0.9500 . ?
C36 H36 0.9500 . ?
C18 C17 1.366(7) . ?
C18 C19 1.402(6) . ?
C18 H18 0.9500 . ?
B12 B11 1.792(7) . ?
B12 B9 1.791(7) . ?
B12 B10 1.792(7) . ?
B12 B7 1.786(7) . ?
B12 H12 1.1200 . ?
C42 C41 1.370(8) . ?
C42 C43 1.391(7) . ?
C42 H42 0.9500 . ?
C44 C43 1.398(7) . ?
C44 H44 0.9500 . ?
C28 C29 1.391(6) . ?
C28 H28 0.9500 . ?
B10 B3 1.767(7) . ?
B10 B9 1.777(7) . ?
B10 B11 1.785(7) . ?
B10 H10 1.1200 . ?
C19 H19 0.9500 . ?
B11 B7 1.795(8) . ?
B11 B3 1.795(7) . ?
B11 H11 1.1200 . ?
C24 C25 1.363(7) . ?
C24 H24 0.9500 . ?
C30 C29 1.368(7) . ?
C30 H30 0.9500 . ?
C43 H43 0.9500 . ?
C29 H29 0.9500 . ?
C22 H22 0.9500 . ?
B7 B6 1.771(8) . ?
B7 H7 1.1200 . ?
C41 H41 0.9500 . ?
B3 H3 1.1200 . ?
C25 H25 0.9500 . ?
B5 B9 1.777(7) . ?
B5 B6 1.792(7) . ?
B5 H5 1.1200 . ?
B6 H6 1.1200 . ?
B9 H9 1.1200 . ?
C17 C16 1.380(7) . ?
C17 H17 0.9500 . ?
C16 H16 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
B4 Pd1 N1 85.53(16) . . ?
B4 Pd1 O1 175.06(15) . . ?
N1 Pd1 O1 89.55(12) . . ?
B4 Pd1 P2 92.87(13) . . ?
N1 Pd1 P2 176.05(10) . . ?
O1 Pd1 P2 92.07(8) . . ?
C27 P2 C33 106.4(2) . . ?
C27 P2 C39 102.24(19) . . ?
C33 P2 C39 100.3(2) . . ?
C27 P2 Pd1 116.58(15) . . ?
C33 P2 Pd1 112.91(14) . . ?
C39 P2 Pd1 116.58(14) . . ?
C26 O1 Pd1 127.2(3) . . ?
C20 N1 C13 114.7(3) . . ?
C20 N1 Pd1 124.2(3) . . ?
C13 N1 Pd1 121.0(3) . . ?
C32 C27 C28 119.6(4) . . ?
C32 C27 P2 117.5(3) . . ?
C28 C27 P2 122.9(4) . . ?
C20 C21 C26 124.6(4) . . ?
C20 C21 C22 116.8(4) . . ?
C26 C21 C22 118.6(4) . . ?
C39 C40 C41 120.7(5) . . ?
C39 C40 H40 119.6 . . ?
C41 C40 H40 119.6 . . ?
C40 C39 C44 118.4(4) . . ?
C40 C39 P2 123.4(4) . . ?
C44 C39 P2 118.0(3) . . ?
C15 C14 C19 118.3(4) . . ?
C15 C14 C2 121.9(4) . . ?
C19 C14 C2 119.7(4) . . ?
C1 B4 B3 57.7(3) . . ?
C1 B4 B5 56.8(3) . . ?
B3 B4 B5 105.0(3) . . ?
C1 B4 B10 101.7(3) . . ?
B3 B4 B10 58.8(3) . . ?
B5 B4 B10 105.1(4) . . ?
C1 B4 B9 101.5(3) . . ?
B3 B4 B9 105.3(4) . . ?
B5 B4 B9 58.9(3) . . ?
B10 B4 B9 58.8(3) . . ?
C1 B4 Pd1 106.9(3) . . ?
B3 B4 Pd1 111.7(3) . . ?
B5 B4 Pd1 118.5(3) . . ?
B10 B4 Pd1 136.0(3) . . ?
B9 B4 Pd1 141.4(3) . . ?
C13 C1 C2 119.4(3) . . ?
C13 C1 B5 120.1(4) . . ?
C2 C1 B5 111.8(3) . . ?
C13 C1 B3 115.9(4) . . ?
C2 C1 B3 62.2(3) . . ?
B5 C1 B3 114.0(3) . . ?
C13 C1 B6 118.8(4) . . ?
C2 C1 B6 60.8(3) . . ?
B5 C1 B6 63.5(3) . . ?
B3 C1 B6 114.2(3) . . ?
C13 C1 B4 116.9(4) . . ?
C2 C1 B4 112.9(3) . . ?
B5 C1 B4 63.2(3) . . ?
B3 C1 B4 62.3(3) . . ?
B6 C1 B4 116.2(3) . . ?
O1 C26 C25 117.9(4) . . ?
O1 C26 C21 124.7(4) . . ?
C25 C26 C21 117.4(4) . . ?
C27 C32 C31 120.3(4) . . ?
C27 C32 H32 119.9 . . ?
C31 C32 H32 119.9 . . ?
C14 C2 C1 120.2(3) . . ?
C14 C2 B11 120.0(4) . . ?
C1 C2 B11 109.7(3) . . ?
C14 C2 B7 120.4(4) . . ?
C1 C2 B7 110.0(3) . . ?
B11 C2 B7 63.3(3) . . ?
C14 C2 B6 118.5(4) . . ?
C1 C2 B6 60.5(3) . . ?
B11 C2 B6 113.8(3) . . ?
B7 C2 B6 62.2(3) . . ?
C14 C2 B3 117.8(4) . . ?
C1 C2 B3 59.7(3) . . ?
B11 C2 B3 62.5(3) . . ?
B7 C2 B3 114.0(3) . . ?
B6 C2 B3 111.9(3) . . ?
C14 C15 C16 121.7(5) . . ?
C14 C15 H15 119.2 . . ?
C16 C15 H15 119.2 . . ?
C38 C37 C36 121.0(4) . . ?
C38 C37 H37 119.5 . . ?
C36 C37 H37 119.5 . . ?
C33 C34 C35 120.5(4) . . ?
C33 C34 H34 119.7 . . ?
C35 C34 H34 119.7 . . ?
C34 C33 C38 119.6(4) . . ?
C34 C33 P2 120.7(3) . . ?
C38 C33 P2 119.6(3) . . ?
N1 C13 C1 109.1(3) . . ?
N1 C13 H13A 109.9 . . ?
C1 C13 H13A 109.9 . . ?
N1 C13 H13B 109.9 . . ?
C1 C13 H13B 109.9 . . ?
H13A C13 H13B 108.3 . . ?
B6 B8 B12 108.3(4) . . ?
B6 B8 B9 108.4(4) . . ?
B12 B8 B9 60.3(3) . . ?
B6 B8 B5 60.7(3) . . ?
B12 B8 B5 108.1(4) . . ?
B9 B8 B5 59.6(3) . . ?
B6 B8 B7 60.0(3) . . ?
B12 B8 B7 60.3(3) . . ?
B9 B8 B7 108.7(4) . . ?
B5 B8 B7 108.7(4) . . ?
B6 B8 H8 121.4 . . ?
B12 B8 H8 121.6 . . ?
B9 B8 H8 121.5 . . ?
B5 B8 H8 121.5 . . ?
B7 B8 H8 121.3 . . ?
C36 C35 C34 119.7(4) . . ?
C36 C35 H35 120.1 . . ?
C34 C35 H35 120.1 . . ?
C22 C23 C24 119.1(5) . . ?
C22 C23 H23 120.4 . . ?
C24 C23 H23 120.4 . . ?
C30 C31 C32 119.0(5) . . ?
C30 C31 H31 120.5 . . ?
C32 C31 H31 120.5 . . ?
N1 C20 C21 128.9(4) . . ?
N1 C20 H20 115.5 . . ?
C21 C20 H20 115.5 . . ?
C35 C36 C37 120.1(5) . . ?
C35 C36 H36 120.0 . . ?
C37 C36 H36 120.0 . . ?
C17 C18 C19 120.4(5) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
B8 B12 B11 107.7(4) . . ?
B8 B12 B9 60.2(3) . . ?
B11 B12 B9 107.5(3) . . ?
B8 B12 B10 107.5(4) . . ?
B11 B12 B10 59.7(3) . . ?
B9 B12 B10 59.5(3) . . ?
B8 B12 B7 60.0(3) . . ?
B11 B12 B7 60.2(3) . . ?
B9 B12 B7 108.4(4) . . ?
B10 B12 B7 108.0(3) . . ?
B8 B12 H12 121.9 . . ?
B11 B12 H12 122.0 . . ?
B9 B12 H12 121.8 . . ?
B10 B12 H12 122.1 . . ?
B7 B12 H12 121.3 . . ?
C41 C42 C43 118.9(5) . . ?
C41 C42 H42 120.5 . . ?
C43 C42 H42 120.5 . . ?
C39 C44 C43 120.4(4) . . ?
C39 C44 H44 119.8 . . ?
C43 C44 H44 119.8 . . ?
C29 C28 C27 119.4(5) . . ?
C29 C28 H28 120.3 . . ?
C27 C28 H28 120.3 . . ?
C37 C38 C33 119.0(4) . . ?
B3 B10 B9 107.7(4) . . ?
B3 B10 B11 60.7(3) . . ?
B9 B10 B11 108.5(4) . . ?
B3 B10 B12 108.4(4) . . ?
B9 B10 B12 60.2(3) . . ?
B11 B10 B12 60.1(3) . . ?
B3 B10 B4 60.1(3) . . ?
B9 B10 B4 60.6(3) . . ?
B11 B10 B4 109.8(3) . . ?
B12 B10 B4 109.7(4) . . ?
B3 B10 H10 121.9 . . ?
B9 B10 H10 121.8 . . ?
B11 B10 H10 120.9 . . ?
B12 B10 H10 121.2 . . ?
B4 B10 H10 120.4 . . ?
C14 C19 C18 120.0(5) . . ?
C14 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C2 B11 B12 104.8(4) . . ?
C2 B11 B10 105.6(4) . . ?
B12 B11 B10 60.1(3) . . ?
C2 B11 B7 58.4(3) . . ?
B12 B11 B7 59.7(3) . . ?
B10 B11 B7 108.0(4) . . ?
C2 B11 B3 59.9(3) . . ?
B12 B11 B3 107.2(4) . . ?
B10 B11 B3 59.2(3) . . ?
B7 B11 B3 107.9(4) . . ?
C2 B11 H11 124.0 . . ?
B12 B11 H11 122.7 . . ?
B10 B11 H11 122.2 . . ?
B7 B11 H11 121.7 . . ?
B3 B11 H11 121.7 . . ?
C25 C24 C23 120.9(5) . . ?
C25 C24 H24 119.5 . . ?
C23 C24 H24 119.5 . . ?
C29 C30 C31 121.6(4) . . ?
C29 C30 H30 119.2 . . ?
C31 C30 H30 119.2 . . ?
C42 C43 C44 120.4(5) . . ?
C42 C43 H43 119.8 . . ?
C44 C43 H43 119.8 . . ?
C30 C29 C28 120.2(5) . . ?
C30 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
C23 C22 C21 122.3(5) . . ?
C23 C22 H22 118.8 . . ?
C21 C22 H22 118.8 . . ?
C2 B7 B6 59.2(3) . . ?
C2 B7 B8 104.9(4) . . ?
B6 B7 B8 59.5(3) . . ?
C2 B7 B12 105.0(4) . . ?
B6 B7 B12 107.3(4) . . ?
B8 B7 B12 59.6(3) . . ?
C2 B7 B11 58.3(3) . . ?
B6 B7 B11 107.3(4) . . ?
B8 B7 B11 107.3(4) . . ?
B12 B7 B11 60.0(3) . . ?
C2 B7 H7 124.3 . . ?
B6 B7 H7 121.8 . . ?
B8 B7 H7 122.7 . . ?
B12 B7 H7 122.5 . . ?
B11 B7 H7 122.0 . . ?
C42 C41 C40 121.1(5) . . ?
C42 C41 H41 119.5 . . ?
C40 C41 H41 119.5 . . ?
C1 B3 C2 58.2(3) . . ?
C1 B3 B10 105.2(3) . . ?
C2 B3 B10 104.6(3) . . ?
C1 B3 B4 60.0(3) . . ?
C2 B3 B4 107.8(3) . . ?
B10 B3 B4 61.1(3) . . ?
C1 B3 B11 104.6(4) . . ?
C2 B3 B11 57.6(3) . . ?
B10 B3 B11 60.1(3) . . ?
B4 B3 B11 110.2(4) . . ?
C1 B3 H3 124.2 . . ?
C2 B3 H3 124.0 . . ?
B10 B3 H3 123.0 . . ?
B4 B3 H3 119.6 . . ?
B11 B3 H3 122.2 . . ?
C24 C25 C26 121.7(5) . . ?
C24 C25 H25 119.2 . . ?
C26 C25 H25 119.2 . . ?
C1 B5 B9 105.2(4) . . ?
C1 B5 B8 104.5(4) . . ?
B9 B5 B8 60.3(3) . . ?
C1 B5 B4 60.0(3) . . ?
B9 B5 B4 60.7(3) . . ?
B8 B5 B4 109.6(4) . . ?
C1 B5 B6 58.9(3) . . ?
B9 B5 B6 107.6(4) . . ?
B8 B5 B6 59.0(3) . . ?
B4 B5 B6 109.8(4) . . ?
C1 B5 H5 124.5 . . ?
B9 B5 H5 122.3 . . ?
B8 B5 H5 122.4 . . ?
B4 B5 H5 119.7 . . ?
B6 B5 H5 121.6 . . ?
C1 B6 C2 58.7(3) . . ?
C1 B6 B8 104.5(4) . . ?
C2 B6 B8 105.3(4) . . ?
C1 B6 B7 105.8(4) . . ?
C2 B6 B7 58.6(3) . . ?
B8 B6 B7 60.6(3) . . ?
C1 B6 B5 57.6(3) . . ?
C2 B6 B5 105.4(4) . . ?
B8 B6 B5 60.3(3) . . ?
B7 B6 B5 108.8(4) . . ?
C1 B6 H6 124.4 . . ?
C2 B6 H6 123.8 . . ?
B8 B6 H6 122.8 . . ?
B7 B6 H6 121.5 . . ?
B5 B6 H6 122.1 . . ?
B5 B9 B8 60.1(3) . . ?
B5 B9 B10 107.6(3) . . ?
B8 B9 B10 107.5(4) . . ?
B5 B9 B12 107.8(4) . . ?
B8 B9 B12 59.4(3) . . ?
B10 B9 B12 60.3(3) . . ?
B5 B9 B4 60.4(3) . . ?
B8 B9 B4 109.2(3) . . ?
B10 B9 B4 60.6(3) . . ?
B12 B9 B4 109.7(3) . . ?
B5 B9 H9 122.0 . . ?
B8 B9 H9 121.8 . . ?
B10 B9 H9 122.0 . . ?
B12 B9 H9 121.4 . . ?
B4 B9 H9 120.3 . . ?
C16 C17 C18 120.3(4) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C17 C16 C15 119.3(5) . . ?
C17 C16 H16 120.4 . . ?
C15 C16 H16 120.4 . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        25.35
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.094


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

data_3
_database_code_depnum_ccdc_archive 'CCDC 1583776'
_audit_update_record             
;
2017-11-03 deposited with the CCDC.
2018-03-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H40 B20 N2 O Pd'
_chemical_formula_sum            'C25 H40 B20 N2 O Pd'
_chemical_formula_weight         707.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 '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                   14.4456(7)
_cell_length_b                   13.2757(6)
_cell_length_c                   19.9354(8)
_cell_angle_alpha                90
_cell_angle_beta                 90.292(2)
_cell_angle_gamma                90
_cell_volume                     3823.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    4987
_cell_measurement_theta_min      2.82
_cell_measurement_theta_max      25.31

_exptl_crystal_description       column
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_F_000             1432
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    0.510
_shelx_estimated_absorpt_T_min   0.883
_shelx_estimated_absorpt_T_max   0.923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6273
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'PHOTON 100 CMOS detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20022
_diffrn_reflns_av_unetI/netI     0.0681
_diffrn_reflns_av_R_equivalents  0.0677
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.820
_diffrn_reflns_theta_max         25.338
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             6956
_reflns_number_gt                4963
_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-2014/7 (Sheldrick, 2014)'
_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)+(0.0975P)²+4.0197P] 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         6956
_refine_ls_number_parameters     588
_refine_ls_number_restraints     1119
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0587
_refine_ls_wR_factor_ref         0.1740
_refine_ls_wR_factor_gt          0.1535
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.003
_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
B11 B 0.5631(5) -0.2458(5) 0.2657(3) 0.0345(15) Uani 1 1 d . . . . .
H11 H 0.5809 -0.1976 0.2215 0.041 Uiso 1 1 calc R U . . .
B12 B 0.6019(5) -0.3718(5) 0.2725(3) 0.0371(16) Uani 1 1 d . . . . .
H12 H 0.6445 -0.4082 0.2325 0.045 Uiso 1 1 calc R U . . .
B13 B 0.6211(6) -0.3970(5) 0.3595(3) 0.0439(17) Uani 1 1 d . . . . .
H13 H 0.6761 -0.4503 0.3773 0.053 Uiso 1 1 calc R U . . .
B14 B 0.5937(5) -0.2846(5) 0.4048(3) 0.0375(16) Uani 1 1 d . . . . .
H14 H 0.6312 -0.2624 0.4518 0.045 Uiso 1 1 calc R U . . .
B15 B 0.4550(5) -0.2347(5) 0.3066(3) 0.0412(16) Uani 1 1 d . . . . .
H15 H 0.4004 -0.1807 0.2892 0.049 Uiso 1 1 calc R U . . .
B16 B 0.4829(5) -0.3451(5) 0.2610(3) 0.0418(17) Uani 1 1 d . . . . .
H16 H 0.4463 -0.3644 0.2130 0.050 Uiso 1 1 calc R U . . .
B17 B 0.5177(6) -0.4391(6) 0.3189(4) 0.0477(18) Uani 1 1 d . . . . .
H17 H 0.5040 -0.5210 0.3095 0.057 Uiso 1 1 calc R U . . .
B18 B 0.5131(6) -0.3855(5) 0.4010(4) 0.051(2) Uani 1 1 d . . . . .
H18 H 0.4965 -0.4321 0.4462 0.061 Uiso 1 1 calc R U . . .
B19 B 0.4750(5) -0.2588(5) 0.3934(3) 0.0457(18) Uani 1 1 d . . . . .
H19 H 0.4338 -0.2205 0.4334 0.055 Uiso 1 1 calc R U . . .
B20 B 0.4269(6) -0.3545(6) 0.3403(4) 0.055(2) Uani 1 1 d . . . . .
H20 H 0.3535 -0.3804 0.3452 0.066 Uiso 1 1 calc R U . . .
C1 C 0.3940(4) 0.1639(4) 0.4271(2) 0.0337(13) Uani 1 1 d . . . . .
C2 C 0.4202(4) 0.2675(4) 0.4204(2) 0.0335(13) Uani 1 1 d D . . . .
C3 C 0.3502(5) 0.3428(5) 0.4191(3) 0.0480(16) Uani 1 1 d . . . . .
H3 H 0.3678 0.4114 0.4145 0.058 Uiso 1 1 calc R U . . .
C4 C 0.2588(5) 0.3194(7) 0.4241(4) 0.063(2) Uani 1 1 d . . . . .
H4 H 0.2132 0.3710 0.4239 0.076 Uiso 1 1 calc R U . . .
C5 C 0.2328(5) 0.2180(7) 0.4296(3) 0.060(2) Uani 1 1 d . . . . .
H5 H 0.1692 0.2009 0.4330 0.072 Uiso 1 1 calc R U . . .
C6 C 0.2979(4) 0.1437(6) 0.4301(3) 0.0460(16) Uani 1 1 d . . . . .
H6 H 0.2779 0.0756 0.4325 0.055 Uiso 1 1 calc R U . . .
C17 C 0.6435(4) -0.2815(4) 0.3258(2) 0.0307(12) Uani 1 1 d D . . . .
C18 C 0.5556(4) -0.2002(4) 0.3462(2) 0.0291(12) Uani 1 1 d . . . . .
C25 C 0.5784(4) -0.0887(4) 0.3536(2) 0.0307(12) Uani 1 1 d . . . . .
H25A H 0.6321 -0.0735 0.3247 0.037 Uiso 1 1 calc R U . . .
H25B H 0.5252 -0.0494 0.3362 0.037 Uiso 1 1 calc R U . . .
N2 N 0.5994(4) -0.0531(4) 0.4209(2) 0.0333(10) Uani 1 1 d D . . . .
H2A H 0.651(3) -0.078(4) 0.431(3) 0.040 Uiso 1 1 d D U . . .
H2B H 0.559(4) -0.073(4) 0.448(3) 0.040 Uiso 1 1 d D U . . .
O1 O 0.4507(3) 0.0893(3) 0.43183(19) 0.0366(9) Uani 1 1 d . . . . .
Pd1 Pd 0.59548(3) 0.10345(3) 0.42367(2) 0.02805(16) Uani 1 1 d . . . . .
C7 C 0.5110(6) 0.3043(10) 0.4146(10) 0.034(3) Uani 0.665(5) 1 d D U P A 1
H7 H 0.5164 0.3753 0.4101 0.041 Uiso 0.665(5) 1 calc R U P A 1
N1 N 0.5883(5) 0.2548(7) 0.4145(5) 0.032(2) Uani 0.665(5) 1 d D U P A 1
C8 C 0.6717(6) 0.3163(6) 0.4046(6) 0.044(2) Uani 0.665(5) 1 d D U P A 1
H8A H 0.6767 0.3677 0.4404 0.053 Uiso 0.665(5) 1 calc R U P A 1
H8B H 0.6682 0.3515 0.3608 0.053 Uiso 0.665(5) 1 calc R U P A 1
C9 C 0.7562(5) 0.2474(6) 0.4064(5) 0.039(2) Uani 0.665(5) 1 d D U P A 1
C10 C 0.8450(6) 0.2679(7) 0.3533(5) 0.042(2) Uani 0.665(5) 1 d D U P A 1
B1 B 0.7684(10) 0.1705(9) 0.3383(6) 0.039(2) Uani 0.665(5) 1 d D U P A 1
H1 H 0.7200 0.1694 0.2943 0.046 Uiso 0.665(5) 1 calc R U P A 1
B2 B 0.7331(10) 0.1210(7) 0.4153(15) 0.037(2) Uani 0.665(5) 1 d D U P A 1
B3 B 0.7905(9) 0.1967(11) 0.4800(6) 0.053(2) Uani 0.665(5) 1 d D U P A 1
H3A H 0.7574 0.2115 0.5297 0.063 Uiso 0.665(5) 1 calc R U P A 1
B4 B 0.8588(8) 0.2885(10) 0.4367(6) 0.054(2) Uani 0.665(5) 1 d D U P A 1
H4A H 0.8704 0.3656 0.4580 0.065 Uiso 0.665(5) 1 calc R U P A 1
B5 B 0.8896(10) 0.1555(10) 0.3296(6) 0.048(3) Uani 0.665(5) 1 d D U P A 1
H5A H 0.9225 0.1425 0.2796 0.058 Uiso 0.665(5) 1 calc R U P A 1
B6 B 0.8223(9) 0.0614(11) 0.3697(6) 0.047(3) Uani 0.665(5) 1 d D U P A 1
H6A H 0.8113 -0.0145 0.3466 0.056 Uiso 0.665(5) 1 calc R U P A 1
B7 B 0.8362(9) 0.0772(11) 0.4590(6) 0.055(3) Uani 0.665(5) 1 d D U P A 1
H7A H 0.8338 0.0129 0.4953 0.066 Uiso 0.665(5) 1 calc R U P A 1
B8 B 0.9123(10) 0.1814(11) 0.4702(6) 0.066(3) Uani 0.665(5) 1 d D U P A 1
H8 H 0.9607 0.1859 0.5141 0.079 Uiso 0.665(5) 1 calc R U P A 1
B9 B 0.9438(8) 0.2279(9) 0.3903(6) 0.054(3) Uani 0.665(5) 1 d D U P A 1
H9 H 1.0129 0.2633 0.3807 0.065 Uiso 0.665(5) 1 calc R U P A 1
B10 B 0.9314(8) 0.0969(9) 0.4040(6) 0.059(3) Uani 0.665(5) 1 d D U P A 1
H10 H 0.9919 0.0441 0.4041 0.071 Uiso 0.665(5) 1 calc R U P A 1
C11 C 0.8427(6) 0.3545(7) 0.3045(4) 0.049(2) Uani 0.665(5) 1 d D U P A 1
C12 C 0.8772(8) 0.4480(7) 0.3208(5) 0.068(3) Uani 0.665(5) 1 d D U P A 1
H12A H 0.8961 0.4602 0.3657 0.081 Uiso 0.665(5) 1 calc R U P A 1
C13 C 0.8854(8) 0.5262(6) 0.2734(5) 0.056(3) Uani 0.665(5) 1 d D U P A 1
H13A H 0.9179 0.5867 0.2833 0.068 Uiso 0.665(5) 1 calc R U P A 1
C14 C 0.8457(7) 0.5109(8) 0.2146(6) 0.062(3) Uani 0.665(5) 1 d D U P A 1
H14A H 0.8415 0.5670 0.1851 0.075 Uiso 0.665(5) 1 calc R U P A 1
C15 C 0.8102(7) 0.4225(8) 0.1922(5) 0.058(3) Uani 0.665(5) 1 d D U P A 1
H15A H 0.7870 0.4149 0.1479 0.070 Uiso 0.665(5) 1 calc R U P A 1
C16 C 0.8098(8) 0.3420(8) 0.2388(5) 0.067(3) Uani 0.665(5) 1 d D U P A 1
H16A H 0.7868 0.2782 0.2252 0.081 Uiso 0.665(5) 1 calc R U P A 1
C7' C 0.5151(8) 0.304(2) 0.426(2) 0.030(6) Uiso 0.335(5) 1 d D U P A 2
H7' H 0.5222 0.3748 0.4233 0.036 Uiso 0.335(5) 1 calc R U P A 2
N1' N 0.5906(8) 0.2536(17) 0.4327(10) 0.029(4) Uiso 0.335(5) 1 d D U P A 2
C8' C 0.6777(8) 0.3085(12) 0.4457(10) 0.035(4) Uiso 0.335(5) 1 d D U P A 2
H8'1 H 0.6807 0.3299 0.4932 0.042 Uiso 0.335(5) 1 calc R U P A 2
H8'2 H 0.6806 0.3694 0.4171 0.042 Uiso 0.335(5) 1 calc R U P A 2
C9' C 0.7590(10) 0.2387(12) 0.4299(10) 0.041(4) Uiso 0.335(5) 1 d D U P A 2
C10' C 0.8608(10) 0.2492(12) 0.4699(8) 0.041(3) Uiso 0.335(5) 1 d D U P A 2
B1' B 0.7877(16) 0.1508(16) 0.4886(10) 0.042(4) Uiso 0.335(5) 1 d D U P A 2
H1' H 0.7527 0.1431 0.5383 0.051 Uiso 0.335(5) 1 calc R U P A 2
B2' B 0.7298(18) 0.1150(13) 0.415(3) 0.039(4) Uiso 0.335(5) 1 d D U P A 2
B3' B 0.773(2) 0.197(2) 0.3489(11) 0.043(4) Uiso 0.335(5) 1 d D U P A 2
H3' H 0.7281 0.2179 0.3054 0.051 Uiso 0.335(5) 1 calc R U P A 2
B4' B 0.8541(16) 0.2820(17) 0.3871(10) 0.044(4) Uiso 0.335(5) 1 d D U P A 2
H4' H 0.8619 0.3614 0.3689 0.052 Uiso 0.335(5) 1 calc R U P A 2
B5' B 0.9068(18) 0.1321(18) 0.4795(9) 0.052(4) Uiso 0.335(5) 1 d D U P A 2
H5' H 0.9510 0.1105 0.5235 0.062 Uiso 0.335(5) 1 calc R U P A 2
B6' B 0.8289(16) 0.0451(18) 0.4422(10) 0.042(4) Uiso 0.335(5) 1 d D U P A 2
H6' H 0.8218 -0.0344 0.4603 0.051 Uiso 0.335(5) 1 calc R U P A 2
B7' B 0.8201(19) 0.076(2) 0.3540(11) 0.046(4) Uiso 0.335(5) 1 d D U P A 2
H7'1 H 0.8068 0.0188 0.3139 0.055 Uiso 0.335(5) 1 calc R U P A 2
B8' B 0.895(2) 0.1821(19) 0.3418(11) 0.050(4) Uiso 0.335(5) 1 d D U P A 2
H8'A H 0.9323 0.1953 0.2934 0.060 Uiso 0.335(5) 1 calc R U P A 2
B9' B 0.9477(19) 0.2125(15) 0.4186(11) 0.056(4) Uiso 0.335(5) 1 d D U P A 2
H9' H 1.0194 0.2441 0.4221 0.067 Uiso 0.335(5) 1 calc R U P A 2
B10' B 0.9278(15) 0.0843(15) 0.3970(11) 0.058(4) Uiso 0.335(5) 1 d D U P A 2
H10' H 0.9850 0.0305 0.3851 0.070 Uiso 0.335(5) 1 calc R U P A 2
C11' C 0.8725(13) 0.3323(12) 0.5204(7) 0.053(5) Uiso 0.335(5) 1 d D U P A 2
C12' C 0.9178(18) 0.4214(13) 0.5021(9) 0.084(7) Uiso 0.335(5) 1 d D U P A 2
H12' H 0.9282 0.4352 0.4560 0.100 Uiso 0.335(5) 1 calc R U P A 2
C13' C 0.9483(15) 0.4912(14) 0.5511(8) 0.067(6) Uiso 0.335(5) 1 d D U P A 2
H13' H 0.9893 0.5451 0.5414 0.080 Uiso 0.335(5) 1 calc R U P A 2
C14' C 0.9142(15) 0.4744(15) 0.6124(9) 0.069(6) Uiso 0.335(5) 1 d D U P A 2
H14' H 0.9294 0.5229 0.6457 0.083 Uiso 0.335(5) 1 calc R U P A 2
C15' C 0.8637(15) 0.4011(14) 0.6315(9) 0.064(6) Uiso 0.335(5) 1 d D U P A 2
H15' H 0.8350 0.4022 0.6742 0.077 Uiso 0.335(5) 1 calc R U P A 2
C16' C 0.8512(18) 0.3182(15) 0.5880(8) 0.084(7) Uiso 0.335(5) 1 d D U P A 2
H16' H 0.8292 0.2553 0.6040 0.101 Uiso 0.335(5) 1 calc R U P A 2
C19 C 0.7394(13) -0.242(4) 0.3151(11) 0.038(3) Uani 0.57(2) 1 d D U P B 3
C20 C 0.7691(11) -0.215(2) 0.2515(10) 0.045(3) Uani 0.57(2) 1 d D U P B 3
H20A H 0.7275 -0.2166 0.2145 0.054 Uiso 0.57(2) 1 calc R U P B 3
C21 C 0.8613(10) -0.1839(14) 0.2425(9) 0.051(3) Uani 0.57(2) 1 d D U P B 3
H21 H 0.8821 -0.1678 0.1987 0.062 Uiso 0.57(2) 1 calc R U P B 3
C22 C 0.9207(10) -0.1765(14) 0.2943(10) 0.058(4) Uani 0.57(2) 1 d D U P B 3
H22 H 0.9823 -0.1543 0.2868 0.069 Uiso 0.57(2) 1 calc R U P B 3
C23 C 0.8935(10) -0.2006(14) 0.3571(9) 0.058(4) Uani 0.57(2) 1 d D U P B 3
H23 H 0.9355 -0.1949 0.3937 0.069 Uiso 0.57(2) 1 calc R U P B 3
C24 C 0.8023(12) -0.2342(18) 0.3676(10) 0.052(4) Uani 0.57(2) 1 d D U P B 3
H24 H 0.7834 -0.2517 0.4117 0.062 Uiso 0.57(2) 1 calc R U P B 3
C19' C 0.7414(18) -0.247(5) 0.3270(15) 0.040(4) Uani 0.43(2) 1 d D U P B 4
C20' C 0.7868(15) -0.220(3) 0.2688(12) 0.046(4) Uani 0.43(2) 1 d D U P B 4
H20' H 0.7532 -0.2201 0.2277 0.056 Uiso 0.43(2) 1 calc R U P B 4
C21' C 0.8805(14) -0.192(2) 0.2680(12) 0.056(4) Uani 0.43(2) 1 d D U P B 4
H21' H 0.9095 -0.1700 0.2278 0.067 Uiso 0.43(2) 1 calc R U P B 4
C22' C 0.9270(13) -0.1966(19) 0.3255(13) 0.060(4) Uani 0.43(2) 1 d D U P B 4
H22' H 0.9905 -0.1780 0.3261 0.072 Uiso 0.43(2) 1 calc R U P B 4
C23' C 0.8877(14) -0.227(2) 0.3830(12) 0.060(4) Uani 0.43(2) 1 d D U P B 4
H23' H 0.9244 -0.2307 0.4225 0.072 Uiso 0.43(2) 1 calc R U P B 4
C24' C 0.7935(16) -0.253(2) 0.3862(12) 0.052(4) Uani 0.43(2) 1 d D U P B 4
H24' H 0.7662 -0.2738 0.4271 0.063 Uiso 0.43(2) 1 calc R U P B 4


_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
B11 C18 1.719(7) . ?
B11 C17 1.731(8) . ?
B11 B16 1.757(10) . ?
B11 B12 1.769(9) . ?
B11 B15 1.772(10) . ?
B11 H11 1.1200 . ?
B12 C17 1.708(8) . ?
B12 B16 1.770(10) . ?
B12 B17 1.773(10) . ?
B12 B13 1.786(9) . ?
B12 H12 1.1200 . ?
B13 C17 1.706(8) . ?
B13 B18 1.776(12) . ?
B13 B17 1.785(10) . ?
B13 B14 1.789(9) . ?
B13 H13 1.1200 . ?
B14 C18 1.707(8) . ?
B14 C17 1.735(8) . ?
B14 B19 1.761(11) . ?
B14 B18 1.775(10) . ?
B14 H14 1.1200 . ?
B15 C18 1.712(8) . ?
B15 B16 1.772(10) . ?
B15 B20 1.773(11) . ?
B15 B19 1.781(10) . ?
B15 H15 1.1200 . ?
B16 B17 1.772(10) . ?
B16 B20 1.783(11) . ?
B16 H16 1.1200 . ?
B17 B20 1.781(12) . ?
B17 B18 1.787(10) . ?
B17 H17 1.1200 . ?
B18 B19 1.776(10) . ?
B18 B20 1.782(12) . ?
B18 H18 1.1200 . ?
B19 C18 1.690(8) . ?
B19 B20 1.792(10) . ?
B19 H19 1.1200 . ?
B20 H20 1.1200 . ?
C1 O1 1.287(7) . ?
C1 C6 1.416(8) . ?
C1 C2 1.433(8) . ?
C2 C7 1.405(10) . ?
C2 C3 1.422(8) . ?
C2 C7' 1.457(15) . ?
C3 C4 1.361(10) . ?
C3 H3 0.9500 . ?
C4 C5 1.401(11) . ?
C4 H4 0.9500 . ?
C5 C6 1.362(10) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C17 C19' 1.487(14) . ?
C17 C19 1.495(11) . ?
C17 C18 1.716(7) . ?
C18 C25 1.524(7) . ?
C25 N2 1.452(7) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
N2 Pd1 2.080(5) . ?
N2 H2A 0.84(4) . ?
N2 H2B 0.84(4) . ?
O1 Pd1 2.108(4) . ?
Pd1 B2' 1.96(3) . ?
Pd1 N1' 2.00(2) . ?
Pd1 B2 2.009(14) . ?
Pd1 N1 2.021(10) . ?
C7 N1 1.296(10) . ?
C7 H7 0.9500 . ?
N1 C8 1.470(9) . ?
C8 C9 1.525(10) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 B3 1.687(15) . ?
C9 B4 1.689(13) . ?
C9 C10 1.690(11) . ?
C9 B1 1.709(14) . ?
C9 B2 1.720(11) . ?
C10 C11 1.507(12) . ?
C10 B9 1.689(14) . ?
C10 B5 1.693(17) . ?
C10 B4 1.697(14) . ?
C10 B1 1.727(14) . ?
B1 B2 1.75(3) . ?
B1 B6 1.758(19) . ?
B1 B5 1.77(2) . ?
B1 H1 1.1200 . ?
B2 B6 1.77(2) . ?
B2 B7 1.82(2) . ?
B2 B3 1.83(2) . ?
B3 B7 1.77(2) . ?
B3 B8 1.783(19) . ?
B3 B4 1.792(16) . ?
B3 H3A 1.1200 . ?
B4 B9 1.740(18) . ?
B4 B8 1.75(2) . ?
B4 H4A 1.1200 . ?
B5 B9 1.730(17) . ?
B5 B6 1.776(16) . ?
B5 B10 1.777(12) . ?
B5 H5A 1.1200 . ?
B6 B10 1.778(12) . ?
B6 B7 1.801(16) . ?
B6 H6A 1.1200 . ?
B7 B8 1.781(19) . ?
B7 B10 1.782(12) . ?
B7 H7A 1.1200 . ?
B8 B10 1.755(13) . ?
B8 B9 1.770(17) . ?
B8 H8 1.1200 . ?
B9 B10 1.770(12) . ?
B9 H9 1.1200 . ?
B10 H10 1.1200 . ?
C11 C12 1.375(11) . ?
C11 C16 1.400(11) . ?
C12 C13 1.410(10) . ?
C12 H12A 0.9500 . ?
C13 C14 1.318(11) . ?
C13 H13A 0.9500 . ?
C14 C15 1.355(11) . ?
C14 H14A 0.9500 . ?
C15 C16 1.415(11) . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9500 . ?
C7' N1' 1.286(16) . ?
C7' H7' 0.9500 . ?
N1' C8' 1.476(15) . ?
C8' C9' 1.529(15) . ?
C8' H8'1 0.9900 . ?
C8' H8'2 0.9900 . ?
C9' C10' 1.676(16) . ?
C9' B1' 1.703(19) . ?
C9' B4' 1.72(3) . ?
C9' B2' 1.720(17) . ?
C9' B3' 1.72(3) . ?
C10' C11' 1.502(16) . ?
C10' B9' 1.70(3) . ?
C10' B5' 1.70(3) . ?
C10' B4' 1.71(2) . ?
C10' B1' 1.721(19) . ?
B1' B5' 1.75(3) . ?
B1' B2' 1.75(4) . ?
B1' B6' 1.78(3) . ?
B1' H1' 1.1200 . ?
B2' B6' 1.79(4) . ?
B2' B3' 1.82(3) . ?
B2' B7' 1.86(5) . ?
B3' B7' 1.74(4) . ?
B3' B8' 1.78(5) . ?
B3' B4' 1.79(2) . ?
B3' H3' 1.1200 . ?
B4' B8' 1.71(4) . ?
B4' B9' 1.75(3) . ?
B4' H4' 1.1200 . ?
B5' B9' 1.72(2) . ?
B5' B6' 1.77(2) . ?
B5' B10' 1.790(15) . ?
B5' H5' 1.1200 . ?
B6' B10' 1.771(15) . ?
B6' B7' 1.81(2) . ?
B6' H6' 1.1200 . ?
B7' B10' 1.775(15) . ?
B7' B8' 1.79(2) . ?
B7' H7'1 1.1200 . ?
B8' B9' 1.75(2) . ?
B8' B10' 1.763(15) . ?
B8' H8'A 1.1200 . ?
B9' B10' 1.778(15) . ?
B9' H9' 1.1200 . ?
B10' H10' 1.1200 . ?
C11' C16' 1.395(13) . ?
C11' C12' 1.402(14) . ?
C12' C13' 1.415(14) . ?
C12' H12' 0.9500 . ?
C13' C14' 1.338(14) . ?
C13' H13' 0.9500 . ?
C14' C15' 1.275(14) . ?
C14' H14' 0.9500 . ?
C15' C16' 1.412(14) . ?
C15' H15' 0.9500 . ?
C16' H16' 0.9500 . ?
C19 C24 1.389(11) . ?
C19 C20 1.390(12) . ?
C20 C21 1.405(12) . ?
C20 H20A 0.9500 . ?
C21 C22 1.343(12) . ?
C21 H21 0.9500 . ?
C22 C23 1.352(13) . ?
C22 H22 0.9500 . ?
C23 C24 1.407(12) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C19' C20' 1.383(13) . ?
C19' C24' 1.398(13) . ?
C20' C21' 1.404(14) . ?
C20' H20' 0.9500 . ?
C21' C22' 1.328(14) . ?
C21' H21' 0.9500 . ?
C22' C23' 1.342(14) . ?
C22' H22' 0.9500 . ?
C23' C24' 1.405(14) . ?
C23' H23' 0.9500 . ?
C24' H24' 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C18 B11 C17 59.7(3) . . ?
C18 B11 B16 105.6(4) . . ?
C17 B11 B16 105.8(4) . . ?
C18 B11 B12 106.4(4) . . ?
C17 B11 B12 58.4(3) . . ?
B16 B11 B12 60.3(4) . . ?
C18 B11 B15 58.7(3) . . ?
C17 B11 B15 107.1(4) . . ?
B16 B11 B15 60.3(4) . . ?
B12 B11 B15 108.8(5) . . ?
C18 B11 H11 123.3 . . ?
C17 B11 H11 123.0 . . ?
B16 B11 H11 122.7 . . ?
B12 B11 H11 121.8 . . ?
B15 B11 H11 121.4 . . ?
C17 B12 B11 59.7(3) . . ?
C17 B12 B16 106.2(4) . . ?
B11 B12 B16 59.5(4) . . ?
C17 B12 B17 105.7(4) . . ?
B11 B12 B17 107.4(5) . . ?
B16 B12 B17 60.0(4) . . ?
C17 B12 B13 58.4(3) . . ?
B11 B12 B13 107.5(4) . . ?
B16 B12 B13 108.0(5) . . ?
B17 B12 B13 60.2(4) . . ?
C17 B12 H12 123.6 . . ?
B11 B12 H12 121.9 . . ?
B16 B12 H12 122.0 . . ?
B17 B12 H12 122.3 . . ?
B13 B12 H12 121.8 . . ?
C17 B13 B18 106.0(5) . . ?
C17 B13 B17 105.2(5) . . ?
B18 B13 B17 60.3(4) . . ?
C17 B13 B12 58.5(3) . . ?
B18 B13 B12 107.7(5) . . ?
B17 B13 B12 59.5(4) . . ?
C17 B13 B14 59.5(3) . . ?
B18 B13 B14 59.7(4) . . ?
B17 B13 B14 107.7(5) . . ?
B12 B13 B14 107.4(4) . . ?
C17 B13 H13 123.8 . . ?
B18 B13 H13 122.0 . . ?
B17 B13 H13 122.4 . . ?
B12 B13 H13 122.1 . . ?
B14 B13 H13 121.7 . . ?
C18 B14 C17 59.8(3) . . ?
C18 B14 B19 58.3(4) . . ?
C17 B14 B19 106.6(4) . . ?
C18 B14 B18 104.9(5) . . ?
C17 B14 B18 104.8(4) . . ?
B19 B14 B18 60.3(4) . . ?
C18 B14 B13 105.9(4) . . ?
C17 B14 B13 57.9(3) . . ?
B19 B14 B13 108.4(5) . . ?
B18 B14 B13 59.7(4) . . ?
C18 B14 H14 123.5 . . ?
C17 B14 H14 123.4 . . ?
B19 B14 H14 121.6 . . ?
B18 B14 H14 123.3 . . ?
B13 B14 H14 122.3 . . ?
C18 B15 B16 105.2(5) . . ?
C18 B15 B11 59.1(3) . . ?
B16 B15 B11 59.4(4) . . ?
C18 B15 B20 105.2(5) . . ?
B16 B15 B20 60.4(4) . . ?
B11 B15 B20 107.7(5) . . ?
C18 B15 B19 57.8(4) . . ?
B16 B15 B19 108.3(5) . . ?
B11 B15 B19 107.1(5) . . ?
B20 B15 B19 60.6(4) . . ?
C18 B15 H15 124.5 . . ?
B16 B15 H15 122.1 . . ?
B11 B15 H15 122.1 . . ?
B20 B15 H15 121.9 . . ?
B19 B15 H15 121.8 . . ?
B11 B16 B12 60.2(4) . . ?
B11 B16 B17 108.0(5) . . ?
B12 B16 B17 60.1(4) . . ?
B11 B16 B15 60.3(4) . . ?
B12 B16 B15 108.8(5) . . ?
B17 B16 B15 108.2(5) . . ?
B11 B16 B20 107.9(5) . . ?
B12 B16 B20 108.4(5) . . ?
B17 B16 B20 60.1(4) . . ?
B15 B16 B20 59.8(4) . . ?
B11 B16 H16 121.7 . . ?
B12 B16 H16 121.3 . . ?
B17 B16 H16 121.7 . . ?
B15 B16 H16 121.4 . . ?
B20 B16 H16 121.8 . . ?
B16 B17 B12 59.9(4) . . ?
B16 B17 B20 60.3(4) . . ?
B12 B17 B20 108.3(5) . . ?
B16 B17 B13 108.0(5) . . ?
B12 B17 B13 60.2(4) . . ?
B20 B17 B13 108.0(5) . . ?
B16 B17 B18 107.7(5) . . ?
B12 B17 B18 107.8(5) . . ?
B20 B17 B18 59.9(5) . . ?
B13 B17 B18 59.6(4) . . ?
B16 B17 H17 121.7 . . ?
B12 B17 H17 121.6 . . ?
B20 B17 H17 121.5 . . ?
B13 B17 H17 121.7 . . ?
B18 B17 H17 122.1 . . ?
B14 B18 B13 60.5(4) . . ?
B14 B18 B19 59.5(4) . . ?
B13 B18 B19 108.3(5) . . ?
B14 B18 B20 108.1(5) . . ?
B13 B18 B20 108.4(5) . . ?
B19 B18 B20 60.5(4) . . ?
B14 B18 B17 108.2(5) . . ?
B13 B18 B17 60.1(4) . . ?
B19 B18 B17 108.1(5) . . ?
B20 B18 B17 59.9(4) . . ?
B14 B18 H18 121.8 . . ?
B13 B18 H18 121.3 . . ?
B19 B18 H18 121.7 . . ?
B20 B18 H18 121.5 . . ?
B17 B18 H18 121.7 . . ?
C18 B19 B14 59.2(4) . . ?
C18 B19 B18 105.6(5) . . ?
B14 B19 B18 60.2(4) . . ?
C18 B19 B15 59.1(4) . . ?
B14 B19 B15 108.3(5) . . ?
B18 B19 B15 107.6(5) . . ?
C18 B19 B20 105.2(5) . . ?
B14 B19 B20 108.2(5) . . ?
B18 B19 B20 59.9(5) . . ?
B15 B19 B20 59.5(4) . . ?
C18 B19 H19 124.0 . . ?
B14 B19 H19 121.1 . . ?
B18 B19 H19 122.3 . . ?
B15 B19 H19 121.8 . . ?
B20 B19 H19 122.4 . . ?
B15 B20 B17 107.8(5) . . ?
B15 B20 B18 107.7(5) . . ?
B17 B20 B18 60.2(4) . . ?
B15 B20 B16 59.8(4) . . ?
B17 B20 B16 59.6(4) . . ?
B18 B20 B16 107.5(6) . . ?
B15 B20 B19 59.9(4) . . ?
B17 B20 B19 107.7(6) . . ?
B18 B20 B19 59.6(4) . . ?
B16 B20 B19 107.3(5) . . ?
B15 B20 H20 121.8 . . ?
B17 B20 H20 121.7 . . ?
B18 B20 H20 121.9 . . ?
B16 B20 H20 122.2 . . ?
B19 B20 H20 122.1 . . ?
O1 C1 C6 118.4(5) . . ?
O1 C1 C2 125.2(5) . . ?
C6 C1 C2 116.4(6) . . ?
C7 C2 C3 114.7(7) . . ?
C7 C2 C1 126.0(7) . . ?
C3 C2 C1 119.3(6) . . ?
C3 C2 C7' 115.9(12) . . ?
C1 C2 C7' 124.0(12) . . ?
C4 C3 C2 121.9(7) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C3 C4 C5 119.0(7) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C6 C5 C4 120.7(7) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C5 C6 C1 122.7(7) . . ?
C5 C6 H6 118.7 . . ?
C1 C6 H6 118.7 . . ?
C19' C17 B13 117(2) . . ?
C19 C17 B13 123.1(19) . . ?
C19' C17 B12 124(2) . . ?
C19 C17 B12 118.5(16) . . ?
B13 C17 B12 63.1(4) . . ?
C19' C17 C18 120(3) . . ?
C19 C17 C18 120(2) . . ?
B13 C17 C18 109.2(4) . . ?
B12 C17 C18 109.3(4) . . ?
C19' C17 B11 124.1(16) . . ?
C19 C17 B11 115.1(12) . . ?
B13 C17 B11 113.0(4) . . ?
B12 C17 B11 61.9(3) . . ?
C18 C17 B11 59.8(3) . . ?
C19' C17 B14 113.1(13) . . ?
C19 C17 B14 121.8(11) . . ?
B13 C17 B14 62.6(4) . . ?
B12 C17 B14 113.6(4) . . ?
C18 C17 B14 59.3(3) . . ?
B11 C17 B14 110.8(4) . . ?
C25 C18 B19 122.8(4) . . ?
C25 C18 B14 120.1(4) . . ?
B19 C18 B14 62.4(4) . . ?
C25 C18 B15 119.2(5) . . ?
B19 C18 B15 63.1(4) . . ?
B14 C18 B15 114.1(5) . . ?
C25 C18 C17 118.3(4) . . ?
B19 C18 C17 110.8(4) . . ?
B14 C18 C17 60.9(3) . . ?
B15 C18 C17 110.5(4) . . ?
C25 C18 B11 114.8(4) . . ?
B19 C18 B11 113.9(4) . . ?
B14 C18 B11 112.7(4) . . ?
B15 C18 B11 62.2(4) . . ?
C17 C18 B11 60.5(3) . . ?
N2 C25 C18 116.8(4) . . ?
N2 C25 H25A 108.1 . . ?
C18 C25 H25A 108.1 . . ?
N2 C25 H25B 108.1 . . ?
C18 C25 H25B 108.1 . . ?
H25A C25 H25B 107.3 . . ?
C25 N2 Pd1 110.1(3) . . ?
C25 N2 H2A 106(4) . . ?
Pd1 N2 H2A 114(4) . . ?
C25 N2 H2B 110(4) . . ?
Pd1 N2 H2B 106(4) . . ?
H2A N2 H2B 110(6) . . ?
C1 O1 Pd1 123.8(3) . . ?
B2' Pd1 N1' 88.0(6) . . ?
B2 Pd1 N1 85.8(4) . . ?
B2' Pd1 N2 92.8(5) . . ?
N1' Pd1 N2 176.3(6) . . ?
B2 Pd1 N2 95.0(3) . . ?
N1 Pd1 N2 173.1(3) . . ?
B2' Pd1 O1 179.2(11) . . ?
N1' Pd1 O1 92.7(3) . . ?
B2 Pd1 O1 178.4(4) . . ?
N1 Pd1 O1 92.6(2) . . ?
N2 Pd1 O1 86.59(17) . . ?
N1 C7 C2 129.0(10) . . ?
N1 C7 H7 115.5 . . ?
C2 C7 H7 115.5 . . ?
C7 N1 C8 115.2(8) . . ?
C7 N1 Pd1 123.2(6) . . ?
C8 N1 Pd1 121.5(6) . . ?
N1 C8 C9 108.7(7) . . ?
N1 C8 H8A 110.0 . . ?
C9 C8 H8A 110.0 . . ?
N1 C8 H8B 110.0 . . ?
C9 C8 H8B 110.0 . . ?
H8A C8 H8B 108.3 . . ?
C8 C9 B3 119.5(8) . . ?
C8 C9 B4 121.0(8) . . ?
B3 C9 B4 64.1(7) . . ?
C8 C9 C10 119.9(7) . . ?
B3 C9 C10 112.9(7) . . ?
B4 C9 C10 60.3(6) . . ?
C8 C9 B1 115.2(8) . . ?
B3 C9 B1 114.9(8) . . ?
B4 C9 B1 112.5(8) . . ?
C10 C9 B1 61.0(6) . . ?
C8 C9 B2 115.6(7) . . ?
B3 C9 B2 65.0(11) . . ?
B4 C9 B2 116.6(9) . . ?
C10 C9 B2 111.7(9) . . ?
B1 C9 B2 61.3(10) . . ?
C11 C10 B9 122.6(7) . . ?
C11 C10 C9 120.8(7) . . ?
B9 C10 C9 108.6(7) . . ?
C11 C10 B5 120.0(8) . . ?
B9 C10 B5 61.5(7) . . ?
C9 C10 B5 108.9(7) . . ?
C11 C10 B4 120.8(8) . . ?
B9 C10 B4 61.8(7) . . ?
C9 C10 B4 59.8(6) . . ?
B5 C10 B4 111.9(8) . . ?
C11 C10 B1 116.6(8) . . ?
B9 C10 B1 112.3(8) . . ?
C9 C10 B1 60.0(6) . . ?
B5 C10 B1 62.4(7) . . ?
B4 C10 B1 111.2(7) . . ?
C9 B1 C10 58.9(5) . . ?
C9 B1 B2 59.7(6) . . ?
C10 B1 B2 108.6(9) . . ?
C9 B1 B6 104.9(8) . . ?
C10 B1 B6 105.9(9) . . ?
B2 B1 B6 60.6(7) . . ?
C9 B1 B5 104.6(8) . . ?
C10 B1 B5 57.9(7) . . ?
B2 B1 B5 109.7(9) . . ?
B6 B1 B5 60.4(7) . . ?
C9 B1 H1 124.3 . . ?
C10 B1 H1 122.8 . . ?
B2 B1 H1 119.9 . . ?
B6 B1 H1 122.8 . . ?
B5 B1 H1 122.4 . . ?
C9 B2 B1 59.0(8) . . ?
C9 B2 B6 104.0(11) . . ?
B1 B2 B6 60.0(10) . . ?
C9 B2 B7 101.7(9) . . ?
B1 B2 B7 107.4(10) . . ?
B6 B2 B7 60.3(7) . . ?
C9 B2 B3 56.6(7) . . ?
B1 B2 B3 106.2(8) . . ?
B6 B2 B3 106.2(9) . . ?
B7 B2 B3 58.0(9) . . ?
C9 B2 Pd1 108.3(7) . . ?
B1 B2 Pd1 114.2(13) . . ?
B6 B2 Pd1 135.6(11) . . ?
B7 B2 Pd1 137.0(14) . . ?
B3 B2 Pd1 116.8(12) . . ?
C9 B3 B7 105.1(8) . . ?
C9 B3 B8 103.6(8) . . ?
B7 B3 B8 60.2(8) . . ?
C9 B3 B4 58.0(6) . . ?
B7 B3 B4 106.8(9) . . ?
B8 B3 B4 58.6(8) . . ?
C9 B3 B2 58.4(7) . . ?
B7 B3 B2 60.6(7) . . ?
B8 B3 B2 107.7(10) . . ?
B4 B3 B2 106.4(10) . . ?
C9 B3 H3A 125.0 . . ?
B7 B3 H3A 122.0 . . ?
B8 B3 H3A 123.0 . . ?
B4 B3 H3A 123.0 . . ?
B2 B3 H3A 121.7 . . ?
C9 B4 C10 59.9(6) . . ?
C9 B4 B9 106.3(8) . . ?
C10 B4 B9 58.9(6) . . ?
C9 B4 B8 105.0(8) . . ?
C10 B4 B8 107.0(9) . . ?
B9 B4 B8 61.0(7) . . ?
C9 B4 B3 57.9(6) . . ?
C10 B4 B3 107.5(8) . . ?
B9 B4 B3 109.5(9) . . ?
B8 B4 B3 60.5(8) . . ?
C9 B4 H4A 124.0 . . ?
C10 B4 H4A 122.3 . . ?
B9 B4 H4A 121.3 . . ?
B8 B4 H4A 122.3 . . ?
B3 B4 H4A 121.4 . . ?
C10 B5 B9 59.1(7) . . ?
C10 B5 B1 59.7(6) . . ?
B9 B5 B1 108.2(9) . . ?
C10 B5 B6 106.5(10) . . ?
B9 B5 B6 108.8(8) . . ?
B1 B5 B6 59.4(7) . . ?
C10 B5 B10 106.3(8) . . ?
B9 B5 B10 60.6(5) . . ?
B1 B5 B10 107.4(8) . . ?
B6 B5 B10 60.0(5) . . ?
C10 B5 H5A 123.2 . . ?
B9 B5 H5A 121.1 . . ?
B1 B5 H5A 121.9 . . ?
B6 B5 H5A 121.9 . . ?
B10 B5 H5A 122.1 . . ?
B1 B6 B2 59.4(9) . . ?
B1 B6 B5 60.2(8) . . ?
B2 B6 B5 108.6(10) . . ?
B1 B6 B10 108.0(9) . . ?
B2 B6 B10 109.3(10) . . ?
B5 B6 B10 60.0(5) . . ?
B1 B6 B7 107.6(11) . . ?
B2 B6 B7 61.2(11) . . ?
B5 B6 B7 107.7(9) . . ?
B10 B6 B7 59.7(5) . . ?
B1 B6 H6A 122.2 . . ?
B2 B6 H6A 120.8 . . ?
B5 B6 H6A 121.7 . . ?
B10 B6 H6A 121.4 . . ?
B7 B6 H6A 121.8 . . ?
B3 B7 B8 60.3(8) . . ?
B3 B7 B10 107.7(9) . . ?
B8 B7 B10 59.0(5) . . ?
B3 B7 B6 107.4(9) . . ?
B8 B7 B6 106.2(8) . . ?
B10 B7 B6 59.5(5) . . ?
B3 B7 B2 61.4(8) . . ?
B8 B7 B2 108.4(9) . . ?
B10 B7 B2 106.9(10) . . ?
B6 B7 B2 58.5(10) . . ?
B3 B7 H7A 121.1 . . ?
B8 B7 H7A 122.2 . . ?
B10 B7 H7A 122.5 . . ?
B6 B7 H7A 123.1 . . ?
B2 B7 H7A 121.7 . . ?
B4 B8 B10 107.7(8) . . ?
B4 B8 B9 59.2(7) . . ?
B10 B8 B9 60.3(6) . . ?
B4 B8 B7 108.2(9) . . ?
B10 B8 B7 60.5(6) . . ?
B9 B8 B7 108.6(8) . . ?
B4 B8 B3 61.0(7) . . ?
B10 B8 B3 108.3(8) . . ?
B9 B8 B3 108.5(9) . . ?
B7 B8 B3 59.5(8) . . ?
B4 B8 H8 121.8 . . ?
B10 B8 H8 121.5 . . ?
B9 B8 H8 121.6 . . ?
B7 B8 H8 121.5 . . ?
B3 B8 H8 121.3 . . ?
C10 B9 B5 59.4(7) . . ?
C10 B9 B4 59.3(6) . . ?
B5 B9 B4 108.1(8) . . ?
C10 B9 B10 106.9(7) . . ?
B5 B9 B10 61.0(5) . . ?
B4 B9 B10 107.4(8) . . ?
C10 B9 B8 106.4(8) . . ?
B5 B9 B8 108.5(7) . . ?
B4 B9 B8 59.8(8) . . ?
B10 B9 B8 59.4(5) . . ?
C10 B9 H9 123.1 . . ?
B5 B9 H9 121.0 . . ?
B4 B9 H9 121.9 . . ?
B10 B9 H9 122.0 . . ?
B8 B9 H9 122.2 . . ?
B8 B10 B9 60.3(7) . . ?
B8 B10 B5 107.1(9) . . ?
B9 B10 B5 58.4(6) . . ?
B8 B10 B6 108.4(8) . . ?
B9 B10 B6 107.0(8) . . ?
B5 B10 B6 59.9(7) . . ?
B8 B10 B7 60.4(7) . . ?
B9 B10 B7 108.6(8) . . ?
B5 B10 B7 108.5(8) . . ?
B6 B10 B7 60.8(6) . . ?
B8 B10 H10 121.6 . . ?
B9 B10 H10 122.4 . . ?
B5 B10 H10 122.5 . . ?
B6 B10 H10 121.6 . . ?
B7 B10 H10 120.7 . . ?
C12 C11 C16 116.6(9) . . ?
C12 C11 C10 121.9(8) . . ?
C16 C11 C10 121.3(8) . . ?
C11 C12 C13 122.6(9) . . ?
C11 C12 H12A 118.7 . . ?
C13 C12 H12A 118.7 . . ?
C14 C13 C12 116.4(9) . . ?
C14 C13 H13A 121.8 . . ?
C12 C13 H13A 121.8 . . ?
C13 C14 C15 126.0(10) . . ?
C13 C14 H14A 117.0 . . ?
C15 C14 H14A 117.0 . . ?
C14 C15 C16 116.2(10) . . ?
C14 C15 H15A 121.9 . . ?
C16 C15 H15A 121.9 . . ?
C11 C16 C15 121.5(10) . . ?
C11 C16 H16A 119.3 . . ?
C15 C16 H16A 119.3 . . ?
N1' C7' C2 129(2) . . ?
N1' C7' H7' 115.3 . . ?
C2 C7' H7' 115.3 . . ?
C7' N1' C8' 119.0(16) . . ?
C7' N1' Pd1 122.4(14) . . ?
C8' N1' Pd1 118.5(10) . . ?
N1' C8' C9' 108.6(12) . . ?
N1' C8' H8'1 110.0 . . ?
C9' C8' H8'1 110.0 . . ?
N1' C8' H8'2 110.0 . . ?
C9' C8' H8'2 110.0 . . ?
H8'1 C8' H8'2 108.3 . . ?
C8' C9' C10' 121.6(12) . . ?
C8' C9' B1' 117.3(16) . . ?
C10' C9' B1' 61.2(8) . . ?
C8' C9' B4' 121.0(14) . . ?
C10' C9' B4' 60.5(8) . . ?
B1' C9' B4' 112.2(12) . . ?
C8' C9' B2' 115.2(12) . . ?
C10' C9' B2' 112.0(13) . . ?
B1' C9' B2' 61.4(14) . . ?
B4' C9' B2' 115.4(16) . . ?
C8' C9' B3' 119.1(15) . . ?
C10' C9' B3' 111.3(14) . . ?
B1' C9' B3' 113.1(14) . . ?
B4' C9' B3' 62.7(11) . . ?
B2' C9' B3' 64.0(15) . . ?
C11' C10' C9' 118.4(13) . . ?
C11' C10' B9' 122.3(12) . . ?
C9' C10' B9' 109.8(12) . . ?
C11' C10' B5' 123.6(13) . . ?
C9' C10' B5' 108.6(12) . . ?
B9' C10' B5' 61.0(10) . . ?
C11' C10' B4' 117.8(13) . . ?
C9' C10' B4' 61.0(11) . . ?
B9' C10' B4' 61.9(12) . . ?
B5' C10' B4' 111.2(13) . . ?
C11' C10' B1' 118.7(13) . . ?
C9' C10' B1' 60.1(8) . . ?
B9' C10' B1' 111.6(13) . . ?
B5' C10' B1' 61.4(13) . . ?
B4' C10' B1' 111.7(11) . . ?
C9' B1' C10' 58.6(8) . . ?
C9' B1' B5' 105.2(14) . . ?
C10' B1' B5' 58.7(11) . . ?
C9' B1' B2' 59.8(9) . . ?
C10' B1' B2' 108.5(13) . . ?
B5' B1' B2' 110.0(16) . . ?
C9' B1' B6' 105.3(14) . . ?
C10' B1' B6' 106.2(14) . . ?
B5' B1' B6' 60.3(12) . . ?
B2' B1' B6' 60.8(14) . . ?
C9' B1' H1' 124.1 . . ?
C10' B1' H1' 122.8 . . ?
B5' B1' H1' 121.9 . . ?
B2' B1' H1' 120.0 . . ?
B6' B1' H1' 122.7 . . ?
C9' B2' B1' 58.8(11) . . ?
C9' B2' B6' 104.4(16) . . ?
B1' B2' B6' 60.6(17) . . ?
C9' B2' B3' 58.1(12) . . ?
B1' B2' B3' 106.2(11) . . ?
B6' B2' B3' 104.4(19) . . ?
C9' B2' B7' 101.8(17) . . ?
B1' B2' B7' 106.8(17) . . ?
B6' B2' B7' 59.4(13) . . ?
B3' B2' B7' 56.4(18) . . ?
C9' B2' Pd1 107.6(13) . . ?
B1' B2' Pd1 115(2) . . ?
B6' B2' Pd1 137(2) . . ?
B3' B2' Pd1 117(2) . . ?
B7' B2' Pd1 137(2) . . ?
C9' B3' B7' 106.9(16) . . ?
C9' B3' B8' 103.6(15) . . ?
B7' B3' B8' 61.3(15) . . ?
C9' B3' B4' 58.6(10) . . ?
B7' B3' B4' 107.8(19) . . ?
B8' B3' B4' 57.4(14) . . ?
C9' B3' B2' 58.0(11) . . ?
B7' B3' B2' 62.9(16) . . ?
B8' B3' B2' 109.8(18) . . ?
B4' B3' B2' 107.1(14) . . ?
C9' B3' H3' 124.9 . . ?
B7' B3' H3' 120.1 . . ?
B8' B3' H3' 122.8 . . ?
B4' B3' H3' 123.2 . . ?
B2' B3' H3' 120.5 . . ?
C10' B4' B8' 107.1(15) . . ?
C10' B4' C9' 58.5(9) . . ?
B8' B4' C9' 106.4(15) . . ?
C10' B4' B9' 58.6(12) . . ?
B8' B4' B9' 60.7(13) . . ?
C9' B4' B9' 105.3(13) . . ?
C10' B4' B3' 106.5(13) . . ?
B8' B4' B3' 60.9(17) . . ?
C9' B4' B3' 58.7(12) . . ?
B9' B4' B3' 108.6(17) . . ?
C10' B4' H4' 123.1 . . ?
B8' B4' H4' 121.5 . . ?
C9' B4' H4' 123.9 . . ?
B9' B4' H4' 122.2 . . ?
B3' B4' H4' 121.6 . . ?
C10' B5' B9' 59.4(13) . . ?
C10' B5' B1' 59.9(11) . . ?
B9' B5' B1' 109.0(17) . . ?
C10' B5' B6' 107.6(16) . . ?
B9' B5' B6' 109.1(11) . . ?
B1' B5' B6' 60.9(13) . . ?
C10' B5' B10' 106.8(13) . . ?
B9' B5' B10' 60.8(7) . . ?
B1' B5' B10' 108.5(14) . . ?
B6' B5' B10' 59.6(7) . . ?
C10' B5' H5' 122.8 . . ?
B9' B5' H5' 120.9 . . ?
B1' B5' H5' 120.9 . . ?
B6' B5' H5' 121.4 . . ?
B10' B5' H5' 122.0 . . ?
B10' B6' B5' 60.7(7) . . ?
B10' B6' B1' 107.7(13) . . ?
B5' B6' B1' 58.9(13) . . ?
B10' B6' B2' 109.9(18) . . ?
B5' B6' B2' 107.1(16) . . ?
B1' B6' B2' 58.6(14) . . ?
B10' B6' B7' 59.4(7) . . ?
B5' B6' B7' 107.5(12) . . ?
B1' B6' B7' 107.6(19) . . ?
B2' B6' B7' 62(2) . . ?
B10' B6' H6' 121.0 . . ?
B5' B6' H6' 122.5 . . ?
B1' B6' H6' 123.0 . . ?
B2' B6' H6' 120.9 . . ?
B7' B6' H6' 121.4 . . ?
B3' B7' B10' 108.0(16) . . ?
B3' B7' B8' 60.3(17) . . ?
B10' B7' B8' 59.2(7) . . ?
B3' B7' B6' 107(2) . . ?
B10' B7' B6' 59.2(7) . . ?
B8' B7' B6' 105.7(11) . . ?
B3' B7' B2' 60.7(15) . . ?
B10' B7' B2' 106.4(17) . . ?
B8' B7' B2' 107(2) . . ?
B6' B7' B2' 58.2(18) . . ?
B3' B7' H7'1 121.1 . . ?
B10' B7' H7'1 122.3 . . ?
B8' B7' H7'1 122.5 . . ?
B6' B7' H7'1 123.5 . . ?
B2' B7' H7'1 122.5 . . ?
B4' B8' B9' 60.7(14) . . ?
B4' B8' B10' 109.5(14) . . ?
B9' B8' B10' 60.8(7) . . ?
B4' B8' B3' 61.8(14) . . ?
B9' B8' B3' 109.3(19) . . ?
B10' B8' B3' 107.0(16) . . ?
B4' B8' B7' 109(2) . . ?
B9' B8' B7' 108.8(12) . . ?
B10' B8' B7' 59.8(7) . . ?
B3' B8' B7' 58.4(16) . . ?
B4' B8' H8'A 120.1 . . ?
B9' B8' H8'A 120.7 . . ?
B10' B8' H8'A 121.7 . . ?
B3' B8' H8'A 122.0 . . ?
B7' B8' H8'A 122.1 . . ?
C10' B9' B5' 59.7(13) . . ?
C10' B9' B4' 59.5(12) . . ?
B5' B9' B4' 108.2(18) . . ?
C10' B9' B8' 106.0(17) . . ?
B5' B9' B8' 108.9(11) . . ?
B4' B9' B8' 58.5(14) . . ?
C10' B9' B10' 107.6(13) . . ?
B5' B9' B10' 61.5(7) . . ?
B4' B9' B10' 107.1(14) . . ?
B8' B9' B10' 59.9(7) . . ?
C10' B9' H9' 122.8 . . ?
B5' B9' H9' 120.6 . . ?
B4' B9' H9' 122.5 . . ?
B8' B9' H9' 122.5 . . ?
B10' B9' H9' 121.5 . . ?
B8' B10' B6' 108.7(14) . . ?
B8' B10' B7' 61.0(10) . . ?
B6' B10' B7' 61.3(8) . . ?
B8' B10' B9' 59.3(9) . . ?
B6' B10' B9' 106.7(13) . . ?
B7' B10' B9' 108.4(14) . . ?
B8' B10' B5' 105.4(13) . . ?
B6' B10' B5' 59.7(9) . . ?
B7' B10' B5' 108.3(13) . . ?
B9' B10' B5' 57.8(8) . . ?
B8' B10' H10' 122.1 . . ?
B6' B10' H10' 121.3 . . ?
B7' B10' H10' 120.3 . . ?
B9' B10' H10' 122.9 . . ?
B5' B10' H10' 123.4 . . ?
C16' C11' C12' 118.1(14) . . ?
C16' C11' C10' 121.6(11) . . ?
C12' C11' C10' 119.7(11) . . ?
C11' C12' C13' 121.1(15) . . ?
C11' C12' H12' 119.5 . . ?
C13' C12' H12' 119.5 . . ?
C14' C13' C12' 114.0(15) . . ?
C14' C13' H13' 123.0 . . ?
C12' C13' H13' 123.0 . . ?
C15' C14' C13' 127.8(17) . . ?
C15' C14' H14' 116.1 . . ?
C13' C14' H14' 116.1 . . ?
C14' C15' C16' 118.9(16) . . ?
C14' C15' H15' 120.6 . . ?
C16' C15' H15' 120.6 . . ?
C11' C16' C15' 117.4(15) . . ?
C11' C16' H16' 121.3 . . ?
C15' C16' H16' 121.3 . . ?
C24 C19 C20 117.6(10) . . ?
C24 C19 C17 121.5(13) . . ?
C20 C19 C17 120.9(13) . . ?
C19 C20 C21 119.4(11) . . ?
C19 C20 H20A 120.3 . . ?
C21 C20 H20A 120.3 . . ?
C22 C21 C20 121.7(11) . . ?
C22 C21 H21 119.2 . . ?
C20 C21 H21 119.2 . . ?
C21 C22 C23 120.5(12) . . ?
C21 C22 H22 119.8 . . ?
C23 C22 H22 119.8 . . ?
C22 C23 C24 119.3(12) . . ?
C22 C23 H23 120.3 . . ?
C24 C23 H23 120.3 . . ?
C19 C24 C23 121.5(11) . . ?
C19 C24 H24 119.3 . . ?
C23 C24 H24 119.3 . . ?
C20' C19' C24' 117.8(13) . . ?
C20' C19' C17 121.5(18) . . ?
C24' C19' C17 120.2(18) . . ?
C19' C20' C21' 122.7(13) . . ?
C19' C20' H20' 118.7 . . ?
C21' C20' H20' 118.7 . . ?
C22' C21' C20' 117.4(14) . . ?
C22' C21' H21' 121.3 . . ?
C20' C21' H21' 121.3 . . ?
C21' C22' C23' 122.4(15) . . ?
C21' C22' H22' 118.8 . . ?
C23' C22' H22' 118.8 . . ?
C22' C23' C24' 121.8(14) . . ?
C22' C23' H23' 119.1 . . ?
C24' C23' H23' 119.1 . . ?
C19' C24' C23' 117.7(13) . . ?
C19' C24' H24' 121.2 . . ?
C23' C24' H24' 121.2 . . ?

_refine_diff_density_max         1.255
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.105

####################################################################### 
# 
# 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_28
_database_code_depnum_ccdc_archive 'CCDC 1583781'
_audit_update_record             
;
2017-11-03 deposited with the CCDC.
2018-03-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H31 B10 N'
_chemical_formula_weight         381.55

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C2/c  '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-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                   17.6118(12)
_cell_length_b                   12.1001(9)
_cell_length_c                   20.3538(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.094(3)
_cell_angle_gamma                90.00
_cell_volume                     4326.4(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    175(2)
_cell_measurement_reflns_used    3919
_cell_measurement_theta_min      0.985
_cell_measurement_theta_max      25.390

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1616
_exptl_absorpt_coefficient_mu    0.060
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      175(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15563
_diffrn_reflns_av_R_equivalents  0.0946
_diffrn_reflns_av_sigmaI/netI    0.0752
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.81
_diffrn_reflns_theta_max         25.39
_reflns_number_total             3919
_reflns_number_gt                2609
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0609P)²+0.8353P] 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         3919
_refine_ls_number_parameters     290
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1079
_refine_ls_R_factor_gt           0.0589
_refine_ls_wR_factor_ref         0.1303
_refine_ls_wR_factor_gt          0.1165
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_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
H1B H 0.1433(15) 0.452(3) 0.2383(14) 0.055(9) Uiso 1 1 d . . .
H1A H 0.1311(13) 0.341(2) 0.2641(13) 0.037(8) Uiso 1 1 d . . .
H13B H 0.2012(10) 0.3963(16) 0.1534(10) 0.013(5) Uiso 1 1 d . . .
H13A H 0.2400(11) 0.3280(16) 0.2144(10) 0.018(5) Uiso 1 1 d . . .
N1 N 0.13160(11) 0.38148(19) 0.22688(11) 0.0263(5) Uani 1 1 d . . .
C18 C 0.21720(11) 0.12071(16) 0.27824(10) 0.0173(5) Uani 1 1 d . . .
C24 C 0.33455(11) 0.18381(17) 0.14434(10) 0.0190(5) Uani 1 1 d . . .
C25 C 0.39076(11) 0.10322(18) 0.15676(11) 0.0234(5) Uani 1 1 d . . .
H25 H 0.3762 0.0276 0.1572 0.028 Uiso 1 1 calc R . .
C27 C 0.48930(12) 0.23938(19) 0.16719(11) 0.0274(6) Uani 1 1 d . . .
H27 H 0.5412 0.2587 0.1767 0.033 Uiso 1 1 calc R . .
C20 C 0.18680(12) 0.09425(19) 0.39198(11) 0.0287(6) Uani 1 1 d . . .
H20 H 0.1515 0.0711 0.4224 0.034 Uiso 1 1 calc R . .
C1 C 0.17311(11) 0.22818(16) 0.15544(10) 0.0158(5) Uani 1 1 d . . .
C26 C 0.46707(12) 0.1305(2) 0.16838(12) 0.0287(6) Uani 1 1 d . . .
H26 H 0.5039 0.0741 0.1771 0.034 Uiso 1 1 calc R . .
C13 C 0.19188(12) 0.33977(18) 0.18802(11) 0.0185(5) Uani 1 1 d . . .
C2 C 0.09507(11) 0.20985(17) 0.09885(10) 0.0182(5) Uani 1 1 d . . .
C28 C 0.43588(12) 0.32001(19) 0.15221(12) 0.0274(6) Uani 1 1 d . . .
H28 H 0.4513 0.3951 0.1500 0.033 Uiso 1 1 calc R . .
C22 C 0.30813(12) 0.16683(19) 0.36949(11) 0.0283(6) Uani 1 1 d . . .
H22 H 0.3567 0.1946 0.3845 0.034 Uiso 1 1 calc R . .
B5 B 0.24840(13) 0.14603(19) 0.13478(12) 0.0184(5) Uani 1 1 d . . .
C14 C 0.03656(12) 0.30484(18) 0.07769(11) 0.0235(5) Uani 1 1 d . . .
C23 C 0.28847(12) 0.15962(18) 0.30251(11) 0.0248(5) Uani 1 1 d . . .
H23 H 0.3243 0.1817 0.2723 0.030 Uiso 1 1 calc R . .
C29 C 0.35981(12) 0.29276(18) 0.14030(11) 0.0240(5) Uani 1 1 d . . .
H29 H 0.3239 0.3496 0.1291 0.029 Uiso 1 1 calc R . .
C19 C 0.16758(12) 0.08845(18) 0.32473(11) 0.0241(5) Uani 1 1 d . . .
H19 H 0.1187 0.0614 0.3100 0.029 Uiso 1 1 calc R . .
C16 C -0.02372(11) 0.3171(2) 0.12780(12) 0.0305(6) Uani 1 1 d . . .
H16A H -0.0628 0.3697 0.1110 0.046 Uiso 1 1 calc R . .
H16B H 0.0003 0.3444 0.1696 0.046 Uiso 1 1 calc R . .
H16C H -0.0473 0.2452 0.1349 0.046 Uiso 1 1 calc R . .
C21 C 0.25771(13) 0.13400(19) 0.41454(12) 0.0293(6) Uani 1 1 d . . .
H21 H 0.2714 0.1386 0.4605 0.035 Uiso 1 1 calc R . .
C15 C 0.07425(12) 0.41743(18) 0.06875(12) 0.0308(6) Uani 1 1 d . . .
H15A H 0.1133 0.4106 0.0370 0.046 Uiso 1 1 calc R . .
H15B H 0.0979 0.4427 0.1112 0.046 Uiso 1 1 calc R . .
H15C H 0.0357 0.4710 0.0524 0.046 Uiso 1 1 calc R . .
B11 B 0.06183(14) 0.0784(2) 0.10753(13) 0.0228(6) Uani 1 1 d . . .
H11 H 0.0001 0.0571 0.0985 0.027 Uiso 1 1 calc R . .
B3 B 0.09601(13) 0.1539(2) 0.17798(13) 0.0203(6) Uani 1 1 d . . .
H3 H 0.0571 0.1840 0.2154 0.024 Uiso 1 1 calc R . .
C17 C -0.00456(14) 0.2739(2) 0.01102(13) 0.0390(7) Uani 1 1 d . . .
H17A H -0.0277 0.2006 0.0142 0.058 Uiso 1 1 calc R . .
H17B H 0.0321 0.2729 -0.0230 0.058 Uiso 1 1 calc R . .
H17C H -0.0443 0.3285 -0.0007 0.058 Uiso 1 1 calc R . .
B6 B 0.18618(13) 0.2113(2) 0.07284(12) 0.0200(6) Uani 1 1 d . . .
H6 H 0.2065 0.2795 0.0412 0.024 Uiso 1 1 calc R . .
B4 B 0.19118(13) 0.1100(2) 0.20235(12) 0.0184(5) Uani 1 1 d . . .
B9 B 0.21502(14) 0.0078(2) 0.14389(13) 0.0228(6) Uani 1 1 d . . .
H9 H 0.2550 -0.0613 0.1585 0.027 Uiso 1 1 calc R . .
B7 B 0.11858(14) 0.1111(2) 0.04206(13) 0.0252(6) Uani 1 1 d . . .
H7 H 0.0953 0.1105 -0.0106 0.030 Uiso 1 1 calc R . .
B12 B 0.13540(14) -0.0131(2) 0.08659(13) 0.0256(6) Uani 1 1 d . . .
H12 H 0.1229 -0.0959 0.0637 0.031 Uiso 1 1 calc R . .
B10 B 0.12113(13) 0.0135(2) 0.17063(13) 0.0225(6) Uani 1 1 d . . .
H10 H 0.0986 -0.0517 0.2032 0.027 Uiso 1 1 calc R . .
B8 B 0.21298(14) 0.0704(2) 0.06466(13) 0.0248(6) Uani 1 1 d . . .
H8 H 0.2521 0.0434 0.0267 0.030 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
N1 C13 1.459(3) . ?
N1 H1B 0.90(3) . ?
N1 H1A 0.90(3) . ?
C18 C19 1.389(3) . ?
C18 C23 1.397(3) . ?
C18 B4 1.585(3) . ?
C24 C29 1.396(3) . ?
C24 C25 1.400(3) . ?
C24 B5 1.583(3) . ?
C25 C26 1.388(3) . ?
C25 H25 0.9500 . ?
C27 C28 1.374(3) . ?
C27 C26 1.375(3) . ?
C27 H27 0.9500 . ?
C20 C21 1.386(3) . ?
C20 C19 1.388(3) . ?
C20 H20 0.9500 . ?
C1 C13 1.530(3) . ?
C1 B3 1.718(3) . ?
C1 B6 1.725(3) . ?
C1 B5 1.733(3) . ?
C1 B4 1.737(3) . ?
C1 C2 1.743(3) . ?
C26 H26 0.9500 . ?
C13 H13B 1.00(2) . ?
C13 H13A 0.98(2) . ?
C2 C14 1.583(3) . ?
C2 B11 1.709(3) . ?
C2 B6 1.725(3) . ?
C2 B7 1.733(3) . ?
C2 B3 1.746(3) . ?
C28 C29 1.384(3) . ?
C28 H28 0.9500 . ?
C22 C21 1.380(3) . ?
C22 C23 1.385(3) . ?
C22 H22 0.9500 . ?
B5 B8 1.771(4) . ?
B5 B9 1.787(3) . ?
B5 B6 1.794(3) . ?
B5 B4 1.815(3) . ?
C14 C16 1.531(3) . ?
C14 C15 1.532(3) . ?
C14 C17 1.538(3) . ?
C23 H23 0.9500 . ?
C29 H29 0.9500 . ?
C19 H19 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C21 H21 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
B11 B7 1.767(3) . ?
B11 B3 1.769(4) . ?
B11 B12 1.779(4) . ?
B11 B10 1.779(4) . ?
B11 H11 1.1200 . ?
B3 B10 1.765(4) . ?
B3 B4 1.794(3) . ?
B3 H3 1.1200 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
B6 B8 1.780(4) . ?
B6 B7 1.782(3) . ?
B6 H6 1.1200 . ?
B4 B10 1.785(3) . ?
B4 B9 1.787(3) . ?
B9 B12 1.777(4) . ?
B9 B10 1.779(3) . ?
B9 B8 1.780(4) . ?
B9 H9 1.1200 . ?
B7 B8 1.763(4) . ?
B7 B12 1.769(4) . ?
B7 H7 1.1200 . ?
B12 B10 1.776(4) . ?
B12 B8 1.782(4) . ?
B12 H12 1.1200 . ?
B10 H10 1.1200 . ?
B8 H8 1.1200 . ?

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
C13 N1 H1B 107.7(17) . . ?
C13 N1 H1A 108.7(15) . . ?
H1B N1 H1A 108(2) . . ?
C19 C18 C23 116.5(2) . . ?
C19 C18 B4 119.26(18) . . ?
C23 C18 B4 124.20(18) . . ?
C29 C24 C25 116.39(19) . . ?
C29 C24 B5 124.90(19) . . ?
C25 C24 B5 118.70(18) . . ?
C26 C25 C24 121.9(2) . . ?
C26 C25 H25 119.0 . . ?
C24 C25 H25 119.0 . . ?
C28 C27 C26 119.5(2) . . ?
C28 C27 H27 120.2 . . ?
C26 C27 H27 120.2 . . ?
C21 C20 C19 119.7(2) . . ?
C21 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
C13 C1 B3 119.77(17) . . ?
C13 C1 B6 119.13(16) . . ?
B3 C1 B6 111.19(16) . . ?
C13 C1 B5 117.77(16) . . ?
B3 C1 B5 113.44(16) . . ?
B6 C1 B5 62.49(13) . . ?
C13 C1 B4 117.60(17) . . ?
B3 C1 B4 62.58(13) . . ?
B6 C1 B4 113.99(16) . . ?
B5 C1 B4 63.10(13) . . ?
C13 C1 C2 122.31(16) . . ?
B3 C1 C2 60.59(12) . . ?
B6 C1 C2 59.65(12) . . ?
B5 C1 C2 110.33(16) . . ?
B4 C1 C2 111.31(15) . . ?
C27 C26 C25 119.9(2) . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
N1 C13 C1 113.40(17) . . ?
N1 C13 H13B 107.9(11) . . ?
C1 C13 H13B 109.8(11) . . ?
N1 C13 H13A 112.8(12) . . ?
C1 C13 H13A 105.1(12) . . ?
H13B C13 H13A 107.7(16) . . ?
C14 C2 B11 118.88(16) . . ?
C14 C2 B6 120.71(17) . . ?
B11 C2 B6 112.00(16) . . ?
C14 C2 B7 120.07(17) . . ?
B11 C2 B7 61.77(14) . . ?
B6 C2 B7 62.02(13) . . ?
C14 C2 C1 123.69(16) . . ?
B11 C2 C1 108.05(16) . . ?
B6 C2 C1 59.65(12) . . ?
B7 C2 C1 108.29(15) . . ?
C14 C2 B3 119.71(17) . . ?
B11 C2 B3 61.59(14) . . ?
B6 C2 B3 109.84(16) . . ?
B7 C2 B3 111.15(17) . . ?
C1 C2 B3 58.99(12) . . ?
C27 C28 C29 120.6(2) . . ?
C27 C28 H28 119.7 . . ?
C29 C28 H28 119.7 . . ?
C21 C22 C23 120.6(2) . . ?
C21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C24 B5 C1 123.21(17) . . ?
C24 B5 B8 121.85(18) . . ?
C1 B5 B8 105.09(16) . . ?
C24 B5 B9 125.24(18) . . ?
C1 B5 B9 104.40(15) . . ?
B8 B5 B9 60.03(14) . . ?
C24 B5 B6 119.42(18) . . ?
C1 B5 B6 58.54(12) . . ?
B8 B5 B6 59.92(14) . . ?
B9 B5 B6 107.24(17) . . ?
C24 B5 B4 123.72(19) . . ?
C1 B5 B4 58.55(12) . . ?
B8 B5 B4 107.68(16) . . ?
B9 B5 B4 59.46(13) . . ?
B6 B5 B4 107.10(15) . . ?
C16 C14 C15 108.64(18) . . ?
C16 C14 C17 107.83(18) . . ?
C15 C14 C17 107.00(19) . . ?
C16 C14 C2 111.00(18) . . ?
C15 C14 C2 113.50(17) . . ?
C17 C14 C2 108.65(18) . . ?
C22 C23 C18 121.6(2) . . ?
C22 C23 H23 119.2 . . ?
C18 C23 H23 119.2 . . ?
C28 C29 C24 121.5(2) . . ?
C28 C29 H29 119.2 . . ?
C24 C29 H29 119.2 . . ?
C20 C19 C18 122.4(2) . . ?
C20 C19 H19 118.8 . . ?
C18 C19 H19 118.8 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C22 C21 C20 119.2(2) . . ?
C22 C21 H21 120.4 . . ?
C20 C21 H21 120.4 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C2 B11 B7 59.79(13) . . ?
C2 B11 B3 60.25(13) . . ?
B7 B11 B3 108.51(17) . . ?
C2 B11 B12 107.08(17) . . ?
B7 B11 B12 59.86(14) . . ?
B3 B11 B12 107.70(17) . . ?
C2 B11 B10 107.33(17) . . ?
B7 B11 B10 107.99(18) . . ?
B3 B11 B10 59.65(14) . . ?
B12 B11 B10 59.88(15) . . ?
C2 B11 H11 122.2 . . ?
B7 B11 H11 121.5 . . ?
B3 B11 H11 121.5 . . ?
B12 B11 H11 122.2 . . ?
B10 B11 H11 122.0 . . ?
C1 B3 C2 60.42(12) . . ?
C1 B3 B10 105.87(16) . . ?
C2 B3 B10 106.33(18) . . ?
C1 B3 B11 106.47(17) . . ?
C2 B3 B11 58.16(13) . . ?
B10 B3 B11 60.46(14) . . ?
C1 B3 B4 59.22(12) . . ?
C2 B3 B4 108.48(16) . . ?
B10 B3 B4 60.21(13) . . ?
B11 B3 B4 109.16(18) . . ?
C1 B3 H3 123.0 . . ?
C2 B3 H3 122.3 . . ?
B10 B3 H3 122.6 . . ?
B11 B3 H3 122.0 . . ?
B4 B3 H3 120.8 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C2 B6 C1 60.69(12) . . ?
C2 B6 B8 106.10(17) . . ?
C1 B6 B8 105.01(17) . . ?
C2 B6 B7 59.20(13) . . ?
C1 B6 B7 106.90(16) . . ?
B8 B6 B7 59.34(14) . . ?
C2 B6 B5 108.34(16) . . ?
C1 B6 B5 58.97(13) . . ?
B8 B6 B5 59.40(14) . . ?
B7 B6 B5 107.85(17) . . ?
C2 B6 H6 121.7 . . ?
C1 B6 H6 122.9 . . ?
B8 B6 H6 123.6 . . ?
B7 B6 H6 122.1 . . ?
B5 B6 H6 121.6 . . ?
C18 B4 C1 119.80(17) . . ?
C18 B4 B10 123.39(18) . . ?
C1 B4 B10 104.18(16) . . ?
C18 B4 B9 129.84(19) . . ?
C1 B4 B9 104.27(17) . . ?
B10 B4 B9 59.73(14) . . ?
C18 B4 B3 116.39(17) . . ?
C1 B4 B3 58.20(12) . . ?
B10 B4 B3 59.07(13) . . ?
B9 B4 B3 106.27(17) . . ?
C18 B4 B5 125.53(17) . . ?
C1 B4 B5 58.35(12) . . ?
B10 B4 B5 106.85(17) . . ?
B9 B4 B5 59.49(13) . . ?
B3 B4 B5 106.11(17) . . ?
B12 B9 B10 59.94(14) . . ?
B12 B9 B8 60.13(15) . . ?
B10 B9 B8 107.56(18) . . ?
B12 B9 B4 108.88(17) . . ?
B10 B9 B4 60.10(13) . . ?
B8 B9 B4 108.54(18) . . ?
B12 B9 B5 108.36(19) . . ?
B10 B9 B5 108.38(17) . . ?
B8 B9 B5 59.52(14) . . ?
B4 B9 B5 61.05(13) . . ?
B12 B9 H9 121.4 . . ?
B10 B9 H9 121.9 . . ?
B8 B9 H9 122.0 . . ?
B4 B9 H9 120.9 . . ?
B5 B9 H9 121.4 . . ?
C2 B7 B8 106.51(17) . . ?
C2 B7 B11 58.44(13) . . ?
B8 B7 B11 108.32(19) . . ?
C2 B7 B12 106.46(18) . . ?
B8 B7 B12 60.58(15) . . ?
B11 B7 B12 60.41(15) . . ?
C2 B7 B6 58.78(13) . . ?
B8 B7 B6 60.29(14) . . ?
B11 B7 B6 106.69(18) . . ?
B12 B7 B6 108.36(18) . . ?
C2 B7 H7 123.7 . . ?
B8 B7 H7 121.5 . . ?
B11 B7 H7 122.2 . . ?
B12 B7 H7 121.4 . . ?
B6 B7 H7 122.1 . . ?
B7 B12 B10 108.03(18) . . ?
B7 B12 B9 108.12(17) . . ?
B10 B12 B9 60.09(14) . . ?
B7 B12 B11 59.73(14) . . ?
B10 B12 B11 60.06(14) . . ?
B9 B12 B11 107.97(18) . . ?
B7 B12 B8 59.54(14) . . ?
B10 B12 B8 107.60(18) . . ?
B9 B12 B8 60.03(14) . . ?
B11 B12 B8 106.96(17) . . ?
B7 B12 H12 121.8 . . ?
B10 B12 H12 121.7 . . ?
B9 B12 H12 121.5 . . ?
B11 B12 H12 122.1 . . ?
B8 B12 H12 122.3 . . ?
B3 B10 B12 108.03(18) . . ?
B3 B10 B9 107.91(17) . . ?
B12 B10 B9 59.97(14) . . ?
B3 B10 B11 59.89(14) . . ?
B12 B10 B11 60.05(15) . . ?
B9 B10 B11 107.87(18) . . ?
B3 B10 B4 60.71(13) . . ?
B12 B10 B4 108.96(17) . . ?
B9 B10 B4 60.17(13) . . ?
B11 B10 B4 109.10(17) . . ?
B3 B10 H10 121.7 . . ?
B12 B10 H10 121.5 . . ?
B9 B10 H10 122.0 . . ?
B11 B10 H10 121.5 . . ?
B4 B10 H10 120.7 . . ?
B7 B8 B5 109.72(18) . . ?
B7 B8 B9 108.24(17) . . ?
B5 B8 B9 60.44(14) . . ?
B7 B8 B6 60.37(14) . . ?
B5 B8 B6 60.68(14) . . ?
B9 B8 B6 108.16(18) . . ?
B7 B8 B12 59.88(14) . . ?
B5 B8 B12 108.87(18) . . ?
B9 B8 B12 59.84(14) . . ?
B6 B8 B12 107.86(17) . . ?
B7 B8 H8 121.1 . . ?
B5 B8 H8 120.5 . . ?
B9 B8 H8 121.8 . . ?
B6 B8 H8 121.6 . . ?
B12 B8 H8 121.9 . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        25.39
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.212
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.050
