# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_tw018_0ma

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H44 B O3 P'
_chemical_formula_sum            'C22 H44 B O3 P'
_chemical_formula_weight         398.35

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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                   14.6340(13)
_cell_length_b                   11.9762(11)
_cell_length_c                   13.9876(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.376(4)
_cell_angle_gamma                90.00
_cell_volume                     2312.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9739
_exptl_absorpt_correction_T_max  0.9868
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20151
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_sigmaI/netI    0.0637
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.48
_diffrn_reflns_theta_max         27.65
_reflns_number_total             5327
_reflns_number_gt                3680
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.1000P)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         5327
_refine_ls_number_parameters     248
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0481
_refine_ls_wR_factor_ref         0.1525
_refine_ls_wR_factor_gt          0.1283
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_restrained_S_all      0.932
_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
P1 P 0.33025(4) 1.03695(4) 0.20229(3) 0.01406(14) Uani 1 1 d . . .
O1 O 0.22640(10) 0.86075(11) 0.22467(10) 0.0175(3) Uani 1 1 d . . .
O2 O 0.29396(10) 0.70227(12) 0.33644(11) 0.0234(3) Uani 1 1 d . . .
C7 C 0.23457(17) 1.21870(17) 0.07747(16) 0.0266(5) Uani 1 1 d . . .
H16 H 0.1944 1.2431 0.0097 0.040 Uiso 1 1 calc R . .
H17 H 0.2988 1.2530 0.0948 0.040 Uiso 1 1 calc R . .
H15 H 0.2041 1.2415 0.1270 0.040 Uiso 1 1 calc R . .
C6 C 0.24470(15) 1.09082(16) 0.07886(14) 0.0192(4) Uani 1 1 d . . .
C1 C 0.31163(14) 0.88546(16) 0.20480(14) 0.0155(4) Uani 1 1 d . . .
H2 H 0.3083 0.8530 0.1386 0.019 Uiso 1 1 calc R . .
H1 H 0.3674 0.8513 0.2577 0.019 Uiso 1 1 calc R . .
C15 C 0.10249(15) 0.73067(19) 0.25411(15) 0.0235(5) Uani 1 1 d . . .
H32 H 0.1008 0.7818 0.3100 0.028 Uiso 1 1 calc R . .
C16 C 0.02611(15) 0.77068(19) 0.15470(15) 0.0258(5) Uani 1 1 d . . .
H33 H 0.0362 0.8514 0.1464 0.031 Uiso 1 1 calc R . .
H34 H -0.0389 0.7618 0.1610 0.031 Uiso 1 1 calc R . .
C17 C 0.02735(16) 0.7097(2) 0.05879(16) 0.0292(5) Uani 1 1 d . . .
H36 H -0.0044 0.6362 0.0557 0.035 Uiso 1 1 calc R . .
H35 H -0.0114 0.7532 -0.0011 0.035 Uiso 1 1 calc R . .
C9 C 0.28087(17) 1.05512(18) -0.00829(15) 0.0255(5) Uani 1 1 d . . .
H18 H 0.2324 1.0753 -0.0733 0.038 Uiso 1 1 calc R . .
H20 H 0.2911 0.9742 -0.0057 0.038 Uiso 1 1 calc R . .
H19 H 0.3420 1.0932 -0.0013 0.038 Uiso 1 1 calc R . .
C14 C 0.30528(16) 0.74437(19) 0.42470(15) 0.0265(5) Uani 1 1 d . . .
H31 H 0.2548 0.7898 0.4319 0.032 Uiso 1 1 calc R . .
O3 O 0.37645(13) 0.72964(15) 0.49920(12) 0.0381(4) Uiso 1 1 d . . .
C19 C 0.20788(15) 0.65543(17) 0.15151(16) 0.0220(4) Uani 1 1 d . . .
H39 H 0.2724 0.6602 0.1417 0.026 Uiso 1 1 calc R . .
C18 C 0.12955(16) 0.69130(19) 0.05250(16) 0.0255(5) Uani 1 1 d . . .
H38 H 0.1252 0.6336 0.0005 0.031 Uiso 1 1 calc R . .
H37 H 0.1508 0.7616 0.0290 0.031 Uiso 1 1 calc R . .
C22 C 0.08647(17) 0.6101(2) 0.28405(18) 0.0332(6) Uani 1 1 d . . .
H44 H 0.1304 0.5964 0.3540 0.040 Uiso 1 1 calc R . .
H45 H 0.0192 0.6037 0.2847 0.040 Uiso 1 1 calc R . .
C21 C 0.10304(18) 0.5185(2) 0.2152(2) 0.0385(6) Uani 1 1 d . . .
H42 H 0.0456 0.5147 0.1530 0.046 Uiso 1 1 calc R . .
H43 H 0.1085 0.4458 0.2504 0.046 Uiso 1 1 calc R . .
C20 C 0.19408(17) 0.53546(18) 0.18448(19) 0.0318(5) Uani 1 1 d . . .
H41 H 0.1906 0.4840 0.1280 0.038 Uiso 1 1 calc R . .
H40 H 0.2518 0.5146 0.2425 0.038 Uiso 1 1 calc R . .
C10 C 0.46100(15) 1.05361(17) 0.21180(15) 0.0194(4) Uani 1 1 d . . .
C13 C 0.52895(16) 1.0312(2) 0.32099(16) 0.0292(5) Uani 1 1 d . . .
H30 H 0.5961 1.0277 0.3218 0.044 Uiso 1 1 calc R . .
H29 H 0.5114 0.9601 0.3450 0.044 Uiso 1 1 calc R . .
H28 H 0.5224 1.0917 0.3655 0.044 Uiso 1 1 calc R . .
C12 C 0.48866(16) 0.96639(18) 0.14477(16) 0.0235(5) Uani 1 1 d . . .
H25 H 0.4471 0.9759 0.0741 0.035 Uiso 1 1 calc R . .
H27 H 0.4799 0.8911 0.1678 0.035 Uiso 1 1 calc R . .
H26 H 0.5565 0.9768 0.1499 0.035 Uiso 1 1 calc R . .
C2 C 0.30539(16) 1.09990(18) 0.31446(15) 0.0224(5) Uani 1 1 d . . .
C3 C 0.34902(18) 1.0254(2) 0.40820(15) 0.0318(6) Uani 1 1 d . . .
H3 H 0.4197 1.0239 0.4262 0.048 Uiso 1 1 calc R . .
H4 H 0.3235 0.9494 0.3930 0.048 Uiso 1 1 calc R . .
H5 H 0.3317 1.0553 0.4651 0.048 Uiso 1 1 calc R . .
C4 C 0.19489(16) 1.1053(2) 0.29450(17) 0.0289(5) Uani 1 1 d . . .
H7 H 0.1830 1.1289 0.3564 0.043 Uiso 1 1 calc R . .
H6 H 0.1664 1.0314 0.2742 0.043 Uiso 1 1 calc R . .
H8 H 0.1653 1.1591 0.2402 0.043 Uiso 1 1 calc R . .
C5 C 0.34795(19) 1.2184(2) 0.33834(18) 0.0326(5) Uani 1 1 d . . .
H9 H 0.3305 1.2499 0.3946 0.049 Uiso 1 1 calc R . .
H10 H 0.3218 1.2659 0.2784 0.049 Uiso 1 1 calc R . .
H11 H 0.4186 1.2149 0.3572 0.049 Uiso 1 1 calc R . .
C8 C 0.14384(15) 1.03713(18) 0.05620(16) 0.0242(5) Uani 1 1 d . . .
H13 H 0.1152 1.0621 0.1067 0.036 Uiso 1 1 calc R . .
H12 H 0.1503 0.9556 0.0591 0.036 Uiso 1 1 calc R . .
H14 H 0.1019 1.0596 -0.0115 0.036 Uiso 1 1 calc R . .
B1 B 0.20757(17) 0.7401(2) 0.24127(17) 0.0199(5) Uani 1 1 d . . .
C11 C 0.48331(17) 1.17124(18) 0.18060(18) 0.0291(5) Uani 1 1 d . . .
H22 H 0.4661 1.2272 0.2228 0.044 Uiso 1 1 calc R . .
H23 H 0.4455 1.1843 0.1092 0.044 Uiso 1 1 calc R . .
H24 H 0.5525 1.1770 0.1899 0.044 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
P1 C1 1.8368(19) . ?
P1 C6 1.879(2) . ?
P1 C2 1.8818(19) . ?
P1 C10 1.884(2) . ?
O1 C1 1.397(2) . ?
O1 B1 1.503(3) . ?
O2 C14 1.292(3) . ?
O2 B1 1.568(3) . ?
C7 C6 1.538(3) . ?
C7 H16 0.9800 . ?
C7 H17 0.9800 . ?
C7 H15 0.9800 . ?
C6 C8 1.543(3) . ?
C6 C9 1.542(3) . ?
C1 H2 0.9900 . ?
C1 H1 0.9900 . ?
C15 C16 1.543(3) . ?
C15 C22 1.543(3) . ?
C15 B1 1.610(3) . ?
C15 H32 1.0000 . ?
C16 C17 1.533(3) . ?
C16 H33 0.9900 . ?
C16 H34 0.9900 . ?
C17 C18 1.543(3) . ?
C17 H36 0.9900 . ?
C17 H35 0.9900 . ?
C9 H18 0.9800 . ?
C9 H20 0.9800 . ?
C9 H19 0.9800 . ?
C14 O3 1.217(3) . ?
C14 H31 0.9500 . ?
C19 C18 1.537(3) . ?
C19 C20 1.543(3) . ?
C19 B1 1.615(3) . ?
C19 H39 1.0000 . ?
C18 H38 0.9900 . ?
C18 H37 0.9900 . ?
C22 C21 1.531(4) . ?
C22 H44 0.9900 . ?
C22 H45 0.9900 . ?
C21 C20 1.543(3) . ?
C21 H42 0.9900 . ?
C21 H43 0.9900 . ?
C20 H41 0.9900 . ?
C20 H40 0.9900 . ?
C10 C11 1.542(3) . ?
C10 C12 1.545(3) . ?
C10 C13 1.544(3) . ?
C13 H30 0.9800 . ?
C13 H29 0.9800 . ?
C13 H28 0.9800 . ?
C12 H25 0.9800 . ?
C12 H27 0.9800 . ?
C12 H26 0.9800 . ?
C2 C5 1.542(3) . ?
C2 C3 1.539(3) . ?
C2 C4 1.548(3) . ?
C3 H3 0.9800 . ?
C3 H4 0.9800 . ?
C3 H5 0.9800 . ?
C4 H7 0.9800 . ?
C4 H6 0.9800 . ?
C4 H8 0.9800 . ?
C5 H9 0.9800 . ?
C5 H10 0.9800 . ?
C5 H11 0.9800 . ?
C8 H13 0.9800 . ?
C8 H12 0.9800 . ?
C8 H14 0.9800 . ?
C11 H22 0.9800 . ?
C11 H23 0.9800 . ?
C11 H24 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 P1 C6 107.39(9) . . ?
C1 P1 C2 107.99(9) . . ?
C6 P1 C2 111.99(9) . . ?
C1 P1 C10 104.89(9) . . ?
C6 P1 C10 112.34(9) . . ?
C2 P1 C10 111.80(9) . . ?
C1 O1 B1 117.12(15) . . ?
C14 O2 B1 120.66(17) . . ?
C6 C7 H16 109.5 . . ?
C6 C7 H17 109.5 . . ?
H16 C7 H17 109.5 . . ?
C6 C7 H15 109.5 . . ?
H16 C7 H15 109.5 . . ?
H17 C7 H15 109.5 . . ?
C7 C6 C8 109.30(17) . . ?
C7 C6 C9 108.85(16) . . ?
C8 C6 C9 106.14(17) . . ?
C7 C6 P1 112.68(14) . . ?
C8 C6 P1 110.24(13) . . ?
C9 C6 P1 109.42(14) . . ?
O1 C1 P1 111.16(13) . . ?
O1 C1 H2 109.4 . . ?
P1 C1 H2 109.4 . . ?
O1 C1 H1 109.4 . . ?
P1 C1 H1 109.4 . . ?
H2 C1 H1 108.0 . . ?
C16 C15 C22 113.92(19) . . ?
C16 C15 B1 108.10(16) . . ?
C22 C15 B1 109.42(18) . . ?
C16 C15 H32 108.4 . . ?
C22 C15 H32 108.4 . . ?
B1 C15 H32 108.4 . . ?
C15 C16 C17 115.18(18) . . ?
C15 C16 H33 108.5 . . ?
C17 C16 H33 108.5 . . ?
C15 C16 H34 108.5 . . ?
C17 C16 H34 108.5 . . ?
H33 C16 H34 107.5 . . ?
C18 C17 C16 114.27(18) . . ?
C18 C17 H36 108.7 . . ?
C16 C17 H36 108.7 . . ?
C18 C17 H35 108.7 . . ?
C16 C17 H35 108.7 . . ?
H36 C17 H35 107.6 . . ?
C6 C9 H18 109.5 . . ?
C6 C9 H20 109.5 . . ?
H18 C9 H20 109.5 . . ?
C6 C9 H19 109.5 . . ?
H18 C9 H19 109.5 . . ?
H20 C9 H19 109.5 . . ?
O3 C14 O2 124.3(2) . . ?
O3 C14 H31 117.9 . . ?
O2 C14 H31 117.9 . . ?
C18 C19 C20 113.40(18) . . ?
C18 C19 B1 109.35(17) . . ?
C20 C19 B1 108.54(17) . . ?
C18 C19 H39 108.5 . . ?
C20 C19 H39 108.5 . . ?
B1 C19 H39 108.5 . . ?
C19 C18 C17 115.84(17) . . ?
C19 C18 H38 108.3 . . ?
C17 C18 H38 108.3 . . ?
C19 C18 H37 108.3 . . ?
C17 C18 H37 108.3 . . ?
H38 C18 H37 107.4 . . ?
C21 C22 C15 115.46(18) . . ?
C21 C22 H44 108.4 . . ?
C15 C22 H44 108.4 . . ?
C21 C22 H45 108.4 . . ?
C15 C22 H45 108.4 . . ?
H44 C22 H45 107.5 . . ?
C22 C21 C20 114.35(19) . . ?
C22 C21 H42 108.7 . . ?
C20 C21 H42 108.7 . . ?
C22 C21 H43 108.7 . . ?
C20 C21 H43 108.7 . . ?
H42 C21 H43 107.6 . . ?
C21 C20 C19 114.64(19) . . ?
C21 C20 H41 108.6 . . ?
C19 C20 H41 108.6 . . ?
C21 C20 H40 108.6 . . ?
C19 C20 H40 108.6 . . ?
H41 C20 H40 107.6 . . ?
C11 C10 C12 108.87(16) . . ?
C11 C10 C13 108.13(18) . . ?
C12 C10 C13 105.69(17) . . ?
C11 C10 P1 112.47(15) . . ?
C12 C10 P1 110.49(14) . . ?
C13 C10 P1 110.92(14) . . ?
C10 C13 H30 109.5 . . ?
C10 C13 H29 109.5 . . ?
H30 C13 H29 109.5 . . ?
C10 C13 H28 109.5 . . ?
H30 C13 H28 109.5 . . ?
H29 C13 H28 109.5 . . ?
C10 C12 H25 109.5 . . ?
C10 C12 H27 109.5 . . ?
H25 C12 H27 109.5 . . ?
C10 C12 H26 109.5 . . ?
H25 C12 H26 109.5 . . ?
H27 C12 H26 109.5 . . ?
C5 C2 C3 109.02(18) . . ?
C5 C2 C4 108.86(18) . . ?
C3 C2 C4 106.93(18) . . ?
C5 C2 P1 111.94(14) . . ?
C3 C2 P1 109.73(14) . . ?
C4 C2 P1 110.22(14) . . ?
C2 C3 H3 109.5 . . ?
C2 C3 H4 109.5 . . ?
H3 C3 H4 109.5 . . ?
C2 C3 H5 109.5 . . ?
H3 C3 H5 109.5 . . ?
H4 C3 H5 109.5 . . ?
C2 C4 H7 109.5 . . ?
C2 C4 H6 109.5 . . ?
H7 C4 H6 109.5 . . ?
C2 C4 H8 109.5 . . ?
H7 C4 H8 109.5 . . ?
H6 C4 H8 109.5 . . ?
C2 C5 H9 109.5 . . ?
C2 C5 H10 109.5 . . ?
H9 C5 H10 109.5 . . ?
C2 C5 H11 109.5 . . ?
H9 C5 H11 109.5 . . ?
H10 C5 H11 109.5 . . ?
C6 C8 H13 109.5 . . ?
C6 C8 H12 109.5 . . ?
H13 C8 H12 109.5 . . ?
C6 C8 H14 109.5 . . ?
H13 C8 H14 109.5 . . ?
H12 C8 H14 109.5 . . ?
O1 B1 O2 105.74(16) . . ?
O1 B1 C15 108.39(17) . . ?
O2 B1 C15 114.57(16) . . ?
O1 B1 C19 115.82(16) . . ?
O2 B1 C19 105.61(16) . . ?
C15 B1 C19 106.96(18) . . ?
C10 C11 H22 109.5 . . ?
C10 C11 H23 109.5 . . ?
H22 C11 H23 109.5 . . ?
C10 C11 H24 109.5 . . ?
H22 C11 H24 109.5 . . ?
H23 C11 H24 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 P1 C6 C7 165.96(14) . . . . ?
C2 P1 C6 C7 47.57(18) . . . . ?
C10 P1 C6 C7 -79.22(16) . . . . ?
C1 P1 C6 C8 43.56(16) . . . . ?
C2 P1 C6 C8 -74.83(16) . . . . ?
C10 P1 C6 C8 158.38(14) . . . . ?
C1 P1 C6 C9 -72.80(15) . . . . ?
C2 P1 C6 C9 168.81(13) . . . . ?
C10 P1 C6 C9 42.01(17) . . . . ?
B1 O1 C1 P1 -172.95(13) . . . . ?
C6 P1 C1 O1 -75.75(14) . . . . ?
C2 P1 C1 O1 45.20(15) . . . . ?
C10 P1 C1 O1 164.56(12) . . . . ?
C22 C15 C16 C17 -66.2(2) . . . . ?
B1 C15 C16 C17 55.7(2) . . . . ?
C15 C16 C17 C18 -44.0(3) . . . . ?
B1 O2 C14 O3 -170.6(2) . . . . ?
C20 C19 C18 C17 70.0(2) . . . . ?
B1 C19 C18 C17 -51.3(2) . . . . ?
C16 C17 C18 C19 41.7(3) . . . . ?
C16 C15 C22 C21 68.7(2) . . . . ?
B1 C15 C22 C21 -52.4(2) . . . . ?
C15 C22 C21 C20 43.2(3) . . . . ?
C22 C21 C20 C19 -44.8(3) . . . . ?
C18 C19 C20 C21 -66.5(3) . . . . ?
B1 C19 C20 C21 55.2(3) . . . . ?
C1 P1 C10 C11 163.59(14) . . . . ?
C6 P1 C10 C11 47.26(17) . . . . ?
C2 P1 C10 C11 -79.64(16) . . . . ?
C1 P1 C10 C12 41.70(16) . . . . ?
C6 P1 C10 C12 -74.62(16) . . . . ?
C2 P1 C10 C12 158.48(14) . . . . ?
C1 P1 C10 C13 -75.17(16) . . . . ?
C6 P1 C10 C13 168.50(14) . . . . ?
C2 P1 C10 C13 41.61(18) . . . . ?
C1 P1 C2 C5 162.60(15) . . . . ?
C6 P1 C2 C5 -79.36(17) . . . . ?
C10 P1 C2 C5 47.72(18) . . . . ?
C1 P1 C2 C3 41.42(18) . . . . ?
C6 P1 C2 C3 159.45(15) . . . . ?
C10 P1 C2 C3 -73.46(17) . . . . ?
C1 P1 C2 C4 -76.08(16) . . . . ?
C6 P1 C2 C4 41.95(18) . . . . ?
C10 P1 C2 C4 169.03(14) . . . . ?
C1 O1 B1 O2 61.00(19) . . . . ?
C1 O1 B1 C15 -175.70(15) . . . . ?
C1 O1 B1 C19 -55.5(2) . . . . ?
C14 O2 B1 O1 65.9(2) . . . . ?
C14 O2 B1 C15 -53.4(3) . . . . ?
C14 O2 B1 C19 -170.81(17) . . . . ?
C16 C15 B1 O1 62.2(2) . . . . ?
C22 C15 B1 O1 -173.22(17) . . . . ?
C16 C15 B1 O2 -179.99(17) . . . . ?
C22 C15 B1 O2 -55.4(2) . . . . ?
C16 C15 B1 C19 -63.3(2) . . . . ?
C22 C15 B1 C19 61.3(2) . . . . ?
C18 C19 B1 O1 -59.4(2) . . . . ?
C20 C19 B1 O1 176.38(17) . . . . ?
C18 C19 B1 O2 -176.06(16) . . . . ?
C20 C19 B1 O2 59.8(2) . . . . ?
C18 C19 B1 C15 61.5(2) . . . . ?
C20 C19 B1 C15 -62.7(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.65
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.056
_database_code_depnum_ccdc_archive 'CCDC 992442'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_tw021_0m

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H38 B O3 P'
_chemical_formula_weight         500.39

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   11.0787(7)
_cell_length_b                   11.8207(9)
_cell_length_c                   12.1674(8)
_cell_angle_alpha                69.226(4)
_cell_angle_beta                 68.012(4)
_cell_angle_gamma                80.563(4)
_cell_volume                     1380.57(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             536
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.9381
_exptl_absorpt_correction_T_max  0.9746
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23342
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.84
_diffrn_reflns_theta_max         27.78
_reflns_number_total             6396
_reflns_number_gt                5136
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.1000P)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         6396
_refine_ls_number_parameters     328
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0404
_refine_ls_wR_factor_ref         0.1455
_refine_ls_wR_factor_gt          0.1321
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.005
_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
P1 P 0.77431(3) 0.59522(3) 0.68717(3) 0.01862(12) Uani 1 1 d . . .
O1 O 0.56007(9) 0.71779(9) 0.76490(9) 0.0206(2) Uani 1 1 d . . .
O2 O 0.36660(9) 0.62969(9) 0.94106(9) 0.0228(2) Uani 1 1 d . . .
O3 O 0.28111(11) 0.47664(11) 0.93268(11) 0.0345(3) Uani 1 1 d . . .
C1 C 1.16563(18) 0.24355(17) 0.89465(19) 0.0410(5) Uani 1 1 d . . .
H20 H 1.1180 0.1817 0.9716 0.061 Uiso 1 1 calc R . .
H21 H 1.2194 0.2874 0.9133 0.061 Uiso 1 1 calc R . .
H1 H 1.2216 0.2047 0.8330 0.061 Uiso 1 1 calc R . .
C2 C 1.06968(14) 0.33148(14) 0.84219(14) 0.0258(3) Uani 1 1 d . . .
C3 C 1.03942(15) 0.44410(15) 0.86072(15) 0.0274(3) Uani 1 1 d . . .
H24 H 1.0802 0.4661 0.9060 0.033 Uiso 1 1 calc R . .
C4 C 0.95054(14) 0.52451(14) 0.81390(14) 0.0257(3) Uani 1 1 d . . .
H25 H 0.9307 0.6009 0.8273 0.031 Uiso 1 1 calc R . .
C5 C 0.89031(13) 0.49284(13) 0.74708(13) 0.0197(3) Uani 1 1 d . . .
C6 C 0.65065(13) 0.63952(14) 0.81377(13) 0.0208(3) Uani 1 1 d . . .
H18 H 0.6070 0.5672 0.8814 0.025 Uiso 1 1 calc R . .
H19 H 0.6906 0.6811 0.8488 0.025 Uiso 1 1 calc R . .
C7 C 0.35850(14) 0.85792(13) 0.79240(13) 0.0219(3) Uani 1 1 d . . .
H11 H 0.3368 0.8308 0.7331 0.026 Uiso 1 1 calc R . .
C8 C 0.44418(15) 0.96939(14) 0.71627(14) 0.0270(3) Uani 1 1 d . . .
H13 H 0.3901 1.0381 0.6819 0.032 Uiso 1 1 calc R . .
H12 H 0.5143 0.9514 0.6446 0.032 Uiso 1 1 calc R . .
C9 C 0.50735(16) 1.00953(14) 0.78973(15) 0.0282(3) Uani 1 1 d . . .
H2 H 0.5794 1.0634 0.7290 0.034 Uiso 1 1 calc R . .
H14 H 0.4417 1.0575 0.8382 0.034 Uiso 1 1 calc R . .
C10 C 1.04470(19) 1.05096(17) 0.28673(16) 0.0407(5) Uani 1 1 d . . .
H38 H 1.0877 1.0871 0.3230 0.061 Uiso 1 1 calc R . .
H3 H 0.9799 1.1091 0.2586 0.061 Uiso 1 1 calc R . .
H37 H 1.1098 1.0301 0.2153 0.061 Uiso 1 1 calc R . .
C11 C 0.97831(16) 0.93825(15) 0.38401(14) 0.0285(4) Uani 1 1 d . . .
C12 C 1.05034(15) 0.83854(16) 0.43349(15) 0.0299(4) Uani 1 1 d . . .
H36 H 1.1425 0.8419 0.4048 0.036 Uiso 1 1 calc R . .
C13 C 0.99059(14) 0.73446(15) 0.52364(14) 0.0259(3) Uani 1 1 d . . .
H35 H 1.0418 0.6679 0.5566 0.031 Uiso 1 1 calc R . .
C14 C 0.85497(14) 0.72716(13) 0.56628(13) 0.0206(3) Uani 1 1 d . . .
C15 C 0.32328(15) 0.57828(15) 0.88783(15) 0.0276(3) Uani 1 1 d . . .
H4 H 0.3239 0.6233 0.8056 0.033 Uiso 1 1 calc R . .
C16 C 0.47299(13) 0.79597(13) 0.95716(13) 0.0188(3) Uani 1 1 d . . .
H17 H 0.5226 0.7296 1.0024 0.023 Uiso 1 1 calc R . .
C17 C 0.56131(15) 0.90545(14) 0.88026(14) 0.0249(3) Uani 1 1 d . . .
H15 H 0.5761 0.9376 0.9389 0.030 Uiso 1 1 calc R . .
H16 H 0.6468 0.8771 0.8313 0.030 Uiso 1 1 calc R . .
C18 C 0.23043(14) 0.88302(14) 0.89044(14) 0.0266(3) Uani 1 1 d . . .
H9 H 0.1752 0.8120 0.9258 0.032 Uiso 1 1 calc R . .
H10 H 0.1835 0.9530 0.8479 0.032 Uiso 1 1 calc R . .
C19 C 0.24746(15) 0.90960(15) 0.99886(14) 0.0272(3) Uani 1 1 d . . .
H8 H 0.2782 0.9929 0.9682 0.033 Uiso 1 1 calc R . .
H7 H 0.1616 0.9061 1.0659 0.033 Uiso 1 1 calc R . .
C20 C 0.34368(14) 0.82134(14) 1.05459(13) 0.0236(3) Uani 1 1 d . . .
H6 H 0.3007 0.7436 1.1074 0.028 Uiso 1 1 calc R . .
H5 H 0.3638 0.8545 1.1097 0.028 Uiso 1 1 calc R . .
C21 C 1.00886(14) 0.30065(14) 0.77605(14) 0.0251(3) Uani 1 1 d . . .
H23 H 1.0286 0.2241 0.7631 0.030 Uiso 1 1 calc R . .
C22 C 0.91990(13) 0.37988(14) 0.72873(13) 0.0219(3) Uani 1 1 d . . .
H22 H 0.8790 0.3574 0.6838 0.026 Uiso 1 1 calc R . .
C23 C 0.70022(13) 0.51719(13) 0.62813(13) 0.0193(3) Uani 1 1 d . . .
C24 C 0.60092(14) 0.43776(14) 0.71178(13) 0.0229(3) Uani 1 1 d . . .
H32 H 0.5667 0.4325 0.7976 0.027 Uiso 1 1 calc R . .
C25 C 0.55257(15) 0.36694(14) 0.66988(14) 0.0260(3) Uani 1 1 d . . .
H31 H 0.4855 0.3128 0.7279 0.031 Uiso 1 1 calc R . .
C26 C 0.59965(15) 0.37277(14) 0.54457(14) 0.0243(3) Uani 1 1 d . . .
C27 C 0.69696(14) 0.45436(15) 0.46092(14) 0.0261(3) Uani 1 1 d . . .
H27 H 0.7295 0.4610 0.3748 0.031 Uiso 1 1 calc R . .
C28 C 0.74681(14) 0.52591(14) 0.50183(13) 0.0243(3) Uani 1 1 d . . .
H26 H 0.8129 0.5810 0.4437 0.029 Uiso 1 1 calc R . .
C29 C 0.54908(18) 0.29249(16) 0.50036(16) 0.0349(4) Uani 1 1 d . . .
H28 H 0.6136 0.2272 0.4854 0.052 Uiso 1 1 calc R . .
H29 H 0.5332 0.3403 0.4225 0.052 Uiso 1 1 calc R . .
H30 H 0.4675 0.2577 0.5644 0.052 Uiso 1 1 calc R . .
C30 C 0.78163(15) 0.82628(15) 0.51645(14) 0.0264(3) Uani 1 1 d . . .
H34 H 0.6896 0.8228 0.5441 0.032 Uiso 1 1 calc R . .
C31 C 0.84329(16) 0.92983(15) 0.42661(14) 0.0292(4) Uani 1 1 d . . .
H33 H 0.7924 0.9966 0.3933 0.035 Uiso 1 1 calc R . .
B1 B 0.44172(15) 0.74982(15) 0.86176(15) 0.0184(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C23 1.7889(15) . ?
P1 C5 1.7925(14) . ?
P1 C14 1.8000(15) . ?
P1 C6 1.8113(14) . ?
O1 C6 1.4031(16) . ?
O1 B1 1.4993(17) . ?
O2 C15 1.2755(18) . ?
O2 B1 1.5666(18) . ?
O3 C15 1.2197(19) . ?
C1 C2 1.514(2) . ?
C1 H20 0.9800 . ?
C1 H21 0.9800 . ?
C1 H1 0.9800 . ?
C2 C21 1.389(2) . ?
C2 C3 1.395(2) . ?
C3 C4 1.388(2) . ?
C3 H24 0.9500 . ?
C4 C5 1.397(2) . ?
C4 H25 0.9500 . ?
C5 C22 1.398(2) . ?
C6 H18 0.9900 . ?
C6 H19 0.9900 . ?
C7 C18 1.539(2) . ?
C7 C8 1.543(2) . ?
C7 B1 1.621(2) . ?
C7 H11 1.0000 . ?
C8 C9 1.547(2) . ?
C8 H13 0.9900 . ?
C8 H12 0.9900 . ?
C9 C17 1.541(2) . ?
C9 H2 0.9900 . ?
C9 H14 0.9900 . ?
C10 C11 1.506(2) . ?
C10 H38 0.9800 . ?
C10 H3 0.9800 . ?
C10 H37 0.9800 . ?
C11 C12 1.392(2) . ?
C11 C31 1.396(2) . ?
C12 C13 1.386(2) . ?
C12 H36 0.9500 . ?
C13 C14 1.400(2) . ?
C13 H35 0.9500 . ?
C14 C30 1.398(2) . ?
C15 H4 0.9500 . ?
C16 C17 1.542(2) . ?
C16 C20 1.5450(19) . ?
C16 B1 1.606(2) . ?
C16 H17 1.0000 . ?
C17 H15 0.9900 . ?
C17 H16 0.9900 . ?
C18 C19 1.541(2) . ?
C18 H9 0.9900 . ?
C18 H10 0.9900 . ?
C19 C20 1.536(2) . ?
C19 H8 0.9900 . ?
C19 H7 0.9900 . ?
C20 H6 0.9900 . ?
C20 H5 0.9900 . ?
C21 C22 1.386(2) . ?
C21 H23 0.9500 . ?
C22 H22 0.9500 . ?
C23 C28 1.396(2) . ?
C23 C24 1.396(2) . ?
C24 C25 1.379(2) . ?
C24 H32 0.9500 . ?
C25 C26 1.394(2) . ?
C25 H31 0.9500 . ?
C26 C27 1.397(2) . ?
C26 C29 1.505(2) . ?
C27 C28 1.388(2) . ?
C27 H27 0.9500 . ?
C28 H26 0.9500 . ?
C29 H28 0.9800 . ?
C29 H29 0.9800 . ?
C29 H30 0.9800 . ?
C30 C31 1.388(2) . ?
C30 H34 0.9500 . ?
C31 H33 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
C23 P1 C5 108.05(7) . . ?
C23 P1 C14 111.21(7) . . ?
C5 P1 C14 109.73(7) . . ?
C23 P1 C6 109.29(7) . . ?
C5 P1 C6 108.83(6) . . ?
C14 P1 C6 109.68(7) . . ?
C6 O1 B1 114.13(10) . . ?
C15 O2 B1 119.33(11) . . ?
C2 C1 H20 109.5 . . ?
C2 C1 H21 109.5 . . ?
H20 C1 H21 109.5 . . ?
C2 C1 H1 109.5 . . ?
H20 C1 H1 109.5 . . ?
H21 C1 H1 109.5 . . ?
C21 C2 C3 118.78(14) . . ?
C21 C2 C1 120.48(15) . . ?
C3 C2 C1 120.73(15) . . ?
C4 C3 C2 120.94(15) . . ?
C4 C3 H24 119.5 . . ?
C2 C3 H24 119.5 . . ?
C3 C4 C5 119.84(14) . . ?
C3 C4 H25 120.1 . . ?
C5 C4 H25 120.1 . . ?
C4 C5 C22 119.44(13) . . ?
C4 C5 P1 120.35(11) . . ?
C22 C5 P1 120.21(11) . . ?
O1 C6 P1 107.65(9) . . ?
O1 C6 H18 110.2 . . ?
P1 C6 H18 110.2 . . ?
O1 C6 H19 110.2 . . ?
P1 C6 H19 110.2 . . ?
H18 C6 H19 108.5 . . ?
C18 C7 C8 113.44(12) . . ?
C18 C7 B1 109.35(11) . . ?
C8 C7 B1 108.55(12) . . ?
C18 C7 H11 108.5 . . ?
C8 C7 H11 108.5 . . ?
B1 C7 H11 108.5 . . ?
C7 C8 C9 115.40(12) . . ?
C7 C8 H13 108.4 . . ?
C9 C8 H13 108.4 . . ?
C7 C8 H12 108.4 . . ?
C9 C8 H12 108.4 . . ?
H13 C8 H12 107.5 . . ?
C17 C9 C8 115.03(13) . . ?
C17 C9 H2 108.5 . . ?
C8 C9 H2 108.5 . . ?
C17 C9 H14 108.5 . . ?
C8 C9 H14 108.5 . . ?
H2 C9 H14 107.5 . . ?
C11 C10 H38 109.5 . . ?
C11 C10 H3 109.5 . . ?
H38 C10 H3 109.5 . . ?
C11 C10 H37 109.5 . . ?
H38 C10 H37 109.5 . . ?
H3 C10 H37 109.5 . . ?
C12 C11 C31 117.89(14) . . ?
C12 C11 C10 120.78(15) . . ?
C31 C11 C10 121.33(16) . . ?
C13 C12 C11 121.45(15) . . ?
C13 C12 H36 119.3 . . ?
C11 C12 H36 119.3 . . ?
C12 C13 C14 120.21(14) . . ?
C12 C13 H35 119.9 . . ?
C14 C13 H35 119.9 . . ?
C30 C14 C13 118.88(14) . . ?
C30 C14 P1 119.92(11) . . ?
C13 C14 P1 121.16(11) . . ?
O3 C15 O2 126.05(15) . . ?
O3 C15 H4 117.0 . . ?
O2 C15 H4 117.0 . . ?
C17 C16 C20 114.77(12) . . ?
C17 C16 B1 108.25(11) . . ?
C20 C16 B1 109.21(12) . . ?
C17 C16 H17 108.1 . . ?
C20 C16 H17 108.1 . . ?
B1 C16 H17 108.1 . . ?
C9 C17 C16 114.90(12) . . ?
C9 C17 H15 108.5 . . ?
C16 C17 H15 108.5 . . ?
C9 C17 H16 108.5 . . ?
C16 C17 H16 108.5 . . ?
H15 C17 H16 107.5 . . ?
C7 C18 C19 114.68(12) . . ?
C7 C18 H9 108.6 . . ?
C19 C18 H9 108.6 . . ?
C7 C18 H10 108.6 . . ?
C19 C18 H10 108.6 . . ?
H9 C18 H10 107.6 . . ?
C20 C19 C18 113.73(12) . . ?
C20 C19 H8 108.8 . . ?
C18 C19 H8 108.8 . . ?
C20 C19 H7 108.8 . . ?
C18 C19 H7 108.8 . . ?
H8 C19 H7 107.7 . . ?
C19 C20 C16 114.81(12) . . ?
C19 C20 H6 108.6 . . ?
C16 C20 H6 108.6 . . ?
C19 C20 H5 108.6 . . ?
C16 C20 H5 108.6 . . ?
H6 C20 H5 107.5 . . ?
C22 C21 C2 120.99(14) . . ?
C22 C21 H23 119.5 . . ?
C2 C21 H23 119.5 . . ?
C21 C22 C5 120.01(14) . . ?
C21 C22 H22 120.0 . . ?
C5 C22 H22 120.0 . . ?
C28 C23 C24 119.09(14) . . ?
C28 C23 P1 121.45(11) . . ?
C24 C23 P1 119.23(11) . . ?
C25 C24 C23 120.01(13) . . ?
C25 C24 H32 120.0 . . ?
C23 C24 H32 120.0 . . ?
C24 C25 C26 121.66(14) . . ?
C24 C25 H31 119.2 . . ?
C26 C25 H31 119.2 . . ?
C25 C26 C27 118.02(14) . . ?
C25 C26 C29 121.29(14) . . ?
C27 C26 C29 120.69(14) . . ?
C28 C27 C26 120.94(14) . . ?
C28 C27 H27 119.5 . . ?
C26 C27 H27 119.5 . . ?
C27 C28 C23 120.25(14) . . ?
C27 C28 H26 119.9 . . ?
C23 C28 H26 119.9 . . ?
C26 C29 H28 109.5 . . ?
C26 C29 H29 109.5 . . ?
H28 C29 H29 109.5 . . ?
C26 C29 H30 109.5 . . ?
H28 C29 H30 109.5 . . ?
H29 C29 H30 109.5 . . ?
C31 C30 C14 120.01(14) . . ?
C31 C30 H34 120.0 . . ?
C14 C30 H34 120.0 . . ?
C30 C31 C11 121.55(15) . . ?
C30 C31 H33 119.2 . . ?
C11 C31 H33 119.2 . . ?
O1 B1 O2 105.80(11) . . ?
O1 B1 C16 114.32(12) . . ?
O2 B1 C16 106.93(11) . . ?
O1 B1 C7 109.08(11) . . ?
O2 B1 C7 113.91(11) . . ?
C16 B1 C7 106.97(12) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C21 C2 C3 C4 -0.2(2) . . . . ?
C1 C2 C3 C4 -179.34(15) . . . . ?
C2 C3 C4 C5 -0.1(2) . . . . ?
C3 C4 C5 C22 0.3(2) . . . . ?
C3 C4 C5 P1 179.48(11) . . . . ?
C23 P1 C5 C4 -171.58(11) . . . . ?
C14 P1 C5 C4 67.02(13) . . . . ?
C6 P1 C5 C4 -53.01(14) . . . . ?
C23 P1 C5 C22 7.55(13) . . . . ?
C14 P1 C5 C22 -113.86(12) . . . . ?
C6 P1 C5 C22 126.12(12) . . . . ?
B1 O1 C6 P1 172.35(10) . . . . ?
C23 P1 C6 O1 -61.20(11) . . . . ?
C5 P1 C6 O1 -178.99(9) . . . . ?
C14 P1 C6 O1 60.96(11) . . . . ?
C18 C7 C8 C9 69.95(16) . . . . ?
B1 C7 C8 C9 -51.82(17) . . . . ?
C7 C8 C9 C17 41.19(18) . . . . ?
C31 C11 C12 C13 -1.0(2) . . . . ?
C10 C11 C12 C13 179.59(15) . . . . ?
C11 C12 C13 C14 0.6(2) . . . . ?
C12 C13 C14 C30 0.0(2) . . . . ?
C12 C13 C14 P1 -177.80(12) . . . . ?
C23 P1 C14 C30 68.42(13) . . . . ?
C5 P1 C14 C30 -172.09(12) . . . . ?
C6 P1 C14 C30 -52.59(14) . . . . ?
C23 P1 C14 C13 -113.82(13) . . . . ?
C5 P1 C14 C13 5.67(14) . . . . ?
C6 P1 C14 C13 125.17(12) . . . . ?
B1 O2 C15 O3 168.23(14) . . . . ?
C8 C9 C17 C16 -42.43(18) . . . . ?
C20 C16 C17 C9 -67.62(16) . . . . ?
B1 C16 C17 C9 54.63(16) . . . . ?
C8 C7 C18 C19 -67.06(16) . . . . ?
B1 C7 C18 C19 54.26(17) . . . . ?
C7 C18 C19 C20 -45.86(18) . . . . ?
C18 C19 C20 C16 46.03(19) . . . . ?
C17 C16 C20 C19 66.87(17) . . . . ?
B1 C16 C20 C19 -54.86(17) . . . . ?
C3 C2 C21 C22 0.2(2) . . . . ?
C1 C2 C21 C22 179.33(15) . . . . ?
C2 C21 C22 C5 0.1(2) . . . . ?
C4 C5 C22 C21 -0.4(2) . . . . ?
P1 C5 C22 C21 -179.49(11) . . . . ?
C5 P1 C23 C28 -94.80(13) . . . . ?
C14 P1 C23 C28 25.68(14) . . . . ?
C6 P1 C23 C28 146.92(12) . . . . ?
C5 P1 C23 C24 79.64(12) . . . . ?
C14 P1 C23 C24 -159.88(11) . . . . ?
C6 P1 C23 C24 -38.64(13) . . . . ?
C28 C23 C24 C25 1.7(2) . . . . ?
P1 C23 C24 C25 -172.88(11) . . . . ?
C23 C24 C25 C26 -0.5(2) . . . . ?
C24 C25 C26 C27 -0.9(2) . . . . ?
C24 C25 C26 C29 178.17(14) . . . . ?
C25 C26 C27 C28 1.1(2) . . . . ?
C29 C26 C27 C28 -177.98(14) . . . . ?
C26 C27 C28 C23 0.1(2) . . . . ?
C24 C23 C28 C27 -1.5(2) . . . . ?
P1 C23 C28 C27 172.95(11) . . . . ?
C13 C14 C30 C31 -0.2(2) . . . . ?
P1 C14 C30 C31 177.57(12) . . . . ?
C14 C30 C31 C11 -0.1(2) . . . . ?
C12 C11 C31 C30 0.7(2) . . . . ?
C10 C11 C31 C30 -179.85(15) . . . . ?
C6 O1 B1 O2 -67.10(14) . . . . ?
C6 O1 B1 C16 50.28(16) . . . . ?
C6 O1 B1 C7 169.97(12) . . . . ?
C15 O2 B1 O1 -62.01(15) . . . . ?
C15 O2 B1 C16 175.75(12) . . . . ?
C15 O2 B1 C7 57.80(16) . . . . ?
C17 C16 B1 O1 56.48(15) . . . . ?
C20 C16 B1 O1 -177.93(11) . . . . ?
C17 C16 B1 O2 173.21(10) . . . . ?
C20 C16 B1 O2 -61.20(14) . . . . ?
C17 C16 B1 C7 -64.39(14) . . . . ?
C20 C16 B1 C7 61.20(14) . . . . ?
C18 C7 B1 O1 174.68(12) . . . . ?
C8 C7 B1 O1 -61.08(15) . . . . ?
C18 C7 B1 O2 56.74(16) . . . . ?
C8 C7 B1 O2 -179.02(11) . . . . ?
C18 C7 B1 C16 -61.18(15) . . . . ?
C8 C7 B1 C16 63.05(14) . . . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        27.78
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.047

#===end
_database_code_depnum_ccdc_archive 'CCDC 992443'
