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

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#
#                 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.
# 
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
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#  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_1b

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H42 N P Si'
_chemical_formula_sum            'C21 H42 N P Si'
_chemical_formula_weight         367.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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   P21/n
_symmetry_space_group_name_Hall  '-P 2yn'

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                   11.3679(6)
_cell_length_b                   17.4007(10)
_cell_length_c                   11.4194(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.718(2)
_cell_angle_gamma                90.00
_cell_volume                     2258.7(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9839
_cell_measurement_theta_min      5.088
_cell_measurement_theta_max      55.040

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             816
_exptl_absorpt_coefficient_mu    0.178
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7026
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
'SADABS. Area-Detector Integration Software. (Siemens Industrial Automation, 1995, Inc.: Madison, WI)'

_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  'Bruker Apex II CCD 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            20105
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         27.54
_reflns_number_total             5193
_reflns_number_gt                4055
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'Bruker SMART. Area-Detector Software Package. (Siemens Industrial Automation, 1993, Inc.: Madison, WI)'
_computing_cell_refinement       
'Bruker SMART. Area-Detector Software Package. (Siemens Industrial Automation, 1993, Inc.: Madison, WI)'
_computing_data_reduction        
'Bruker SAINT. Area-Detector Integration Software. (Siemens Industrial Automation, 1995, Inc.: Madison, WI)'
_computing_structure_solution    
'SHELX-97. Programs for Crystal Structure Analysis. (G. M. Sheldrick, 1997, Release 97-2, University of Gttingen, Germany)'
_computing_structure_refinement  
'SHELX-97. Programs for Crystal Structure Analysis. (G. M. Sheldrick, 1997, Release 97-2, University of Gttingen, Germany)'
_computing_molecular_graphics    
'Ortep for Windows (L. J. Farrugia, J. Appl. Cryst. 1997, 30, 565)'
_computing_publication_material  
'WinGX v1.70.01 (L. J. Farrugia, J. Appl. Cryst. 1999, 32, 837)'

_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)+(0.0407P)²+0.8643P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5193
_refine_ls_number_parameters     220
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0381
_refine_ls_wR_factor_ref         0.0960
_refine_ls_wR_factor_gt          0.0871
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.009
_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 0.24631(3) 0.13271(2) 0.02437(3) 0.01681(10) Uani 1 1 d . . .
Si1 Si 0.45901(4) 0.23663(2) -0.02927(4) 0.02173(11) Uani 1 1 d . . .
N1 N 0.36427(11) 0.17665(7) 0.03299(11) 0.0230(3) Uani 1 1 d . . .
C13 C 0.21991(16) -0.03243(10) 0.35101(15) 0.0353(4) Uani 1 1 d . . .
H13A H 0.1994 -0.0494 0.4310 0.042 Uiso 1 1 calc R . .
H13B H 0.2638 -0.0745 0.3129 0.042 Uiso 1 1 calc R . .
C14 C 0.29665(16) 0.03879(11) 0.35823(14) 0.0334(4) Uani 1 1 d . . .
H14A H 0.3706 0.0262 0.4008 0.040 Uiso 1 1 calc R . .
H14B H 0.2553 0.0790 0.4031 0.040 Uiso 1 1 calc R . .
C15 C 0.32598(14) 0.06985(10) 0.23686(13) 0.0264(4) Uani 1 1 d . . .
H15A H 0.3743 0.0317 0.1947 0.032 Uiso 1 1 calc R . .
H15B H 0.3726 0.1176 0.2452 0.032 Uiso 1 1 calc R . .
C10 C 0.21365(13) 0.08656(8) 0.16550(12) 0.0194(3) Uani 1 1 d . . .
H10 H 0.1684 0.1252 0.2116 0.023 Uiso 1 1 calc R . .
C4 C 0.24207(12) 0.05744(8) -0.08833(12) 0.0190(3) Uani 1 1 d . . .
H4 H 0.1683 0.0269 -0.0784 0.023 Uiso 1 1 calc R . .
C9 C 0.34749(13) 0.00300(9) -0.07346(13) 0.0236(3) Uani 1 1 d . . .
H9A H 0.4213 0.0329 -0.0784 0.028 Uiso 1 1 calc R . .
H9B H 0.3450 -0.0211 0.0050 0.028 Uiso 1 1 calc R . .
C8 C 0.34734(15) -0.05958(9) -0.16661(14) 0.0292(4) Uani 1 1 d . . .
H8A H 0.4182 -0.0921 -0.1564 0.035 Uiso 1 1 calc R . .
H8B H 0.2773 -0.0927 -0.1570 0.035 Uiso 1 1 calc R . .
C7 C 0.34601(15) -0.02513(10) -0.28875(14) 0.0327(4) Uani 1 1 d . . .
H7A H 0.3412 -0.0669 -0.3475 0.039 Uiso 1 1 calc R . .
H7B H 0.4202 0.0033 -0.3013 0.039 Uiso 1 1 calc R . .
C19 C -0.10085(17) 0.27947(11) 0.0233(2) 0.0492(6) Uani 1 1 d . . .
H19A H -0.1608 0.3162 -0.0063 0.059 Uiso 1 1 calc R . .
H19B H -0.1253 0.2618 0.1018 0.059 Uiso 1 1 calc R . .
C20 C 0.01663(17) 0.31950(10) 0.03333(17) 0.0421(5) Uani 1 1 d . . .
H20A H 0.0111 0.3620 0.0907 0.051 Uiso 1 1 calc R . .
H20B H 0.0370 0.3420 -0.0435 0.051 Uiso 1 1 calc R . .
C21 C 0.11369(16) 0.26384(10) 0.07228(16) 0.0344(4) Uani 1 1 d . . .
H21A H 0.1902 0.2910 0.0736 0.041 Uiso 1 1 calc R . .
H21B H 0.0978 0.2456 0.1527 0.041 Uiso 1 1 calc R . .
C16 C 0.12036(12) 0.19493(8) -0.01050(13) 0.0207(3) Uani 1 1 d . . .
H16 H 0.1355 0.2166 -0.0900 0.025 Uiso 1 1 calc R . .
C12 C 0.10793(15) -0.01551(10) 0.28115(15) 0.0324(4) Uani 1 1 d . . .
H12A H 0.0608 0.0233 0.3231 0.039 Uiso 1 1 calc R . .
H12B H 0.0603 -0.0630 0.2743 0.039 Uiso 1 1 calc R . .
C11 C 0.13629(14) 0.01428(9) 0.15895(14) 0.0256(3) Uani 1 1 d . . .
H11A H 0.0622 0.0264 0.1165 0.031 Uiso 1 1 calc R . .
H11B H 0.1777 -0.0262 0.1147 0.031 Uiso 1 1 calc R . .
C1 C 0.57110(14) 0.18385(10) -0.11653(15) 0.0313(4) Uani 1 1 d . . .
H1A H 0.6109 0.1459 -0.0665 0.047 Uiso 1 1 calc R . .
H1B H 0.6291 0.2204 -0.1465 0.047 Uiso 1 1 calc R . .
H1C H 0.5322 0.1576 -0.1823 0.047 Uiso 1 1 calc R . .
C2 C 0.54096(18) 0.29027(12) 0.08728(18) 0.0454(5) Uani 1 1 d . . .
H2A H 0.4850 0.3175 0.1370 0.068 Uiso 1 1 calc R . .
H2B H 0.5941 0.3274 0.0510 0.068 Uiso 1 1 calc R . .
H2C H 0.5868 0.2540 0.1351 0.068 Uiso 1 1 calc R . .
C3 C 0.38754(17) 0.30895(11) -0.12902(17) 0.0409(5) Uani 1 1 d . . .
H3A H 0.3425 0.2822 -0.1903 0.061 Uiso 1 1 calc R . .
H3B H 0.4482 0.3408 -0.1651 0.061 Uiso 1 1 calc R . .
H3C H 0.3346 0.3416 -0.0838 0.061 Uiso 1 1 calc R . .
C5 C 0.24101(14) 0.09172(9) -0.21214(13) 0.0250(3) Uani 1 1 d . . .
H5A H 0.1698 0.1238 -0.2229 0.030 Uiso 1 1 calc R . .
H5B H 0.3107 0.1252 -0.2214 0.030 Uiso 1 1 calc R . .
C6 C 0.24230(15) 0.02902(10) -0.30571(14) 0.0319(4) Uani 1 1 d . . .
H6A H 0.1682 -0.0007 -0.3024 0.038 Uiso 1 1 calc R . .
H6B H 0.2466 0.0531 -0.3841 0.038 Uiso 1 1 calc R . .
C17 C 0.00123(14) 0.15518(10) -0.01905(17) 0.0336(4) Uani 1 1 d . . .
H17A H -0.0191 0.1336 0.0583 0.040 Uiso 1 1 calc R . .
H17B H 0.0057 0.1121 -0.0755 0.040 Uiso 1 1 calc R . .
C18 C -0.09460(16) 0.21120(12) -0.0586(2) 0.0501(5) Uani 1 1 d . . .
H18A H -0.0779 0.2293 -0.1389 0.060 Uiso 1 1 calc R . .
H18B H -0.1715 0.1845 -0.0605 0.060 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 N1 1.5457(12) . ?
P1 C16 1.8348(15) . ?
P1 C4 1.8365(14) . ?
P1 C10 1.8425(14) . ?
Si1 N1 1.6655(13) . ?
Si1 C2 1.8653(18) . ?
Si1 C1 1.8686(16) . ?
Si1 C3 1.8757(18) . ?
C13 C14 1.517(2) . ?
C13 C12 1.523(2) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.528(2) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C10 1.534(2) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C10 C11 1.536(2) . ?
C10 H10 1.0000 . ?
C4 C5 1.534(2) . ?
C4 C9 1.535(2) . ?
C4 H4 1.0000 . ?
C9 C8 1.522(2) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C8 C7 1.518(2) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C7 C6 1.520(2) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C19 C20 1.509(3) . ?
C19 C18 1.515(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.530(2) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C16 1.529(2) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C16 C17 1.523(2) . ?
C16 H16 1.0000 . ?
C12 C11 1.527(2) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C5 C6 1.527(2) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C17 C18 1.526(2) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 P1 C16 113.32(7) . . ?
N1 P1 C4 114.36(7) . . ?
C16 P1 C4 104.79(7) . . ?
N1 P1 C10 110.12(7) . . ?
C16 P1 C10 106.37(7) . . ?
C4 P1 C10 107.36(7) . . ?
N1 Si1 C2 109.20(8) . . ?
N1 Si1 C1 111.63(7) . . ?
C2 Si1 C1 106.77(9) . . ?
N1 Si1 C3 113.71(8) . . ?
C2 Si1 C3 107.83(10) . . ?
C1 Si1 C3 107.39(8) . . ?
P1 N1 Si1 147.99(9) . . ?
C14 C13 C12 110.30(14) . . ?
C14 C13 H13A 109.6 . . ?
C12 C13 H13A 109.6 . . ?
C14 C13 H13B 109.6 . . ?
C12 C13 H13B 109.6 . . ?
H13A C13 H13B 108.1 . . ?
C13 C14 C15 111.80(13) . . ?
C13 C14 H14A 109.3 . . ?
C15 C14 H14A 109.3 . . ?
C13 C14 H14B 109.3 . . ?
C15 C14 H14B 109.3 . . ?
H14A C14 H14B 107.9 . . ?
C14 C15 C10 111.05(13) . . ?
C14 C15 H15A 109.4 . . ?
C10 C15 H15A 109.4 . . ?
C14 C15 H15B 109.4 . . ?
C10 C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
C15 C10 C11 110.06(12) . . ?
C15 C10 P1 111.83(10) . . ?
C11 C10 P1 115.84(10) . . ?
C15 C10 H10 106.1 . . ?
C11 C10 H10 106.1 . . ?
P1 C10 H10 106.1 . . ?
C5 C4 C9 109.80(12) . . ?
C5 C4 P1 111.61(10) . . ?
C9 C4 P1 110.42(10) . . ?
C5 C4 H4 108.3 . . ?
C9 C4 H4 108.3 . . ?
P1 C4 H4 108.3 . . ?
C8 C9 C4 111.72(12) . . ?
C8 C9 H9A 109.3 . . ?
C4 C9 H9A 109.3 . . ?
C8 C9 H9B 109.3 . . ?
C4 C9 H9B 109.3 . . ?
H9A C9 H9B 107.9 . . ?
C7 C8 C9 111.06(13) . . ?
C7 C8 H8A 109.4 . . ?
C9 C8 H8A 109.4 . . ?
C7 C8 H8B 109.4 . . ?
C9 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
C8 C7 C6 111.15(13) . . ?
C8 C7 H7A 109.4 . . ?
C6 C7 H7A 109.4 . . ?
C8 C7 H7B 109.4 . . ?
C6 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
C20 C19 C18 111.13(15) . . ?
C20 C19 H19A 109.4 . . ?
C18 C19 H19A 109.4 . . ?
C20 C19 H19B 109.4 . . ?
C18 C19 H19B 109.4 . . ?
H19A C19 H19B 108.0 . . ?
C19 C20 C21 111.34(15) . . ?
C19 C20 H20A 109.4 . . ?
C21 C20 H20A 109.4 . . ?
C19 C20 H20B 109.4 . . ?
C21 C20 H20B 109.4 . . ?
H20A C20 H20B 108.0 . . ?
C16 C21 C20 110.97(14) . . ?
C16 C21 H21A 109.4 . . ?
C20 C21 H21A 109.4 . . ?
C16 C21 H21B 109.4 . . ?
C20 C21 H21B 109.4 . . ?
H21A C21 H21B 108.0 . . ?
C17 C16 C21 110.17(13) . . ?
C17 C16 P1 115.90(11) . . ?
C21 C16 P1 111.91(11) . . ?
C17 C16 H16 106.0 . . ?
C21 C16 H16 106.0 . . ?
P1 C16 H16 106.0 . . ?
C13 C12 C11 111.09(13) . . ?
C13 C12 H12A 109.4 . . ?
C11 C12 H12A 109.4 . . ?
C13 C12 H12B 109.4 . . ?
C11 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
C12 C11 C10 111.15(13) . . ?
C12 C11 H11A 109.4 . . ?
C10 C11 H11A 109.4 . . ?
C12 C11 H11B 109.4 . . ?
C10 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
Si1 C1 H1A 109.5 . . ?
Si1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Si1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C6 C5 C4 111.53(13) . . ?
C6 C5 H5A 109.3 . . ?
C4 C5 H5A 109.3 . . ?
C6 C5 H5B 109.3 . . ?
C4 C5 H5B 109.3 . . ?
H5A C5 H5B 108.0 . . ?
C7 C6 C5 111.59(13) . . ?
C7 C6 H6A 109.3 . . ?
C5 C6 H6A 109.3 . . ?
C7 C6 H6B 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 108.0 . . ?
C16 C17 C18 111.09(14) . . ?
C16 C17 H17A 109.4 . . ?
C18 C17 H17A 109.4 . . ?
C16 C17 H17B 109.4 . . ?
C18 C17 H17B 109.4 . . ?
H17A C17 H17B 108.0 . . ?
C19 C18 C17 110.90(17) . . ?
C19 C18 H18A 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 108.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C16 P1 N1 Si1 -53.27(18) . . . . ?
C4 P1 N1 Si1 66.75(18) . . . . ?
C10 P1 N1 Si1 -172.27(15) . . . . ?
C2 Si1 N1 P1 151.33(16) . . . . ?
C1 Si1 N1 P1 -90.84(17) . . . . ?
C3 Si1 N1 P1 30.86(19) . . . . ?
C12 C13 C14 C15 -56.39(19) . . . . ?
C13 C14 C15 C10 56.23(19) . . . . ?
C14 C15 C10 C11 -55.24(17) . . . . ?
C14 C15 C10 P1 174.52(11) . . . . ?
N1 P1 C10 C15 -25.96(13) . . . . ?
C16 P1 C10 C15 -149.13(11) . . . . ?
C4 P1 C10 C15 99.12(11) . . . . ?
N1 P1 C10 C11 -153.14(11) . . . . ?
C16 P1 C10 C11 83.69(12) . . . . ?
C4 P1 C10 C11 -28.06(13) . . . . ?
N1 P1 C4 C5 -70.06(12) . . . . ?
C16 P1 C4 C5 54.62(12) . . . . ?
C10 P1 C4 C5 167.44(10) . . . . ?
N1 P1 C4 C9 52.37(12) . . . . ?
C16 P1 C4 C9 177.05(10) . . . . ?
C10 P1 C4 C9 -70.12(11) . . . . ?
C5 C4 C9 C8 -55.82(17) . . . . ?
P1 C4 C9 C8 -179.31(11) . . . . ?
C4 C9 C8 C7 56.62(18) . . . . ?
C9 C8 C7 C6 -55.74(18) . . . . ?
C18 C19 C20 C21 -55.9(2) . . . . ?
C19 C20 C21 C16 55.9(2) . . . . ?
C20 C21 C16 C17 -55.86(18) . . . . ?
C20 C21 C16 P1 173.66(12) . . . . ?
N1 P1 C16 C17 -179.42(11) . . . . ?
C4 P1 C16 C17 55.24(13) . . . . ?
C10 P1 C16 C17 -58.28(13) . . . . ?
N1 P1 C16 C21 -51.95(13) . . . . ?
C4 P1 C16 C21 -177.29(11) . . . . ?
C10 P1 C16 C21 69.19(12) . . . . ?
C14 C13 C12 C11 56.71(19) . . . . ?
C13 C12 C11 C10 -57.19(18) . . . . ?
C15 C10 C11 C12 56.01(17) . . . . ?
P1 C10 C11 C12 -175.92(11) . . . . ?
C9 C4 C5 C6 55.00(17) . . . . ?
P1 C4 C5 C6 177.79(11) . . . . ?
C8 C7 C6 C5 55.33(19) . . . . ?
C4 C5 C6 C7 -55.45(18) . . . . ?
C21 C16 C17 C18 56.6(2) . . . . ?
P1 C16 C17 C18 -175.10(13) . . . . ?
C20 C19 C18 C17 56.3(2) . . . . ?
C16 C17 C18 C19 -56.9(2) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.54
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.046
_database_code_depnum_ccdc_archive 'CCDC 1018460'
#######################################################################
#
#                 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_1d

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H24 N P Si'
_chemical_formula_sum            'C21 H24 N P Si'
_chemical_formula_weight         349.47

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'


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

_cell_length_a                   8.7098(7)
_cell_length_b                   11.0404(11)
_cell_length_c                   11.3544(11)
_cell_angle_alpha                62.456(5)
_cell_angle_beta                 88.191(6)
_cell_angle_gamma                87.019(6)
_cell_volume                     966.74(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4233
_cell_measurement_theta_min      4.683
_cell_measurement_theta_max      56.368

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             372
_exptl_absorpt_coefficient_mu    0.206
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6908
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   
'SADABS. Area-Detector Integration Software. (Siemens Industrial Automation, 1995, Inc.: Madison, WI)'

_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  'Bruker Apex II CCD 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            13299
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.0735
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.02
_diffrn_reflns_theta_max         27.88
_reflns_number_total             4611
_reflns_number_gt                3160
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'Bruker SMART. Area-Detector Software Package. (Siemens Industrial Automation, 1993, Inc.: Madison, WI)'
_computing_cell_refinement       
'Bruker SMART. Area-Detector Software Package. (Siemens Industrial Automation, 1993, Inc.: Madison, WI)'
_computing_data_reduction        
'Bruker SAINT. Area-Detector Integration Software. (Siemens Industrial Automation, 1995, Inc.: Madison, WI)'
_computing_structure_solution    
'SHELX-97. Programs for Crystal Structure Analysis. (G. M. Sheldrick, 1997, Release 97-2, University of Gttingen, Germany)'
_computing_structure_refinement  
'SHELX-97. Programs for Crystal Structure Analysis. (G. M. Sheldrick, 1997, Release 97-2, University of Gttingen, Germany)'
_computing_molecular_graphics    
'Ortep for Windows (L. J. Farrugia, J. Appl. Cryst. 1997, 30, 565)'
_computing_publication_material  
'WinGX v1.70.01 (L. J. Farrugia, J. Appl. Cryst. 1999, 32, 837)'

_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)+(0.0401P)²+0.1827P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4611
_refine_ls_number_parameters     220
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0460
_refine_ls_wR_factor_ref         0.1064
_refine_ls_wR_factor_gt          0.0938
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_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
C1 C 0.4550(3) 0.8891(3) 0.3517(3) 0.0507(8) Uani 1 1 d . . .
H1A H 0.4872 0.9144 0.4190 0.076 Uiso 1 1 calc R . .
H1B H 0.4394 0.9718 0.2670 0.076 Uiso 1 1 calc R . .
H1C H 0.5349 0.8291 0.3407 0.076 Uiso 1 1 calc R . .
C2 C 0.2152(3) 0.7526(3) 0.2750(2) 0.0482(7) Uani 1 1 d . . .
H2A H 0.2995 0.6993 0.2593 0.072 Uiso 1 1 calc R . .
H2B H 0.1932 0.8365 0.1927 0.072 Uiso 1 1 calc R . .
H2C H 0.1233 0.6983 0.3041 0.072 Uiso 1 1 calc R . .
C3 C 0.1197(3) 0.9212(3) 0.4075(3) 0.0547(8) Uani 1 1 d . . .
H3A H 0.0211 0.8765 0.4329 0.082 Uiso 1 1 calc R . .
H3B H 0.1113 0.9996 0.3188 0.082 Uiso 1 1 calc R . .
H3C H 0.1464 0.9527 0.4717 0.082 Uiso 1 1 calc R . .
C4 C 0.2821(2) 0.6789(2) 0.78930(19) 0.0203(4) Uani 1 1 d . . .
C5 C 0.2838(2) 0.8205(2) 0.7376(2) 0.0282(5) Uani 1 1 d . . .
H5 H 0.3342 0.8728 0.6552 0.034 Uiso 1 1 calc R . .
C6 C 0.2133(2) 0.8858(3) 0.8046(2) 0.0348(6) Uani 1 1 d . . .
H6 H 0.2157 0.9824 0.7684 0.042 Uiso 1 1 calc R . .
C7 C 0.1391(2) 0.8106(3) 0.9243(2) 0.0347(6) Uani 1 1 d . . .
H7 H 0.0894 0.8556 0.9698 0.042 Uiso 1 1 calc R . .
C8 C 0.1373(2) 0.6708(3) 0.9776(2) 0.0341(6) Uani 1 1 d . . .
H8 H 0.0871 0.6192 1.0603 0.041 Uiso 1 1 calc R . .
C9 C 0.2083(2) 0.6048(2) 0.9108(2) 0.0266(5) Uani 1 1 d . . .
H9 H 0.2068 0.5081 0.9484 0.032 Uiso 1 1 calc R . .
C10 C 0.3457(2) 0.4213(2) 0.78913(19) 0.0186(4) Uani 1 1 d . . .
C11 C 0.2254(2) 0.3583(2) 0.7655(2) 0.0247(5) Uani 1 1 d . . .
H11 H 0.1555 0.4107 0.6958 0.030 Uiso 1 1 calc R . .
C12 C 0.2059(2) 0.2196(2) 0.8428(2) 0.0321(5) Uani 1 1 d . . .
H12 H 0.1230 0.1772 0.8260 0.038 Uiso 1 1 calc R . .
C13 C 0.3074(3) 0.1430(2) 0.9443(2) 0.0330(6) Uani 1 1 d . . .
H13 H 0.2943 0.0478 0.9972 0.040 Uiso 1 1 calc R . .
C14 C 0.4272(3) 0.2042(2) 0.9691(2) 0.0329(5) Uani 1 1 d . . .
H14 H 0.4967 0.1512 1.0390 0.039 Uiso 1 1 calc R . .
C15 C 0.4467(2) 0.3425(2) 0.8924(2) 0.0262(5) Uani 1 1 d . . .
H15 H 0.5295 0.3843 0.9100 0.031 Uiso 1 1 calc R . .
C16 C 0.5694(2) 0.6290(2) 0.6832(2) 0.0209(4) Uani 1 1 d . . .
C17 C 0.6392(2) 0.6744(2) 0.7628(2) 0.0269(5) Uani 1 1 d . . .
H17 H 0.5788 0.6937 0.8238 0.032 Uiso 1 1 calc R . .
C18 C 0.7969(2) 0.6919(2) 0.7540(2) 0.0353(6) Uani 1 1 d . . .
H18 H 0.8437 0.7240 0.8082 0.042 Uiso 1 1 calc R . .
C19 C 0.8853(2) 0.6628(2) 0.6668(2) 0.0378(6) Uani 1 1 d . . .
H19 H 0.9930 0.6747 0.6609 0.045 Uiso 1 1 calc R . .
C20 C 0.8178(2) 0.6166(3) 0.5885(2) 0.0414(7) Uani 1 1 d . . .
H20 H 0.8794 0.5957 0.5291 0.050 Uiso 1 1 calc R . .
C21 C 0.6600(2) 0.6000(2) 0.5952(2) 0.0325(5) Uani 1 1 d . . .
H21 H 0.6141 0.5689 0.5399 0.039 Uiso 1 1 calc R . .
N1 N 0.28681(17) 0.65320(17) 0.55208(16) 0.0204(4) Uani 1 1 d . . .
Si1 Si 0.27168(6) 0.79758(6) 0.40566(6) 0.02307(15) Uani 1 1 d . . .
P1 P 0.36471(5) 0.60316(5) 0.68829(5) 0.01779(14) 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
C1 Si1 1.865(2) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 Si1 1.855(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 Si1 1.858(2) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C9 1.393(3) . ?
C4 C5 1.394(3) . ?
C4 P1 1.818(2) . ?
C5 C6 1.382(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.383(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.374(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.386(3) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.386(3) . ?
C10 C15 1.395(3) . ?
C10 P1 1.807(2) . ?
C11 C12 1.385(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.382(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.376(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.381(3) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.387(3) . ?
C16 C21 1.393(3) . ?
C16 P1 1.8149(19) . ?
C17 C18 1.392(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.377(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.371(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.391(3) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
N1 P1 1.5474(17) . ?
N1 Si1 1.6921(17) . ?

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
Si1 C1 H1A 109.5 . . ?
Si1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Si1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C9 C4 C5 118.24(19) . . ?
C9 C4 P1 123.84(17) . . ?
C5 C4 P1 117.78(15) . . ?
C6 C5 C4 120.9(2) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C5 C6 C7 120.0(2) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C8 C7 C6 120.1(2) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C8 C9 120.1(2) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
C8 C9 C4 120.7(2) . . ?
C8 C9 H9 119.6 . . ?
C4 C9 H9 119.6 . . ?
C11 C10 C15 118.75(19) . . ?
C11 C10 P1 119.22(15) . . ?
C15 C10 P1 122.02(16) . . ?
C12 C11 C10 120.6(2) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C13 C12 C11 119.8(2) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C14 C13 C12 120.2(2) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C13 C14 C15 120.1(2) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C14 C15 C10 120.5(2) . . ?
C14 C15 H15 119.7 . . ?
C10 C15 H15 119.7 . . ?
C17 C16 C21 118.93(18) . . ?
C17 C16 P1 123.36(15) . . ?
C21 C16 P1 117.71(16) . . ?
C16 C17 C18 120.4(2) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C19 C18 C17 120.1(2) . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C20 C19 C18 120.0(2) . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C19 C20 C21 120.5(2) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 H20 119.7 . . ?
C20 C21 C16 120.0(2) . . ?
C20 C21 H21 120.0 . . ?
C16 C21 H21 120.0 . . ?
P1 N1 Si1 138.42(11) . . ?
N1 Si1 C2 109.01(10) . . ?
N1 Si1 C3 113.07(10) . . ?
C2 Si1 C3 105.78(14) . . ?
N1 Si1 C1 113.02(10) . . ?
C2 Si1 C1 107.88(13) . . ?
C3 Si1 C1 107.71(14) . . ?
N1 P1 C10 110.73(9) . . ?
N1 P1 C16 115.87(9) . . ?
C10 P1 C16 105.07(9) . . ?
N1 P1 C4 114.54(9) . . ?
C10 P1 C4 104.68(9) . . ?
C16 P1 C4 104.93(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 C4 C5 C6 -0.5(3) . . . . ?
P1 C4 C5 C6 175.31(17) . . . . ?
C4 C5 C6 C7 -0.3(3) . . . . ?
C5 C6 C7 C8 0.9(3) . . . . ?
C6 C7 C8 C9 -0.7(3) . . . . ?
C7 C8 C9 C4 -0.1(3) . . . . ?
C5 C4 C9 C8 0.7(3) . . . . ?
P1 C4 C9 C8 -174.82(16) . . . . ?
C15 C10 C11 C12 -0.2(3) . . . . ?
P1 C10 C11 C12 -178.73(16) . . . . ?
C10 C11 C12 C13 0.0(3) . . . . ?
C11 C12 C13 C14 0.2(3) . . . . ?
C12 C13 C14 C15 -0.1(3) . . . . ?
C13 C14 C15 C10 -0.2(3) . . . . ?
C11 C10 C15 C14 0.3(3) . . . . ?
P1 C10 C15 C14 178.79(16) . . . . ?
C21 C16 C17 C18 0.6(3) . . . . ?
P1 C16 C17 C18 179.93(16) . . . . ?
C16 C17 C18 C19 -0.7(3) . . . . ?
C17 C18 C19 C20 0.1(4) . . . . ?
C18 C19 C20 C21 0.6(4) . . . . ?
C19 C20 C21 C16 -0.7(4) . . . . ?
C17 C16 C21 C20 0.1(3) . . . . ?
P1 C16 C21 C20 -179.26(18) . . . . ?
P1 N1 Si1 C2 159.69(16) . . . . ?
P1 N1 Si1 C3 -82.96(19) . . . . ?
P1 N1 Si1 C1 39.75(19) . . . . ?
Si1 N1 P1 C10 -172.29(13) . . . . ?
Si1 N1 P1 C16 -52.79(18) . . . . ?
Si1 N1 P1 C4 69.64(17) . . . . ?
C11 C10 P1 N1 -24.57(18) . . . . ?
C15 C10 P1 N1 156.94(16) . . . . ?
C11 C10 P1 C16 -150.37(16) . . . . ?
C15 C10 P1 C16 31.13(18) . . . . ?
C11 C10 P1 C4 99.37(17) . . . . ?
C15 C10 P1 C4 -79.13(17) . . . . ?
C17 C16 P1 N1 137.84(18) . . . . ?
C21 C16 P1 N1 -42.8(2) . . . . ?
C17 C16 P1 C10 -99.62(19) . . . . ?
C21 C16 P1 C10 79.70(18) . . . . ?
C17 C16 P1 C4 10.5(2) . . . . ?
C21 C16 P1 C4 -170.21(16) . . . . ?
C9 C4 P1 N1 115.54(17) . . . . ?
C5 C4 P1 N1 -60.00(18) . . . . ?
C9 C4 P1 C10 -5.91(19) . . . . ?
C5 C4 P1 C10 178.55(15) . . . . ?
C9 C4 P1 C16 -116.28(17) . . . . ?
C5 C4 P1 C16 68.18(17) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.88
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.059
_database_code_depnum_ccdc_archive 'CCDC 1018461'
#######################################################################
#
#                 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_2d

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H29 B N P'
_chemical_formula_sum            'C26 H29 B N P'
_chemical_formula_weight         397.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'


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

_cell_length_a                   8.7677(10)
_cell_length_b                   10.9331(14)
_cell_length_c                   12.2994(16)
_cell_angle_alpha                65.520(6)
_cell_angle_beta                 89.735(6)
_cell_angle_gamma                87.405(6)
_cell_volume                     1071.8(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9939
_cell_measurement_theta_min      4.651
_cell_measurement_theta_max      55.054

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             424
_exptl_absorpt_coefficient_mu    0.141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6984
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
'SADABS. Area-Detector Integration Software. (Siemens Industrial Automation, 1995, Inc.: Madison, WI)'

_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  'Bruker Apex II CCD 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            18329
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.82
_diffrn_reflns_theta_max         27.53
_reflns_number_total             4867
_reflns_number_gt                4044
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'Bruker SMART. Area-Detector Software Package. (Siemens Industrial Automation, 1993, Inc.: Madison, WI)'
_computing_cell_refinement       
'Bruker SMART. Area-Detector Software Package. (Siemens Industrial Automation, 1993, Inc.: Madison, WI)'
_computing_data_reduction        
'Bruker SAINT. Area-Detector Integration Software. (Siemens Industrial Automation, 1995, Inc.: Madison, WI)'
_computing_structure_solution    
'SHELX-97. Programs for Crystal Structure Analysis. (G. M. Sheldrick, 1997, Release 97-2, University of Gttingen, Germany)'
_computing_structure_refinement  
'SHELX-97. Programs for Crystal Structure Analysis. (G. M. Sheldrick, 1997, Release 97-2, University of Gttingen, Germany)'
_computing_molecular_graphics    
'Ortep for Windows (L. J. Farrugia, J. Appl. Cryst. 1997, 30, 565)'
_computing_publication_material  
'WinGX v1.70.01 (L. J. Farrugia, J. Appl. Cryst. 1999, 32, 837)'

_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)+(0.0379P)²+0.4860P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4867
_refine_ls_number_parameters     262
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0380
_refine_ls_wR_factor_ref         0.0942
_refine_ls_wR_factor_gt          0.0882
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_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
C1 C 0.85955(17) 0.74113(15) 0.61208(13) 0.0234(3) Uani 1 1 d . . .
H1 H 0.9196 0.8232 0.5916 0.028 Uiso 1 1 calc R . .
C2 C 0.96736(18) 0.62099(15) 0.61955(14) 0.0276(3) Uani 1 1 d . . .
H2A H 1.0223 0.6466 0.5433 0.033 Uiso 1 1 calc R . .
H2B H 1.0443 0.6018 0.6839 0.033 Uiso 1 1 calc R . .
C3 C 0.88202(19) 0.49335(15) 0.64416(15) 0.0292(3) Uani 1 1 d . . .
H3A H 0.9552 0.4227 0.6420 0.035 Uiso 1 1 calc R . .
H3B H 0.8391 0.4605 0.7254 0.035 Uiso 1 1 calc R . .
C4 C 0.75301(18) 0.51629(15) 0.55388(14) 0.0270(3) Uani 1 1 d . . .
H4A H 0.6958 0.4332 0.5788 0.032 Uiso 1 1 calc R . .
H4B H 0.7976 0.5343 0.4749 0.032 Uiso 1 1 calc R . .
C5 C 0.64020(17) 0.63533(14) 0.54142(13) 0.0230(3) Uani 1 1 d . . .
H5 H 0.5636 0.6513 0.4764 0.028 Uiso 1 1 calc R . .
C6 C 0.55718(19) 0.60751(17) 0.66066(15) 0.0330(4) Uani 1 1 d . . .
H6A H 0.4455 0.6180 0.6454 0.040 Uiso 1 1 calc R . .
H6B H 0.5813 0.5132 0.7174 0.040 Uiso 1 1 calc R . .
C7 C 0.6020(2) 0.70129(18) 0.71810(16) 0.0385(4) Uani 1 1 d . . .
H7A H 0.5576 0.7927 0.6694 0.046 Uiso 1 1 calc R . .
H7B H 0.5563 0.6700 0.7983 0.046 Uiso 1 1 calc R . .
C8 C 0.7738(2) 0.70989(17) 0.73082(14) 0.0336(4) Uani 1 1 d . . .
H8A H 0.8156 0.6234 0.7925 0.040 Uiso 1 1 calc R . .
H8B H 0.7924 0.7811 0.7585 0.040 Uiso 1 1 calc R . .
C9 C 0.67647(15) 1.09542(13) 0.18415(12) 0.0162(3) Uani 1 1 d . . .
C10 C 0.58451(17) 1.16512(14) 0.08299(13) 0.0222(3) Uani 1 1 d . . .
H10 H 0.5025 1.1222 0.0652 0.027 Uiso 1 1 calc R . .
C11 C 0.61317(19) 1.29737(15) 0.00845(13) 0.0273(3) Uani 1 1 d . . .
H11 H 0.5509 1.3447 -0.0607 0.033 Uiso 1 1 calc R . .
C12 C 0.73194(19) 1.36063(15) 0.03435(14) 0.0277(3) Uani 1 1 d . . .
H12 H 0.7514 1.4510 -0.0173 0.033 Uiso 1 1 calc R . .
C13 C 0.82242(18) 1.29269(15) 0.13522(14) 0.0264(3) Uani 1 1 d . . .
H13 H 0.9032 1.3367 0.1532 0.032 Uiso 1 1 calc R . .
C14 C 0.79511(16) 1.15995(14) 0.21035(13) 0.0212(3) Uani 1 1 d . . .
H14 H 0.8574 1.1133 0.2796 0.025 Uiso 1 1 calc R . .
C15 C 0.71670(15) 0.83231(13) 0.18670(12) 0.0173(3) Uani 1 1 d . . .
C26 C 0.37841(17) 0.91692(15) 0.38965(14) 0.0261(3) Uani 1 1 d . . .
H26 H 0.4390 0.9356 0.4443 0.031 Uiso 1 1 calc R . .
C16 C 0.80576(17) 0.89402(15) 0.08624(13) 0.0232(3) Uani 1 1 d . . .
H16 H 0.8263 0.9864 0.0596 0.028 Uiso 1 1 calc R . .
C17 C 0.86482(18) 0.82109(16) 0.02463(15) 0.0293(4) Uani 1 1 d . . .
H17 H 0.9252 0.8639 -0.0440 0.035 Uiso 1 1 calc R . .
C18 C 0.83574(18) 0.68625(16) 0.06311(15) 0.0279(3) Uani 1 1 d . . .
H18 H 0.8772 0.6365 0.0214 0.033 Uiso 1 1 calc R . .
C19 C 0.74653(17) 0.62377(15) 0.16213(14) 0.0247(3) Uani 1 1 d . . .
H19 H 0.7256 0.5316 0.1877 0.030 Uiso 1 1 calc R . .
C20 C 0.68757(16) 0.69580(14) 0.22421(13) 0.0215(3) Uani 1 1 d . . .
H20 H 0.6271 0.6523 0.2926 0.026 Uiso 1 1 calc R . .
C21 C 0.44695(15) 0.90000(13) 0.29375(12) 0.0180(3) Uani 1 1 d . . .
C22 C 0.35694(16) 0.87147(15) 0.21507(14) 0.0244(3) Uani 1 1 d . . .
H22 H 0.4025 0.8598 0.1496 0.029 Uiso 1 1 calc R . .
C23 C 0.19996(17) 0.86003(16) 0.23213(16) 0.0327(4) Uani 1 1 d . . .
H23 H 0.1390 0.8398 0.1786 0.039 Uiso 1 1 calc R . .
C24 C 0.13287(18) 0.87808(16) 0.32668(16) 0.0352(4) Uani 1 1 d . . .
H24 H 0.0258 0.8710 0.3377 0.042 Uiso 1 1 calc R . .
C25 C 0.22159(18) 0.90649(17) 0.40523(16) 0.0340(4) Uani 1 1 d . . .
H25 H 0.1752 0.9189 0.4701 0.041 Uiso 1 1 calc R . .
N1 N 0.74595(13) 0.87836(11) 0.39715(10) 0.0188(2) Uani 1 1 d . . .
B1 B 0.74223(18) 0.76366(16) 0.50639(14) 0.0194(3) Uani 1 1 d . . .
P1 P 0.65131(4) 0.91908(3) 0.27798(3) 0.01516(9) 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
C1 C8 1.554(2) . ?
C1 C2 1.554(2) . ?
C1 B1 1.591(2) . ?
C1 H1 1.0000 . ?
C2 C3 1.530(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.527(2) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.554(2) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.554(2) . ?
C5 B1 1.601(2) . ?
C5 H5 1.0000 . ?
C6 C7 1.531(2) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.526(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C14 1.3935(19) . ?
C9 C10 1.3953(19) . ?
C9 P1 1.8137(14) . ?
C10 C11 1.388(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.384(2) . ?
C11 H11 0.9500 . ?
C12 C13 1.383(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.391(2) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C16 1.393(2) . ?
C15 C20 1.4030(19) . ?
C15 P1 1.8212(14) . ?
C26 C25 1.391(2) . ?
C26 C21 1.397(2) . ?
C26 H26 0.9500 . ?
C16 C17 1.392(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.385(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.383(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.389(2) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C22 1.391(2) . ?
C21 P1 1.8135(14) . ?
C22 C23 1.395(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.382(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.383(3) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
N1 B1 1.409(2) . ?
N1 P1 1.5723(12) . ?

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
C8 C1 C2 111.87(13) . . ?
C8 C1 B1 110.62(13) . . ?
C2 C1 B1 104.82(12) . . ?
C8 C1 H1 109.8 . . ?
C2 C1 H1 109.8 . . ?
B1 C1 H1 109.8 . . ?
C3 C2 C1 112.80(13) . . ?
C3 C2 H2A 109.0 . . ?
C1 C2 H2A 109.0 . . ?
C3 C2 H2B 109.0 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
C4 C3 C2 112.63(13) . . ?
C4 C3 H3A 109.1 . . ?
C2 C3 H3A 109.1 . . ?
C4 C3 H3B 109.1 . . ?
C2 C3 H3B 109.1 . . ?
H3A C3 H3B 107.8 . . ?
C3 C4 C5 113.05(12) . . ?
C3 C4 H4A 109.0 . . ?
C5 C4 H4A 109.0 . . ?
C3 C4 H4B 109.0 . . ?
C5 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
C6 C5 C4 111.22(13) . . ?
C6 C5 B1 110.07(12) . . ?
C4 C5 B1 105.79(12) . . ?
C6 C5 H5 109.9 . . ?
C4 C5 H5 109.9 . . ?
B1 C5 H5 109.9 . . ?
C7 C6 C5 113.11(13) . . ?
C7 C6 H6A 109.0 . . ?
C5 C6 H6A 109.0 . . ?
C7 C6 H6B 109.0 . . ?
C5 C6 H6B 109.0 . . ?
H6A C6 H6B 107.8 . . ?
C8 C7 C6 114.50(14) . . ?
C8 C7 H7A 108.6 . . ?
C6 C7 H7A 108.6 . . ?
C8 C7 H7B 108.6 . . ?
C6 C7 H7B 108.6 . . ?
H7A C7 H7B 107.6 . . ?
C7 C8 C1 112.79(13) . . ?
C7 C8 H8A 109.0 . . ?
C1 C8 H8A 109.0 . . ?
C7 C8 H8B 109.0 . . ?
C1 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
C14 C9 C10 119.62(13) . . ?
C14 C9 P1 119.14(11) . . ?
C10 C9 P1 121.15(10) . . ?
C11 C10 C9 119.82(13) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C12 C11 C10 120.32(14) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C13 C12 C11 120.18(14) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C12 C13 C14 120.01(14) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C13 C14 C9 120.05(14) . . ?
C13 C14 H14 120.0 . . ?
C9 C14 H14 120.0 . . ?
C16 C15 C20 118.79(12) . . ?
C16 C15 P1 121.98(10) . . ?
C20 C15 P1 119.01(10) . . ?
C25 C26 C21 120.08(15) . . ?
C25 C26 H26 120.0 . . ?
C21 C26 H26 120.0 . . ?
C17 C16 C15 120.40(13) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C18 C17 C16 120.15(14) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C19 C18 C17 120.17(14) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C18 C19 C20 120.00(14) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
C19 C20 C15 120.50(13) . . ?
C19 C20 H20 119.7 . . ?
C15 C20 H20 119.7 . . ?
C22 C21 C26 119.31(13) . . ?
C22 C21 P1 123.43(11) . . ?
C26 C21 P1 117.26(11) . . ?
C21 C22 C23 120.15(15) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 H22 119.9 . . ?
C24 C23 C22 120.17(16) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 120.02(14) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C24 C25 C26 120.28(16) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
B1 N1 P1 130.86(11) . . ?
N1 B1 C1 121.07(13) . . ?
N1 B1 C5 128.67(13) . . ?
C1 B1 C5 110.04(12) . . ?
N1 P1 C21 116.12(6) . . ?
N1 P1 C9 108.78(6) . . ?
C21 P1 C9 106.16(6) . . ?
N1 P1 C15 113.99(6) . . ?
C21 P1 C15 106.62(6) . . ?
C9 P1 C15 104.26(6) . . ?

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
C8 C1 C2 C3 60.87(17) . . . . ?
B1 C1 C2 C3 -59.05(16) . . . . ?
C1 C2 C3 C4 54.65(18) . . . . ?
C2 C3 C4 C5 -53.14(18) . . . . ?
C3 C4 C5 C6 -63.06(17) . . . . ?
C3 C4 C5 B1 56.44(16) . . . . ?
C4 C5 C6 C7 112.76(16) . . . . ?
B1 C5 C6 C7 -4.15(19) . . . . ?
C5 C6 C7 C8 -50.6(2) . . . . ?
C6 C7 C8 C1 51.29(19) . . . . ?
C2 C1 C8 C7 -113.42(15) . . . . ?
B1 C1 C8 C7 3.04(18) . . . . ?
C14 C9 C10 C11 0.9(2) . . . . ?
P1 C9 C10 C11 -175.63(11) . . . . ?
C9 C10 C11 C12 -0.4(2) . . . . ?
C10 C11 C12 C13 -0.4(2) . . . . ?
C11 C12 C13 C14 0.6(2) . . . . ?
C12 C13 C14 C9 -0.1(2) . . . . ?
C10 C9 C14 C13 -0.7(2) . . . . ?
P1 C9 C14 C13 175.92(11) . . . . ?
C20 C15 C16 C17 -0.1(2) . . . . ?
P1 C15 C16 C17 174.37(12) . . . . ?
C15 C16 C17 C18 -0.2(2) . . . . ?
C16 C17 C18 C19 0.7(2) . . . . ?
C17 C18 C19 C20 -0.9(2) . . . . ?
C18 C19 C20 C15 0.5(2) . . . . ?
C16 C15 C20 C19 0.0(2) . . . . ?
P1 C15 C20 C19 -174.71(11) . . . . ?
C25 C26 C21 C22 -0.6(2) . . . . ?
C25 C26 C21 P1 178.61(12) . . . . ?
C26 C21 C22 C23 0.0(2) . . . . ?
P1 C21 C22 C23 -179.13(11) . . . . ?
C21 C22 C23 C24 0.5(2) . . . . ?
C22 C23 C24 C25 -0.5(2) . . . . ?
C23 C24 C25 C26 -0.1(2) . . . . ?
C21 C26 C25 C24 0.6(2) . . . . ?
P1 N1 B1 C1 175.66(10) . . . . ?
P1 N1 B1 C5 1.7(2) . . . . ?
C8 C1 B1 N1 129.07(14) . . . . ?
C2 C1 B1 N1 -110.18(15) . . . . ?
C8 C1 B1 C5 -55.94(15) . . . . ?
C2 C1 B1 C5 64.81(14) . . . . ?
C6 C5 B1 N1 -129.07(15) . . . . ?
C4 C5 B1 N1 110.68(16) . . . . ?
C6 C5 B1 C1 56.43(15) . . . . ?
C4 C5 B1 C1 -63.82(14) . . . . ?
B1 N1 P1 C21 46.68(15) . . . . ?
B1 N1 P1 C9 166.28(12) . . . . ?
B1 N1 P1 C15 -77.86(14) . . . . ?
C22 C21 P1 N1 -149.99(12) . . . . ?
C26 C21 P1 N1 30.84(13) . . . . ?
C22 C21 P1 C9 88.99(13) . . . . ?
C26 C21 P1 C9 -90.17(12) . . . . ?
C22 C21 P1 C15 -21.75(14) . . . . ?
C26 C21 P1 C15 159.08(11) . . . . ?
C14 C9 P1 N1 15.31(13) . . . . ?
C10 C9 P1 N1 -168.16(11) . . . . ?
C14 C9 P1 C21 140.94(11) . . . . ?
C10 C9 P1 C21 -42.53(13) . . . . ?
C14 C9 P1 C15 -106.67(11) . . . . ?
C10 C9 P1 C15 69.87(12) . . . . ?
C16 C15 P1 N1 -101.70(13) . . . . ?
C20 C15 P1 N1 72.79(12) . . . . ?
C16 C15 P1 C21 128.83(12) . . . . ?
C20 C15 P1 C21 -56.68(12) . . . . ?
C16 C15 P1 C9 16.77(13) . . . . ?
C20 C15 P1 C9 -168.74(11) . . . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        27.53
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.045
_database_code_depnum_ccdc_archive 'CCDC 1018462'
#######################################################################
#
#                 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_3c

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H37 B N P, C24 H37 B N P'
_chemical_formula_sum            'C48 H74 B2 N2 P2'
_chemical_formula_weight         762.65

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'


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

_cell_length_a                   12.0582(6)
_cell_length_b                   12.7370(6)
_cell_length_c                   15.7609(7)
_cell_angle_alpha                96.504(3)
_cell_angle_beta                 100.999(2)
_cell_angle_gamma                97.696(3)
_cell_volume                     2330.67(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8138
_cell_measurement_theta_min      4.98
_cell_measurement_theta_max      53.36

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.087
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             832
_exptl_absorpt_coefficient_mu    0.126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7085
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   
'SADABS. Area-Detector Integration Software. (Siemens Industrial Automation, 1995, Inc.: Madison, WI)'

_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  'Bruker Apex II CCD 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            38090
_diffrn_reflns_av_R_equivalents  0.0709
_diffrn_reflns_av_unetI/netI     0.1060
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.33
_diffrn_reflns_theta_max         27.12
_reflns_number_total             10233
_reflns_number_gt                5615
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'Bruker SMART. Area-Detector Software Package. (Siemens Industrial Automation, 1993, Inc.: Madison, WI)'
_computing_cell_refinement       
'Bruker SMART. Area-Detector Software Package. (Siemens Industrial Automation, 1993, Inc.: Madison, WI)'
_computing_data_reduction        
'Bruker SAINT. Area-Detector Integration Software. (Siemens Industrial Automation, 1995, Inc.: Madison, WI)'
_computing_structure_solution    
'SHELX-97. Programs for Crystal Structure Analysis. (G. M. Sheldrick, 1997, Release 97-2, University of Gttingen, Germany)'
_computing_structure_refinement  
'SHELX-97. Programs for Crystal Structure Analysis. (G. M. Sheldrick, 1997, Release 97-2, University of Gttingen, Germany)'
_computing_molecular_graphics    
'Ortep for Windows (L. J. Farrugia, J. Appl. Cryst. 1997, 30, 565)'
_computing_publication_material  
'WinGX v1.70.01 (L. J. Farrugia, J. Appl. Cryst. 1999, 32, 837)'

_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)+(0.0668P)²+0.3625P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10233
_refine_ls_number_parameters     505
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1392
_refine_ls_R_factor_gt           0.0629
_refine_ls_wR_factor_ref         0.1617
_refine_ls_wR_factor_gt          0.1323
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.001

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
C1 C 0.6908(3) 0.7695(3) 0.3664(2) 0.0519(9) Uani 1 1 d . . .
H1A H 0.6906 0.7854 0.3063 0.062 Uiso 1 1 calc R . .
H1B H 0.7700 0.7908 0.4008 0.062 Uiso 1 1 calc R . .
C2 C 0.6556(3) 0.6487(3) 0.3630(2) 0.0620(11) Uani 1 1 d . . .
H2A H 0.6552 0.6321 0.4222 0.093 Uiso 1 1 calc R . .
H2B H 0.7102 0.6106 0.3383 0.093 Uiso 1 1 calc R . .
H2C H 0.5788 0.6261 0.3263 0.093 Uiso 1 1 calc R . .
C3 C 0.4604(3) 0.8067(3) 0.34138(19) 0.0532(9) Uani 1 1 d . . .
H3A H 0.4690 0.8132 0.2809 0.064 Uiso 1 1 calc R . .
H3B H 0.4349 0.7301 0.3440 0.064 Uiso 1 1 calc R . .
C4 C 0.3679(3) 0.8705(3) 0.3624(2) 0.0675(11) Uani 1 1 d . . .
H4A H 0.3578 0.8637 0.4219 0.101 Uiso 1 1 calc R . .
H4B H 0.2956 0.8427 0.3209 0.101 Uiso 1 1 calc R . .
H4C H 0.3910 0.9461 0.3578 0.101 Uiso 1 1 calc R . .
C5 C 0.6413(3) 0.9868(3) 0.4016(2) 0.0632(11) Uani 1 1 d . . .
H5A H 0.5858 1.0294 0.4216 0.076 Uiso 1 1 calc R . .
H5B H 0.7166 1.0130 0.4412 0.076 Uiso 1 1 calc R . .
C6 C 0.6509(5) 1.0097(4) 0.3092(2) 0.0978(16) Uani 1 1 d . . .
H6A H 0.7082 0.9710 0.2892 0.147 Uiso 1 1 calc R . .
H6B H 0.6739 1.0867 0.3104 0.147 Uiso 1 1 calc R . .
H6C H 0.5766 0.9860 0.2692 0.147 Uiso 1 1 calc R . .
C7 C 0.5717(2) 0.7884(2) 0.66116(16) 0.0251(6) Uani 1 1 d . . .
C8 C 0.6204(2) 0.83440(19) 0.74877(16) 0.0237(6) Uani 1 1 d . . .
C9 C 0.5608(2) 0.8183(2) 0.81473(17) 0.0272(6) Uani 1 1 d . . .
H9 H 0.5945 0.8516 0.8726 0.033 Uiso 1 1 calc R . .
C10 C 0.4537(2) 0.7553(2) 0.79903(17) 0.0300(6) Uani 1 1 d . . .
C11 C 0.4065(2) 0.7097(2) 0.71355(18) 0.0336(7) Uani 1 1 d . . .
H11 H 0.3339 0.6652 0.7012 0.040 Uiso 1 1 calc R . .
C12 C 0.4614(2) 0.7268(2) 0.64532(17) 0.0326(7) Uani 1 1 d . . .
C13 C 0.7365(2) 0.9043(2) 0.77277(17) 0.0282(6) Uani 1 1 d . . .
H13A H 0.7318 0.9716 0.7487 0.042 Uiso 1 1 calc R . .
H13B H 0.7921 0.8671 0.7487 0.042 Uiso 1 1 calc R . .
H13C H 0.7608 0.9196 0.8365 0.042 Uiso 1 1 calc R . .
C14 C 0.3914(3) 0.7368(2) 0.87158(19) 0.0425(8) Uani 1 1 d . . .
H14A H 0.3157 0.6944 0.8471 0.064 Uiso 1 1 calc R . .
H14B H 0.3827 0.8058 0.9018 0.064 Uiso 1 1 calc R . .
H14C H 0.4353 0.6981 0.9130 0.064 Uiso 1 1 calc R . .
C15 C 0.3982(3) 0.6749(3) 0.55412(19) 0.0492(9) Uani 1 1 d . . .
H15A H 0.3408 0.6146 0.5584 0.074 Uiso 1 1 calc R . .
H15B H 0.4529 0.6490 0.5213 0.074 Uiso 1 1 calc R . .
H15C H 0.3603 0.7277 0.5238 0.074 Uiso 1 1 calc R . .
C16 C 0.7620(2) 0.7600(2) 0.59128(16) 0.0272(6) Uani 1 1 d . . .
C17 C 0.7715(2) 0.6513(2) 0.59787(17) 0.0309(7) Uani 1 1 d . . .
C18 C 0.8742(3) 0.6144(2) 0.59339(18) 0.0383(7) Uani 1 1 d . . .
H18 H 0.8779 0.5408 0.5964 0.046 Uiso 1 1 calc R . .
C19 C 0.9711(2) 0.6805(3) 0.58471(17) 0.0369(7) Uani 1 1 d . . .
C20 C 0.9633(2) 0.7876(2) 0.58318(17) 0.0352(7) Uani 1 1 d . . .
H20 H 1.0295 0.8354 0.5799 0.042 Uiso 1 1 calc R . .
C21 C 0.8619(2) 0.8281(2) 0.58632(16) 0.0297(6) Uani 1 1 d . . .
C22 C 0.6718(3) 0.5725(2) 0.6102(2) 0.0425(8) Uani 1 1 d . . .
H22A H 0.6943 0.5015 0.6117 0.064 Uiso 1 1 calc R . .
H22B H 0.6066 0.5690 0.5616 0.064 Uiso 1 1 calc R . .
H22C H 0.6501 0.5960 0.6653 0.064 Uiso 1 1 calc R . .
C23 C 1.0818(3) 0.6393(3) 0.5809(2) 0.0572(10) Uani 1 1 d . . .
H23A H 1.1345 0.6595 0.6377 0.086 Uiso 1 1 calc R . .
H23B H 1.1162 0.6706 0.5360 0.086 Uiso 1 1 calc R . .
H23C H 1.0666 0.5612 0.5663 0.086 Uiso 1 1 calc R . .
C24 C 0.8663(3) 0.9480(2) 0.5887(2) 0.0429(8) Uani 1 1 d . . .
H24A H 0.9182 0.9852 0.6424 0.064 Uiso 1 1 calc R . .
H24B H 0.7895 0.9658 0.5872 0.064 Uiso 1 1 calc R . .
H24C H 0.8941 0.9704 0.5380 0.064 Uiso 1 1 calc R . .
C25 C 0.9823(2) 0.6540(2) 1.32342(18) 0.0359(7) Uani 1 1 d . . .
H25A H 0.9173 0.6266 1.3491 0.043 Uiso 1 1 calc R . .
H25B H 1.0470 0.6167 1.3444 0.043 Uiso 1 1 calc R . .
C26 C 1.0176(3) 0.7743(2) 1.35487(19) 0.0462(8) Uani 1 1 d . . .
H26A H 1.0863 0.8006 1.3341 0.069 Uiso 1 1 calc R . .
H26B H 1.0337 0.7872 1.4188 0.069 Uiso 1 1 calc R . .
H26C H 0.9552 0.8121 1.3318 0.069 Uiso 1 1 calc R . .
C27 C 1.0730(2) 0.6523(2) 1.1673(2) 0.0344(7) Uani 1 1 d . . .
H27A H 1.0549 0.6363 1.1028 0.041 Uiso 1 1 calc R . .
H27B H 1.1023 0.7299 1.1830 0.041 Uiso 1 1 calc R . .
C28 C 1.1686(3) 0.5906(3) 1.2025(3) 0.0598(10) Uani 1 1 d . . .
H28A H 1.1852 0.6029 1.2665 0.090 Uiso 1 1 calc R . .
H28B H 1.2377 0.6156 1.1817 0.090 Uiso 1 1 calc R . .
H28C H 1.1441 0.5140 1.1819 0.090 Uiso 1 1 calc R . .
C29 C 0.9007(2) 0.4807(2) 1.18226(18) 0.0335(7) Uani 1 1 d . . .
H29A H 0.9630 0.4465 1.2127 0.040 Uiso 1 1 calc R . .
H29B H 0.8315 0.4596 1.2055 0.040 Uiso 1 1 calc R . .
C30 C 0.8761(3) 0.4387(2) 1.08429(19) 0.0432(8) Uani 1 1 d . . .
H30A H 0.8196 0.4770 1.0530 0.065 Uiso 1 1 calc R . .
H30B H 0.8458 0.3620 1.0748 0.065 Uiso 1 1 calc R . .
H30C H 0.9470 0.4502 1.0625 0.065 Uiso 1 1 calc R . .
C31 C 0.6625(2) 0.75589(18) 1.09882(15) 0.0200(6) Uani 1 1 d . . .
C32 C 0.5728(2) 0.67691(19) 1.10792(15) 0.0216(6) Uani 1 1 d . . .
C33 C 0.4632(2) 0.7021(2) 1.10696(16) 0.0268(6) Uani 1 1 d . . .
H33 H 0.4043 0.6475 1.1126 0.032 Uiso 1 1 calc R . .
C34 C 0.4372(2) 0.8035(2) 1.09807(16) 0.0266(6) Uani 1 1 d . . .
C35 C 0.5250(2) 0.8810(2) 1.08929(16) 0.0273(6) Uani 1 1 d . . .
H35 H 0.5098 0.9515 1.0838 0.033 Uiso 1 1 calc R . .
C36 C 0.6353(2) 0.85875(19) 1.08822(16) 0.0251(6) Uani 1 1 d . . .
C37 C 0.5898(2) 0.56232(19) 1.11719(18) 0.0291(6) Uani 1 1 d . . .
H37A H 0.6120 0.5299 1.0648 0.044 Uiso 1 1 calc R . .
H37B H 0.5182 0.5211 1.1242 0.044 Uiso 1 1 calc R . .
H37C H 0.6501 0.5621 1.1685 0.044 Uiso 1 1 calc R . .
C38 C 0.3185(2) 0.8289(2) 1.0973(2) 0.0391(7) Uani 1 1 d . . .
H38A H 0.2658 0.7900 1.0446 0.059 Uiso 1 1 calc R . .
H38B H 0.3194 0.9060 1.0978 0.059 Uiso 1 1 calc R . .
H38C H 0.2930 0.8072 1.1491 0.059 Uiso 1 1 calc R . .
C39 C 0.7244(2) 0.9497(2) 1.0787(2) 0.0379(7) Uani 1 1 d . . .
H39A H 0.6890 1.0139 1.0715 0.057 Uiso 1 1 calc R . .
H39B H 0.7560 0.9298 1.0273 0.057 Uiso 1 1 calc R . .
H39C H 0.7860 0.9642 1.1310 0.057 Uiso 1 1 calc R . .
C40 C 0.8554(2) 0.75489(18) 1.02503(16) 0.0198(6) Uani 1 1 d . . .
C41 C 0.9582(2) 0.82839(18) 1.03959(16) 0.0198(6) Uani 1 1 d . . .
C42 C 1.0154(2) 0.84321(19) 0.97201(16) 0.0224(6) Uani 1 1 d . . .
H42 H 1.0839 0.8937 0.9835 0.027 Uiso 1 1 calc R . .
C43 C 0.9763(2) 0.78718(19) 0.88865(16) 0.0218(6) Uani 1 1 d . . .
C44 C 0.8740(2) 0.71606(19) 0.87376(17) 0.0236(6) Uani 1 1 d . . .
H44 H 0.8444 0.6775 0.8169 0.028 Uiso 1 1 calc R . .
C45 C 0.8135(2) 0.69955(19) 0.93957(16) 0.0219(6) Uani 1 1 d . . .
C46 C 1.0075(2) 0.89895(19) 1.12699(16) 0.0262(6) Uani 1 1 d . . .
H46A H 1.0879 0.8915 1.1464 0.039 Uiso 1 1 calc R . .
H46B H 0.9642 0.8769 1.1704 0.039 Uiso 1 1 calc R . .
H46C H 1.0022 0.9738 1.1204 0.039 Uiso 1 1 calc R . .
C47 C 1.0392(2) 0.8044(2) 0.81629(17) 0.0323(7) Uani 1 1 d . . .
H47A H 1.0167 0.8661 0.7894 0.048 Uiso 1 1 calc R . .
H47B H 1.0200 0.7404 0.7721 0.048 Uiso 1 1 calc R . .
H47C H 1.1218 0.8177 0.8402 0.048 Uiso 1 1 calc R . .
C48 C 0.7027(2) 0.62090(19) 0.91706(17) 0.0278(6) Uani 1 1 d . . .
H48A H 0.6819 0.5986 0.8538 0.042 Uiso 1 1 calc R . .
H48B H 0.6419 0.6551 0.9362 0.042 Uiso 1 1 calc R . .
H48C H 0.7128 0.5581 0.9466 0.042 Uiso 1 1 calc R . .
N1 N 0.58702(19) 0.84003(18) 0.51067(14) 0.0327(6) Uani 1 1 d . . .
N2 N 0.83827(17) 0.68221(16) 1.17258(14) 0.0263(5) Uani 1 1 d . . .
B1 B 0.6396(3) 0.8001(2) 0.5844(2) 0.0287(7) Uani 1 1 d . . .
B2 B 0.7899(2) 0.7293(2) 1.10192(19) 0.0214(7) Uani 1 1 d . . .
P1 P 0.59823(7) 0.84903(7) 0.41397(5) 0.0399(2) Uani 1 1 d . . .
P2 P 0.94137(6) 0.62390(5) 1.20608(5) 0.02610(19) 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
C1 C2 1.532(5) . ?
C1 P1 1.813(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.529(4) . ?
C3 P1 1.804(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.540(5) . ?
C5 P1 1.805(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C12 1.413(4) . ?
C7 C8 1.418(3) . ?
C7 B1 1.595(4) . ?
C8 C9 1.390(4) . ?
C8 C13 1.512(3) . ?
C9 C10 1.389(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.385(4) . ?
C10 C14 1.506(4) . ?
C11 C12 1.388(4) . ?
C11 H11 0.9500 . ?
C12 C15 1.522(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C21 1.408(4) . ?
C16 C17 1.418(4) . ?
C16 B1 1.614(4) . ?
C17 C18 1.394(4) . ?
C17 C22 1.517(4) . ?
C18 C19 1.384(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.383(4) . ?
C19 C23 1.507(4) . ?
C20 C21 1.397(4) . ?
C20 H20 0.9500 . ?
C21 C24 1.516(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.532(4) . ?
C25 P2 1.803(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.534(4) . ?
C27 P2 1.813(3) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.534(4) . ?
C29 P2 1.801(3) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C36 1.413(3) . ?
C31 C32 1.415(3) . ?
C31 B2 1.610(4) . ?
C32 C33 1.398(3) . ?
C32 C37 1.520(3) . ?
C33 C34 1.386(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.385(4) . ?
C34 C38 1.507(4) . ?
C35 C36 1.399(3) . ?
C35 H35 0.9500 . ?
C36 C39 1.512(4) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 C45 1.413(3) . ?
C40 C41 1.413(3) . ?
C40 B2 1.607(4) . ?
C41 C42 1.392(3) . ?
C41 C46 1.524(3) . ?
C42 C43 1.385(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.392(3) . ?
C43 C47 1.506(4) . ?
C44 C45 1.396(4) . ?
C44 H44 0.9500 . ?
C45 C48 1.514(3) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
N1 B1 1.396(4) . ?
N1 P1 1.571(2) . ?
N2 B2 1.392(3) . ?
N2 P2 1.569(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
C2 C1 P1 113.6(2) . . ?
C2 C1 H1A 108.9 . . ?
P1 C1 H1A 108.9 . . ?
C2 C1 H1B 108.9 . . ?
P1 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 P1 114.0(2) . . ?
C4 C3 H3A 108.7 . . ?
P1 C3 H3A 108.7 . . ?
C4 C3 H3B 108.7 . . ?
P1 C3 H3B 108.7 . . ?
H3A C3 H3B 107.6 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 P1 116.8(3) . . ?
C6 C5 H5A 108.1 . . ?
P1 C5 H5A 108.1 . . ?
C6 C5 H5B 108.1 . . ?
P1 C5 H5B 108.1 . . ?
H5A C5 H5B 107.3 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C12 C7 C8 116.8(2) . . ?
C12 C7 B1 121.1(2) . . ?
C8 C7 B1 122.1(2) . . ?
C9 C8 C7 120.5(2) . . ?
C9 C8 C13 118.2(2) . . ?
C7 C8 C13 121.2(2) . . ?
C10 C9 C8 122.4(2) . . ?
C10 C9 H9 118.8 . . ?
C8 C9 H9 118.8 . . ?
C11 C10 C9 117.1(3) . . ?
C11 C10 C14 121.3(3) . . ?
C9 C10 C14 121.7(2) . . ?
C10 C11 C12 122.4(3) . . ?
C10 C11 H11 118.8 . . ?
C12 C11 H11 118.8 . . ?
C11 C12 C7 120.8(2) . . ?
C11 C12 C15 117.0(3) . . ?
C7 C12 C15 122.2(3) . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C10 C14 H14A 109.5 . . ?
C10 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C10 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C21 C16 C17 117.0(2) . . ?
C21 C16 B1 122.5(2) . . ?
C17 C16 B1 120.4(2) . . ?
C18 C17 C16 120.2(3) . . ?
C18 C17 C22 118.2(3) . . ?
C16 C17 C22 121.6(2) . . ?
C19 C18 C17 122.7(3) . . ?
C19 C18 H18 118.6 . . ?
C17 C18 H18 118.6 . . ?
C20 C19 C18 116.9(3) . . ?
C20 C19 C23 121.1(3) . . ?
C18 C19 C23 122.0(3) . . ?
C19 C20 C21 122.5(3) . . ?
C19 C20 H20 118.8 . . ?
C21 C20 H20 118.8 . . ?
C20 C21 C16 120.6(3) . . ?
C20 C21 C24 117.2(3) . . ?
C16 C21 C24 122.1(2) . . ?
C17 C22 H22A 109.5 . . ?
C17 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C17 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C23 H23A 109.5 . . ?
C19 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C19 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 P2 112.40(19) . . ?
C26 C25 H25A 109.1 . . ?
P2 C25 H25A 109.1 . . ?
C26 C25 H25B 109.1 . . ?
P2 C25 H25B 109.1 . . ?
H25A C25 H25B 107.9 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 P2 115.7(2) . . ?
C28 C27 H27A 108.4 . . ?
P2 C27 H27A 108.4 . . ?
C28 C27 H27B 108.4 . . ?
P2 C27 H27B 108.4 . . ?
H27A C27 H27B 107.4 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 P2 113.15(19) . . ?
C30 C29 H29A 108.9 . . ?
P2 C29 H29A 108.9 . . ?
C30 C29 H29B 108.9 . . ?
P2 C29 H29B 108.9 . . ?
H29A C29 H29B 107.8 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C36 C31 C32 117.0(2) . . ?
C36 C31 B2 121.9(2) . . ?
C32 C31 B2 121.1(2) . . ?
C33 C32 C31 120.3(2) . . ?
C33 C32 C37 117.4(2) . . ?
C31 C32 C37 122.2(2) . . ?
C34 C33 C32 122.6(2) . . ?
C34 C33 H33 118.7 . . ?
C32 C33 H33 118.7 . . ?
C35 C34 C33 117.1(2) . . ?
C35 C34 C38 121.2(2) . . ?
C33 C34 C38 121.7(2) . . ?
C34 C35 C36 122.1(2) . . ?
C34 C35 H35 118.9 . . ?
C36 C35 H35 118.9 . . ?
C35 C36 C31 120.8(2) . . ?
C35 C36 C39 117.5(2) . . ?
C31 C36 C39 121.6(2) . . ?
C32 C37 H37A 109.5 . . ?
C32 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C32 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C34 C38 H38A 109.5 . . ?
C34 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C34 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C45 C40 C41 117.2(2) . . ?
C45 C40 B2 120.1(2) . . ?
C41 C40 B2 122.6(2) . . ?
C42 C41 C40 120.5(2) . . ?
C42 C41 C46 117.1(2) . . ?
C40 C41 C46 122.3(2) . . ?
C43 C42 C41 122.5(2) . . ?
C43 C42 H42 118.7 . . ?
C41 C42 H42 118.7 . . ?
C42 C43 C44 117.1(2) . . ?
C42 C43 C47 121.8(2) . . ?
C44 C43 C47 121.1(2) . . ?
C43 C44 C45 122.2(2) . . ?
C43 C44 H44 118.9 . . ?
C45 C44 H44 118.9 . . ?
C44 C45 C40 120.5(2) . . ?
C44 C45 C48 118.4(2) . . ?
C40 C45 C48 121.1(2) . . ?
C41 C46 H46A 109.5 . . ?
C41 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C41 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C43 C47 H47A 109.5 . . ?
C43 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C43 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C45 C48 H48A 109.5 . . ?
C45 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C45 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
B1 N1 P1 140.5(2) . . ?
B2 N2 P2 142.1(2) . . ?
N1 B1 C7 118.0(2) . . ?
N1 B1 C16 122.2(3) . . ?
C7 B1 C16 119.8(2) . . ?
N2 B2 C40 122.6(2) . . ?
N2 B2 C31 117.0(2) . . ?
C40 B2 C31 120.5(2) . . ?
N1 P1 C3 109.81(15) . . ?
N1 P1 C5 110.43(14) . . ?
C3 P1 C5 105.90(17) . . ?
N1 P1 C1 118.47(14) . . ?
C3 P1 C1 103.55(15) . . ?
C5 P1 C1 107.82(18) . . ?
N2 P2 C29 111.11(12) . . ?
N2 P2 C25 109.29(13) . . ?
C29 P2 C25 105.80(13) . . ?
N2 P2 C27 119.26(12) . . ?
C29 P2 C27 105.12(14) . . ?
C25 P2 C27 105.34(14) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.12
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.056
_database_code_depnum_ccdc_archive 'CCDC 1018463'
#######################################################################
#
#                 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_3d

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H37 B N P'
_chemical_formula_sum            'C36 H37 B N P'
_chemical_formula_weight         525.45

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'



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                   16.3277(4)
_cell_length_b                   11.4623(3)
_cell_length_c                   16.3393(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.8330(10)
_cell_angle_gamma                90.00
_cell_volume                     2956.05(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    248
_cell_measurement_theta_min      6.256
_cell_measurement_theta_max      54.925

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1120
_exptl_absorpt_coefficient_mu    0.118
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7195
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
'SADABS. Area-Detector Integration Software. (Siemens Industrial Automation, 1995, Inc.: Madison, WI)'

_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  'Bruker Apex II CCD 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            14775
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.20
_diffrn_reflns_theta_max         27.49
_reflns_number_total             6740
_reflns_number_gt                5551
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'Bruker SMART. Area-Detector Software Package. (Siemens Industrial Automation, 1993, Inc.: Madison, WI)'
_computing_cell_refinement       
'Bruker SMART. Area-Detector Software Package. (Siemens Industrial Automation, 1993, Inc.: Madison, WI)'
_computing_data_reduction        
'Bruker SAINT. Area-Detector Integration Software. (Siemens Industrial Automation, 1995, Inc.: Madison, WI)'
_computing_structure_solution    
'SHELX-97. Programs for Crystal Structure Analysis. (G. M. Sheldrick, 1997, Release 97-2, University of Gttingen, Germany)'
_computing_structure_refinement  
'SHELX-97. Programs for Crystal Structure Analysis. (G. M. Sheldrick, 1997, Release 97-2, University of Gttingen, Germany)'
_computing_molecular_graphics    
'Ortep for Windows (L. J. Farrugia, J. Appl. Cryst. 1997, 30, 565)'
_computing_publication_material  
'WinGX v1.70.01 (L. J. Farrugia, J. Appl. Cryst. 1999, 32, 837)'

_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)+(0.0501P)²+1.2623P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6740
_refine_ls_number_parameters     358
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0391
_refine_ls_wR_factor_ref         0.1073
_refine_ls_wR_factor_gt          0.1001
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.015
_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 0.35278(2) 0.32986(3) 0.15738(2) 0.01443(9) Uani 1 1 d . . .
N1 N 0.30680(7) 0.43275(10) 0.19134(7) 0.0161(2) Uani 1 1 d . . .
C1 C 0.21366(9) -0.02250(13) 0.12404(11) 0.0270(3) Uani 1 1 d . . .
H1 H 0.1829 -0.0937 0.1181 0.032 Uiso 1 1 calc R . .
C2 C 0.24568(10) 0.02560(14) 0.20353(10) 0.0271(3) Uani 1 1 d . . .
H27 H 0.2376 -0.0132 0.2522 0.033 Uiso 1 1 calc R . .
C3 C 0.28954(9) 0.13036(13) 0.21213(9) 0.0212(3) Uani 1 1 d . . .
H28 H 0.3108 0.1636 0.2667 0.025 Uiso 1 1 calc R . .
C4 C 0.30273(8) 0.18742(12) 0.14101(9) 0.0168(3) Uani 1 1 d . . .
C5 C 0.15378(8) 0.35687(12) 0.18411(8) 0.0164(3) Uani 1 1 d . . .
C6 C 0.11636(8) 0.32316(13) 0.09978(9) 0.0197(3) Uani 1 1 d . . .
C7 C 0.05972(9) 0.22964(14) 0.08253(10) 0.0259(3) Uani 1 1 d . . .
H18 H 0.0350 0.2089 0.0252 0.031 Uiso 1 1 calc R . .
C8 C 0.03842(9) 0.16617(13) 0.14622(11) 0.0276(3) Uani 1 1 d . . .
C9 C -0.01960(11) 0.06154(16) 0.12651(14) 0.0420(5) Uani 1 1 d . . .
H2 H -0.0429 0.0554 0.0651 0.063 Uiso 1 1 calc R . .
H20 H -0.0660 0.0707 0.1540 0.063 Uiso 1 1 calc R . .
H19 H 0.0125 -0.0093 0.1476 0.063 Uiso 1 1 calc R . .
C10 C 0.42006(10) 0.44232(16) -0.08756(10) 0.0294(4) Uani 1 1 d . . .
H3 H 0.4347 0.4668 -0.1375 0.035 Uiso 1 1 calc R . .
C11 C 0.37463(10) 0.51607(15) -0.04868(10) 0.0275(3) Uani 1 1 d . . .
H37 H 0.3578 0.5909 -0.0720 0.033 Uiso 1 1 calc R . .
C12 C 0.35348(9) 0.48037(13) 0.02499(9) 0.0220(3) Uani 1 1 d . . .
H36 H 0.3223 0.5311 0.0517 0.026 Uiso 1 1 calc R . .
C13 C 0.37775(8) 0.37117(12) 0.05952(8) 0.0180(3) Uani 1 1 d . . .
C14 C 0.21328(8) 0.57173(12) 0.25413(8) 0.0168(3) Uani 1 1 d . . .
C15 C 0.26299(9) 0.60139(13) 0.33583(9) 0.0203(3) Uani 1 1 d . . .
C16 C 0.33836(9) 0.52985(15) 0.38236(9) 0.0266(3) Uani 1 1 d . . .
H6 H 0.3908 0.5700 0.3803 0.040 Uiso 1 1 calc R . .
H5 H 0.3365 0.4531 0.3555 0.040 Uiso 1 1 calc R . .
H4 H 0.3367 0.5200 0.4415 0.040 Uiso 1 1 calc R . .
C17 C 0.24294(10) 0.69930(14) 0.37773(10) 0.0267(3) Uani 1 1 d . . .
H14 H 0.2758 0.7155 0.4335 0.032 Uiso 1 1 calc R . .
C18 C 0.17687(10) 0.77365(14) 0.34102(11) 0.0283(3) Uani 1 1 d . . .
C19 C 0.15211(12) 0.87559(16) 0.38824(13) 0.0411(5) Uani 1 1 d . . .
H7 H 0.1866 0.8751 0.4469 0.062 Uiso 1 1 calc R . .
H9 H 0.0921 0.8692 0.3875 0.062 Uiso 1 1 calc R . .
H8 H 0.1616 0.9486 0.3609 0.062 Uiso 1 1 calc R . .
C20 C 0.13135(10) 0.74879(13) 0.25894(10) 0.0256(3) Uani 1 1 d . . .
H13 H 0.0880 0.8010 0.2309 0.031 Uiso 1 1 calc R . .
C21 C 0.14720(9) 0.64945(13) 0.21626(9) 0.0211(3) Uani 1 1 d . . .
C22 C 0.09172(11) 0.62870(15) 0.12834(10) 0.0327(4) Uani 1 1 d . . .
H11 H 0.0492 0.6907 0.1137 0.049 Uiso 1 1 calc R . .
H12 H 0.0633 0.5531 0.1265 0.049 Uiso 1 1 calc R . .
H10 H 0.1267 0.6288 0.0877 0.049 Uiso 1 1 calc R . .
C23 C 0.12981(9) 0.29417(13) 0.24858(9) 0.0200(3) Uani 1 1 d . . .
C24 C 0.07371(9) 0.20065(13) 0.22902(10) 0.0254(3) Uani 1 1 d . . .
H21 H 0.0592 0.1593 0.2737 0.030 Uiso 1 1 calc R . .
C25 C 0.13616(10) 0.38491(14) 0.02562(9) 0.0267(3) Uani 1 1 d . . .
H15 H 0.1602 0.3291 -0.0073 0.040 Uiso 1 1 calc R . .
H17 H 0.1772 0.4474 0.0464 0.040 Uiso 1 1 calc R . .
H16 H 0.0840 0.4183 -0.0104 0.040 Uiso 1 1 calc R . .
C26 C 0.16892(10) 0.32021(15) 0.34083(9) 0.0284(3) Uani 1 1 d . . .
H23 H 0.1313 0.2923 0.3747 0.043 Uiso 1 1 calc R . .
H22 H 0.1771 0.4046 0.3486 0.043 Uiso 1 1 calc R . .
H24 H 0.2238 0.2807 0.3591 0.043 Uiso 1 1 calc R . .
C27 C 0.22646(9) 0.03298(13) 0.05335(10) 0.0252(3) Uani 1 1 d . . .
H25 H 0.2048 -0.0005 -0.0011 0.030 Uiso 1 1 calc R . .
C28 C 0.27082(9) 0.13763(13) 0.06135(9) 0.0215(3) Uani 1 1 d . . .
H26 H 0.2794 0.1753 0.0124 0.026 Uiso 1 1 calc R . .
C29 C 0.45488(8) 0.30520(12) 0.23110(8) 0.0169(3) Uani 1 1 d . . .
C30 C 0.50039(9) 0.20226(13) 0.23122(9) 0.0237(3) Uani 1 1 d . . .
H33 H 0.4759 0.1399 0.1948 0.028 Uiso 1 1 calc R . .
C31 C 0.58154(9) 0.19033(14) 0.28437(10) 0.0264(3) Uani 1 1 d . . .
H32 H 0.6124 0.1201 0.2840 0.032 Uiso 1 1 calc R . .
C32 C 0.61707(9) 0.28051(14) 0.33752(10) 0.0273(3) Uani 1 1 d . . .
H29 H 0.6726 0.2726 0.3734 0.033 Uiso 1 1 calc R . .
C33 C 0.57207(10) 0.38255(14) 0.33869(11) 0.0287(3) Uani 1 1 d . . .
H31 H 0.5964 0.4442 0.3758 0.034 Uiso 1 1 calc R . .
C34 C 0.49119(9) 0.39461(12) 0.28544(10) 0.0227(3) Uani 1 1 d . . .
H30 H 0.4605 0.4648 0.2863 0.027 Uiso 1 1 calc R . .
C35 C 0.42385(9) 0.29757(14) 0.01955(10) 0.0245(3) Uani 1 1 d . . .
H35 H 0.4413 0.2229 0.0429 0.029 Uiso 1 1 calc R . .
C36 C 0.44424(10) 0.33309(15) -0.05408(10) 0.0300(3) Uani 1 1 d . . .
H34 H 0.4748 0.2823 -0.0815 0.036 Uiso 1 1 calc R . .
B1 B 0.22770(9) 0.45263(13) 0.20759(9) 0.0153(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 N1 1.5735(11) . ?
P1 C13 1.8113(14) . ?
P1 C29 1.8115(13) . ?
P1 C4 1.8147(14) . ?
N1 B1 1.4021(18) . ?
C1 C27 1.381(2) . ?
C1 C2 1.384(2) . ?
C1 H1 0.9500 . ?
C2 C3 1.387(2) . ?
C2 H27 0.9500 . ?
C3 C4 1.3973(19) . ?
C3 H28 0.9500 . ?
C4 C28 1.3943(19) . ?
C5 C6 1.4106(19) . ?
C5 C23 1.4109(19) . ?
C5 B1 1.604(2) . ?
C6 C7 1.397(2) . ?
C6 C25 1.508(2) . ?
C7 C8 1.385(2) . ?
C7 H18 0.9500 . ?
C8 C24 1.385(2) . ?
C8 C9 1.511(2) . ?
C9 H2 0.9800 . ?
C9 H20 0.9800 . ?
C9 H19 0.9800 . ?
C10 C11 1.382(2) . ?
C10 C36 1.383(2) . ?
C10 H3 0.9500 . ?
C11 C12 1.396(2) . ?
C11 H37 0.9500 . ?
C12 C13 1.388(2) . ?
C12 H36 0.9500 . ?
C13 C35 1.399(2) . ?
C14 C21 1.4137(19) . ?
C14 C15 1.4147(19) . ?
C14 B1 1.609(2) . ?
C15 C17 1.396(2) . ?
C15 C16 1.512(2) . ?
C16 H6 0.9800 . ?
C16 H5 0.9800 . ?
C16 H4 0.9800 . ?
C17 C18 1.385(2) . ?
C17 H14 0.9500 . ?
C18 C20 1.386(2) . ?
C18 C19 1.511(2) . ?
C19 H7 0.9800 . ?
C19 H9 0.9800 . ?
C19 H8 0.9800 . ?
C20 C21 1.394(2) . ?
C20 H13 0.9500 . ?
C21 C22 1.508(2) . ?
C22 H11 0.9800 . ?
C22 H12 0.9800 . ?
C22 H10 0.9800 . ?
C23 C24 1.393(2) . ?
C23 C26 1.509(2) . ?
C24 H21 0.9500 . ?
C25 H15 0.9800 . ?
C25 H17 0.9800 . ?
C25 H16 0.9800 . ?
C26 H23 0.9800 . ?
C26 H22 0.9800 . ?
C26 H24 0.9800 . ?
C27 C28 1.390(2) . ?
C27 H25 0.9500 . ?
C28 H26 0.9500 . ?
C29 C34 1.3859(19) . ?
C29 C30 1.3942(19) . ?
C30 C31 1.393(2) . ?
C30 H33 0.9500 . ?
C31 C32 1.379(2) . ?
C31 H32 0.9500 . ?
C32 C33 1.384(2) . ?
C32 H29 0.9500 . ?
C33 C34 1.390(2) . ?
C33 H31 0.9500 . ?
C34 H30 0.9500 . ?
C35 C36 1.389(2) . ?
C35 H35 0.9500 . ?
C36 H34 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
N1 P1 C13 110.54(6) . . ?
N1 P1 C29 108.87(6) . . ?
C13 P1 C29 104.54(6) . . ?
N1 P1 C4 119.26(6) . . ?
C13 P1 C4 107.44(6) . . ?
C29 P1 C4 105.11(6) . . ?
B1 N1 P1 137.26(10) . . ?
C27 C1 C2 119.98(14) . . ?
C27 C1 H1 120.0 . . ?
C2 C1 H1 120.0 . . ?
C1 C2 C3 120.08(14) . . ?
C1 C2 H27 120.0 . . ?
C3 C2 H27 120.0 . . ?
C2 C3 C4 120.44(14) . . ?
C2 C3 H28 119.8 . . ?
C4 C3 H28 119.8 . . ?
C28 C4 C3 118.98(13) . . ?
C28 C4 P1 123.53(11) . . ?
C3 C4 P1 117.26(10) . . ?
C6 C5 C23 117.14(12) . . ?
C6 C5 B1 122.17(12) . . ?
C23 C5 B1 120.38(12) . . ?
C7 C6 C5 120.42(13) . . ?
C7 C6 C25 117.72(13) . . ?
C5 C6 C25 121.86(13) . . ?
C8 C7 C6 122.16(14) . . ?
C8 C7 H18 118.9 . . ?
C6 C7 H18 118.9 . . ?
C7 C8 C24 117.52(14) . . ?
C7 C8 C9 121.40(16) . . ?
C24 C8 C9 121.06(16) . . ?
C8 C9 H2 109.5 . . ?
C8 C9 H20 109.5 . . ?
H2 C9 H20 109.5 . . ?
C8 C9 H19 109.5 . . ?
H2 C9 H19 109.5 . . ?
H20 C9 H19 109.5 . . ?
C11 C10 C36 120.30(14) . . ?
C11 C10 H3 119.8 . . ?
C36 C10 H3 119.8 . . ?
C10 C11 C12 119.83(15) . . ?
C10 C11 H37 120.1 . . ?
C12 C11 H37 120.1 . . ?
C13 C12 C11 120.44(14) . . ?
C13 C12 H36 119.8 . . ?
C11 C12 H36 119.8 . . ?
C12 C13 C35 119.07(13) . . ?
C12 C13 P1 119.28(10) . . ?
C35 C13 P1 121.61(11) . . ?
C21 C14 C15 116.79(13) . . ?
C21 C14 B1 121.02(12) . . ?
C15 C14 B1 122.13(12) . . ?
C17 C15 C14 120.39(14) . . ?
C17 C15 C16 116.88(13) . . ?
C14 C15 C16 122.73(13) . . ?
C15 C16 H6 109.5 . . ?
C15 C16 H5 109.5 . . ?
H6 C16 H5 109.5 . . ?
C15 C16 H4 109.5 . . ?
H6 C16 H4 109.5 . . ?
H5 C16 H4 109.5 . . ?
C18 C17 C15 122.45(14) . . ?
C18 C17 H14 118.8 . . ?
C15 C17 H14 118.8 . . ?
C17 C18 C20 117.23(14) . . ?
C17 C18 C19 122.35(16) . . ?
C20 C18 C19 120.38(16) . . ?
C18 C19 H7 109.5 . . ?
C18 C19 H9 109.5 . . ?
H7 C19 H9 109.5 . . ?
C18 C19 H8 109.5 . . ?
H7 C19 H8 109.5 . . ?
H9 C19 H8 109.5 . . ?
C18 C20 C21 122.00(14) . . ?
C18 C20 H13 119.0 . . ?
C21 C20 H13 119.0 . . ?
C20 C21 C14 120.96(14) . . ?
C20 C21 C22 117.53(13) . . ?
C14 C21 C22 121.50(13) . . ?
C21 C22 H11 109.5 . . ?
C21 C22 H12 109.5 . . ?
H11 C22 H12 109.5 . . ?
C21 C22 H10 109.5 . . ?
H11 C22 H10 109.5 . . ?
H12 C22 H10 109.5 . . ?
C24 C23 C5 120.83(13) . . ?
C24 C23 C26 117.83(13) . . ?
C5 C23 C26 121.19(13) . . ?
C8 C24 C23 121.89(14) . . ?
C8 C24 H21 119.1 . . ?
C23 C24 H21 119.1 . . ?
C6 C25 H15 109.5 . . ?
C6 C25 H17 109.5 . . ?
H15 C25 H17 109.5 . . ?
C6 C25 H16 109.5 . . ?
H15 C25 H16 109.5 . . ?
H17 C25 H16 109.5 . . ?
C23 C26 H23 109.5 . . ?
C23 C26 H22 109.5 . . ?
H23 C26 H22 109.5 . . ?
C23 C26 H24 109.5 . . ?
H23 C26 H24 109.5 . . ?
H22 C26 H24 109.5 . . ?
C1 C27 C28 120.37(14) . . ?
C1 C27 H25 119.8 . . ?
C28 C27 H25 119.8 . . ?
C27 C28 C4 120.15(14) . . ?
C27 C28 H26 119.9 . . ?
C4 C28 H26 119.9 . . ?
C34 C29 C30 118.98(13) . . ?
C34 C29 P1 118.72(10) . . ?
C30 C29 P1 122.17(11) . . ?
C31 C30 C29 120.37(14) . . ?
C31 C30 H33 119.8 . . ?
C29 C30 H33 119.8 . . ?
C32 C31 C30 119.93(14) . . ?
C32 C31 H32 120.0 . . ?
C30 C31 H32 120.0 . . ?
C31 C32 C33 120.21(14) . . ?
C31 C32 H29 119.9 . . ?
C33 C32 H29 119.9 . . ?
C32 C33 C34 119.87(14) . . ?
C32 C33 H31 120.1 . . ?
C34 C33 H31 120.1 . . ?
C29 C34 C33 120.64(13) . . ?
C29 C34 H30 119.7 . . ?
C33 C34 H30 119.7 . . ?
C36 C35 C13 120.30(15) . . ?
C36 C35 H35 119.8 . . ?
C13 C35 H35 119.8 . . ?
C10 C36 C35 120.04(15) . . ?
C10 C36 H34 120.0 . . ?
C35 C36 H34 120.0 . . ?
N1 B1 C5 121.12(12) . . ?
N1 B1 C14 118.73(12) . . ?
C5 B1 C14 120.10(11) . . ?

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
C13 P1 N1 B1 117.49(14) . . . . ?
C29 P1 N1 B1 -128.22(14) . . . . ?
C4 P1 N1 B1 -7.74(17) . . . . ?
C27 C1 C2 C3 0.9(2) . . . . ?
C1 C2 C3 C4 -0.8(2) . . . . ?
C2 C3 C4 C28 0.3(2) . . . . ?
C2 C3 C4 P1 174.88(11) . . . . ?
N1 P1 C4 C28 111.63(12) . . . . ?
C13 P1 C4 C28 -15.07(13) . . . . ?
C29 P1 C4 C28 -126.01(12) . . . . ?
N1 P1 C4 C3 -62.73(12) . . . . ?
C13 P1 C4 C3 170.57(10) . . . . ?
C29 P1 C4 C3 59.63(12) . . . . ?
C23 C5 C6 C7 -1.5(2) . . . . ?
B1 C5 C6 C7 172.12(13) . . . . ?
C23 C5 C6 C25 179.10(13) . . . . ?
B1 C5 C6 C25 -7.3(2) . . . . ?
C5 C6 C7 C8 -0.5(2) . . . . ?
C25 C6 C7 C8 178.99(14) . . . . ?
C6 C7 C8 C24 1.8(2) . . . . ?
C6 C7 C8 C9 -176.92(14) . . . . ?
C36 C10 C11 C12 0.4(2) . . . . ?
C10 C11 C12 C13 0.0(2) . . . . ?
C11 C12 C13 C35 0.1(2) . . . . ?
C11 C12 C13 P1 177.64(11) . . . . ?
N1 P1 C13 C12 -1.78(13) . . . . ?
C29 P1 C13 C12 -118.78(12) . . . . ?
C4 P1 C13 C12 129.89(11) . . . . ?
N1 P1 C13 C35 175.66(11) . . . . ?
C29 P1 C13 C35 58.66(13) . . . . ?
C4 P1 C13 C35 -52.68(13) . . . . ?
C21 C14 C15 C17 3.91(19) . . . . ?
B1 C14 C15 C17 -173.31(13) . . . . ?
C21 C14 C15 C16 -176.97(13) . . . . ?
B1 C14 C15 C16 5.8(2) . . . . ?
C14 C15 C17 C18 -2.6(2) . . . . ?
C16 C15 C17 C18 178.21(14) . . . . ?
C15 C17 C18 C20 -1.4(2) . . . . ?
C15 C17 C18 C19 176.43(14) . . . . ?
C17 C18 C20 C21 4.0(2) . . . . ?
C19 C18 C20 C21 -173.88(14) . . . . ?
C18 C20 C21 C14 -2.6(2) . . . . ?
C18 C20 C21 C22 177.78(14) . . . . ?
C15 C14 C21 C20 -1.4(2) . . . . ?
B1 C14 C21 C20 175.84(12) . . . . ?
C15 C14 C21 C22 178.20(13) . . . . ?
B1 C14 C21 C22 -4.6(2) . . . . ?
C6 C5 C23 C24 2.10(19) . . . . ?
B1 C5 C23 C24 -171.62(13) . . . . ?
C6 C5 C23 C26 177.45(13) . . . . ?
B1 C5 C23 C26 3.7(2) . . . . ?
C7 C8 C24 C23 -1.1(2) . . . . ?
C9 C8 C24 C23 177.56(14) . . . . ?
C5 C23 C24 C8 -0.8(2) . . . . ?
C26 C23 C24 C8 -176.32(14) . . . . ?
C2 C1 C27 C28 -0.5(2) . . . . ?
C1 C27 C28 C4 0.0(2) . . . . ?
C3 C4 C28 C27 0.2(2) . . . . ?
P1 C4 C28 C27 -174.10(11) . . . . ?
N1 P1 C29 C34 -21.68(13) . . . . ?
C13 P1 C29 C34 96.46(12) . . . . ?
C4 P1 C29 C34 -150.53(11) . . . . ?
N1 P1 C29 C30 162.51(12) . . . . ?
C13 P1 C29 C30 -79.35(13) . . . . ?
C4 P1 C29 C30 33.66(13) . . . . ?
C34 C29 C30 C31 -0.9(2) . . . . ?
P1 C29 C30 C31 174.93(12) . . . . ?
C29 C30 C31 C32 0.3(2) . . . . ?
C30 C31 C32 C33 0.5(2) . . . . ?
C31 C32 C33 C34 -0.7(2) . . . . ?
C30 C29 C34 C33 0.7(2) . . . . ?
P1 C29 C34 C33 -175.29(12) . . . . ?
C32 C33 C34 C29 0.1(2) . . . . ?
C12 C13 C35 C36 -0.6(2) . . . . ?
P1 C13 C35 C36 -178.04(11) . . . . ?
C11 C10 C36 C35 -0.8(2) . . . . ?
C13 C35 C36 C10 0.9(2) . . . . ?
P1 N1 B1 C5 -4.8(2) . . . . ?
P1 N1 B1 C14 172.69(11) . . . . ?
C6 C5 B1 N1 -64.24(18) . . . . ?
C23 C5 B1 N1 109.15(15) . . . . ?
C6 C5 B1 C14 118.35(14) . . . . ?
C23 C5 B1 C14 -68.26(17) . . . . ?
C21 C14 B1 N1 122.93(14) . . . . ?
C15 C14 B1 N1 -59.97(17) . . . . ?
C21 C14 B1 C5 -59.59(17) . . . . ?
C15 C14 B1 C5 117.51(14) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.046
_database_code_depnum_ccdc_archive 'CCDC 1018464'
#######################################################################
#
#                 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_5a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H33 Cl N P Si'
_chemical_formula_sum            'C14 H33 Cl N P Si'
_chemical_formula_weight         309.92

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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                   9.9618(7)
_cell_length_b                   12.7168(10)
_cell_length_c                   14.8199(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.454(2)
_cell_angle_gamma                90.00
_cell_volume                     1840.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6001
_cell_measurement_theta_min      4.541
_cell_measurement_theta_max      54.914

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             680
_exptl_absorpt_coefficient_mu    0.348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6400
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
'SADABS. Area-Detector Integration Software. (Siemens Industrial Automation, 1995, Inc.: Madison, WI)'

_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  'Bruker Apex II CCD 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            16773
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         27.47
_reflns_number_total             4205
_reflns_number_gt                2842
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'Bruker SMART. Area-Detector Software Package. (Siemens Industrial Automation, 1993, Inc.: Madison, WI)'
_computing_cell_refinement       
'Bruker SMART. Area-Detector Software Package. (Siemens Industrial Automation, 1993, Inc.: Madison, WI)'
_computing_data_reduction        
'Bruker SAINT. Area-Detector Integration Software. (Siemens Industrial Automation, 1995, Inc.: Madison, WI)'
_computing_structure_solution    
'SHELX-97. Programs for Crystal Structure Analysis. (G. M. Sheldrick, 1997, Release 97-2, University of Gttingen, Germany)'
_computing_structure_refinement  
'SHELX-97. Programs for Crystal Structure Analysis. (G. M. Sheldrick, 1997, Release 97-2, University of Gttingen, Germany)'
_computing_molecular_graphics    
'Ortep for Windows (L. J. Farrugia, J. Appl. Cryst. 1997, 30, 565)'
_computing_publication_material  
'WinGX v1.70.01 (L. J. Farrugia, J. Appl. Cryst. 1999, 32, 837)'

_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)+(0.0782P)²+0.2023P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4205
_refine_ls_number_parameters     174
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0438
_refine_ls_wR_factor_ref         0.1413
_refine_ls_wR_factor_gt          0.1206
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_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
C1 C 0.6419(3) 0.63121(17) 0.25614(16) 0.0380(6) Uani 1 1 d . . .
H1A H 0.6090 0.5705 0.2173 0.057 Uiso 1 1 calc R . .
H1B H 0.5905 0.6367 0.3058 0.057 Uiso 1 1 calc R . .
H1C H 0.7395 0.6223 0.2826 0.057 Uiso 1 1 calc R . .
C2 C 0.6577(2) 0.87072(17) 0.25969(15) 0.0356(5) Uani 1 1 d . . .
H2A H 0.7564 0.8732 0.2845 0.053 Uiso 1 1 calc R . .
H2B H 0.6082 0.8671 0.3105 0.053 Uiso 1 1 calc R . .
H2C H 0.6299 0.9341 0.2232 0.053 Uiso 1 1 calc R . .
C3 C 0.7093(2) 0.87590(15) -0.05620(14) 0.0263(4) Uani 1 1 d . . .
C4 C 0.5576(2) 0.87235(19) -0.10312(16) 0.0418(6) Uani 1 1 d . . .
H4A H 0.5292 0.9415 -0.1292 0.063 Uiso 1 1 calc R . .
H4B H 0.5023 0.8535 -0.0577 0.063 Uiso 1 1 calc R . .
H4C H 0.5442 0.8197 -0.1524 0.063 Uiso 1 1 calc R . .
C5 C 0.7219(2) 0.96828(17) 0.01247(16) 0.0403(6) Uani 1 1 d . . .
H5A H 0.6876 1.0327 -0.0205 0.060 Uiso 1 1 calc R . .
H5B H 0.8183 0.9778 0.0420 0.060 Uiso 1 1 calc R . .
H5C H 0.6680 0.9530 0.0595 0.060 Uiso 1 1 calc R . .
C6 C 0.7941(2) 0.90079(17) -0.12952(15) 0.0364(5) Uani 1 1 d . . .
H6A H 0.7878 0.8419 -0.1728 0.055 Uiso 1 1 calc R . .
H6B H 0.8900 0.9117 -0.0996 0.055 Uiso 1 1 calc R . .
H6C H 0.7585 0.9647 -0.1629 0.055 Uiso 1 1 calc R . .
C7 C 0.94832(19) 0.73954(14) 0.04648(14) 0.0232(4) Uani 1 1 d . . .
C8 C 0.9826(2) 0.65934(18) 0.12618(15) 0.0359(5) Uani 1 1 d . . .
H8A H 0.9522 0.5891 0.1036 0.054 Uiso 1 1 calc R . .
H8B H 0.9355 0.6795 0.1757 0.054 Uiso 1 1 calc R . .
H8C H 1.0817 0.6585 0.1498 0.054 Uiso 1 1 calc R . .
C9 C 1.0222(2) 0.70742(18) -0.03067(14) 0.0327(5) Uani 1 1 d . . .
H9A H 0.9964 0.7555 -0.0829 0.049 Uiso 1 1 calc R . .
H9B H 0.9961 0.6355 -0.0505 0.049 Uiso 1 1 calc R . .
H9C H 1.1215 0.7108 -0.0080 0.049 Uiso 1 1 calc R . .
C10 C 1.0070(2) 0.84457(18) 0.08698(15) 0.0362(5) Uani 1 1 d . . .
H10A H 1.1036 0.8354 0.1160 0.054 Uiso 1 1 calc R . .
H10B H 0.9557 0.8685 0.1332 0.054 Uiso 1 1 calc R . .
H10C H 0.9991 0.8970 0.0377 0.054 Uiso 1 1 calc R . .
C11 C 0.6877(2) 0.63321(16) -0.06422(14) 0.0273(5) Uani 1 1 d . . .
C12 C 0.7517(2) 0.53164(17) -0.01892(16) 0.0384(6) Uani 1 1 d . . .
H12A H 0.7407 0.5293 0.0453 0.058 Uiso 1 1 calc R . .
H12B H 0.8494 0.5300 -0.0210 0.058 Uiso 1 1 calc R . .
H12C H 0.7058 0.4708 -0.0521 0.058 Uiso 1 1 calc R . .
C13 C 0.7107(3) 0.63693(19) -0.16388(14) 0.0403(6) Uani 1 1 d . . .
H13A H 0.6737 0.5729 -0.1964 0.060 Uiso 1 1 calc R . .
H13B H 0.8090 0.6417 -0.1634 0.060 Uiso 1 1 calc R . .
H13C H 0.6640 0.6985 -0.1953 0.060 Uiso 1 1 calc R . .
C14 C 0.5329(2) 0.62425(19) -0.06606(17) 0.0435(6) Uani 1 1 d . . .
H14A H 0.4986 0.5574 -0.0947 0.065 Uiso 1 1 calc R . .
H14B H 0.4848 0.6827 -0.1017 0.065 Uiso 1 1 calc R . .
H14C H 0.5168 0.6269 -0.0030 0.065 Uiso 1 1 calc R . .
N1 N 0.69327(17) 0.75003(12) 0.09796(12) 0.0275(4) Uani 1 1 d . . .
P1 P 0.75571(5) 0.74972(3) 0.01016(3) 0.01740(15) Uani 1 1 d . . .
Si1 Si 0.61696(5) 0.75270(4) 0.18544(4) 0.01992(16) Uani 1 1 d . . .
Cl1 Cl 0.40188(6) 0.76098(5) 0.14058(5) 0.0468(2) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 Si1 1.856(2) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 Si1 1.858(2) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.534(3) . ?
C3 C6 1.536(3) . ?
C3 C5 1.543(3) . ?
C3 P1 1.8908(19) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C10 1.532(3) . ?
C7 C9 1.533(3) . ?
C7 C8 1.546(3) . ?
C7 P1 1.8915(19) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.535(3) . ?
C11 C13 1.540(3) . ?
C11 C14 1.541(3) . ?
C11 P1 1.890(2) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
N1 P1 1.5498(16) . ?
N1 Si1 1.6282(16) . ?
Si1 Cl1 2.1161(8) . ?

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
Si1 C1 H1A 109.5 . . ?
Si1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Si1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 C6 108.44(17) . . ?
C4 C3 C5 105.39(17) . . ?
C6 C3 C5 108.99(17) . . ?
C4 C3 P1 109.15(14) . . ?
C6 C3 P1 115.52(13) . . ?
C5 C3 P1 108.88(14) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C10 C7 C9 108.80(16) . . ?
C10 C7 C8 105.47(17) . . ?
C9 C7 C8 109.16(16) . . ?
C10 C7 P1 109.77(13) . . ?
C9 C7 P1 114.59(14) . . ?
C8 C7 P1 108.66(13) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C13 108.52(17) . . ?
C12 C11 C14 105.83(17) . . ?
C13 C11 C14 108.91(18) . . ?
C12 C11 P1 109.57(14) . . ?
C13 C11 P1 115.53(14) . . ?
C14 C11 P1 108.05(14) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
P1 N1 Si1 175.79(13) . . ?
N1 P1 C11 109.54(9) . . ?
N1 P1 C3 109.69(8) . . ?
C11 P1 C3 109.85(10) . . ?
N1 P1 C7 108.35(9) . . ?
C11 P1 C7 109.77(8) . . ?
C3 P1 C7 109.61(9) . . ?
N1 Si1 C1 113.63(9) . . ?
N1 Si1 C2 114.01(9) . . ?
C1 Si1 C2 110.43(11) . . ?
N1 Si1 Cl1 110.77(7) . . ?
C1 Si1 Cl1 103.46(8) . . ?
C2 Si1 Cl1 103.55(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Si1 N1 P1 C11 -70.6(16) . . . . ?
Si1 N1 P1 C3 50.0(16) . . . . ?
Si1 N1 P1 C7 169.7(16) . . . . ?
C12 C11 P1 N1 -71.89(16) . . . . ?
C13 C11 P1 N1 165.21(15) . . . . ?
C14 C11 P1 N1 42.97(17) . . . . ?
C12 C11 P1 C3 167.56(13) . . . . ?
C13 C11 P1 C3 44.65(18) . . . . ?
C14 C11 P1 C3 -77.59(16) . . . . ?
C12 C11 P1 C7 46.97(16) . . . . ?
C13 C11 P1 C7 -75.94(17) . . . . ?
C14 C11 P1 C7 161.82(15) . . . . ?
C4 C3 P1 N1 -73.44(16) . . . . ?
C6 C3 P1 N1 164.10(16) . . . . ?
C5 C3 P1 N1 41.12(17) . . . . ?
C4 C3 P1 C11 47.03(16) . . . . ?
C6 C3 P1 C11 -75.44(18) . . . . ?
C5 C3 P1 C11 161.59(14) . . . . ?
C4 C3 P1 C7 167.71(14) . . . . ?
C6 C3 P1 C7 45.25(18) . . . . ?
C5 C3 P1 C7 -77.73(15) . . . . ?
C10 C7 P1 N1 -73.59(15) . . . . ?
C9 C7 P1 N1 163.65(14) . . . . ?
C8 C7 P1 N1 41.27(16) . . . . ?
C10 C7 P1 C11 166.82(14) . . . . ?
C9 C7 P1 C11 44.07(17) . . . . ?
C8 C7 P1 C11 -78.31(16) . . . . ?
C10 C7 P1 C3 46.08(16) . . . . ?
C9 C7 P1 C3 -76.68(16) . . . . ?
C8 C7 P1 C3 160.95(14) . . . . ?
P1 N1 Si1 C1 127.7(16) . . . . ?
P1 N1 Si1 C2 -104.5(16) . . . . ?
P1 N1 Si1 Cl1 11.8(16) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.064
_database_code_depnum_ccdc_archive 'CCDC 1018465'
#######################################################################
#
#                 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_6a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H32 B Cl N P'
_chemical_formula_sum            'C18 H32 B Cl N P'
_chemical_formula_weight         339.68

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_space_group_name_Hall  'P 2yb'

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

_cell_length_a                   8.7750(9)
_cell_length_b                   22.773(2)
_cell_length_c                   19.917(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.781(4)
_cell_angle_gamma                90.00
_cell_volume                     3922.2(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6066
_cell_measurement_theta_min      4.521
_cell_measurement_theta_max      49.488

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1472
_exptl_absorpt_coefficient_mu    0.274
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6673
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
'SADABS. Area-Detector Integration Software. (Siemens Industrial Automation, 1995, Inc.: Madison, WI)'

_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  'Bruker Apex II CCD 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            31274
_diffrn_reflns_av_R_equivalents  0.0764
_diffrn_reflns_av_unetI/netI     0.1737
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.37
_diffrn_reflns_theta_max         27.46
_reflns_number_total             16698
_reflns_number_gt                9225
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'Bruker SMART. Area-Detector Software Package. (Siemens Industrial Automation, 1993, Inc.: Madison, WI)'
_computing_cell_refinement       
'Bruker SMART. Area-Detector Software Package. (Siemens Industrial Automation, 1993, Inc.: Madison, WI)'
_computing_data_reduction        
'Bruker SAINT. Area-Detector Integration Software. (Siemens Industrial Automation, 1995, Inc.: Madison, WI)'
_computing_structure_solution    
'SHELX-97. Programs for Crystal Structure Analysis. (G. M. Sheldrick, 1997, Release 97-2, University of Gttingen, Germany)'
_computing_structure_refinement  
'SHELX-97. Programs for Crystal Structure Analysis. (G. M. Sheldrick, 1997, Release 97-2, University of Gttingen, Germany)'
_computing_molecular_graphics    
'Ortep for Windows (L. J. Farrugia, J. Appl. Cryst. 1997, 30, 565)'
_computing_publication_material  
'WinGX v1.70.01 (L. J. Farrugia, J. Appl. Cryst. 1999, 32, 837)'

_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)+(0.0482P)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    constr
_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   0.48(7)
_refine_ls_number_reflns         16698
_refine_ls_number_parameters     829
_refine_ls_number_restraints     97
_refine_ls_R_factor_all          0.1564
_refine_ls_R_factor_gt           0.0722
_refine_ls_wR_factor_ref         0.1485
_refine_ls_wR_factor_gt          0.1180
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_restrained_S_all      0.981
_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
C1 C 0.7666(6) 0.8625(2) 0.9825(2) 0.0256(13) Uani 1 1 d . . .
C2 C 0.6531(7) 0.8644(3) 0.9151(2) 0.0373(15) Uani 1 1 d . . .
H2A H 0.5535 0.8479 0.9217 0.056 Uiso 1 1 calc R . .
H2B H 0.6946 0.8413 0.8808 0.056 Uiso 1 1 calc R . .
H2C H 0.6384 0.9051 0.8996 0.056 Uiso 1 1 calc R . .
C3 C 0.9291(6) 0.8814(2) 0.9703(3) 0.0334(14) Uani 1 1 d . . .
H3A H 0.9696 0.8519 0.9421 0.050 Uiso 1 1 calc R . .
H3B H 0.9987 0.8848 1.0141 0.050 Uiso 1 1 calc R . .
H3C H 0.9218 0.9194 0.9469 0.050 Uiso 1 1 calc R . .
C4 C 0.7838(6) 0.7976(2) 1.0078(3) 0.0314(14) Uani 1 1 d . . .
H4A H 0.8490 0.7962 1.0529 0.047 Uiso 1 1 calc R . .
H4B H 0.8317 0.7742 0.9756 0.047 Uiso 1 1 calc R . .
H4C H 0.6815 0.7815 1.0106 0.047 Uiso 1 1 calc R . .
C5 C 0.5013(6) 0.8973(2) 1.0575(2) 0.0265(13) Uani 1 1 d . . .
C6 C 0.4578(6) 0.8311(2) 1.0535(3) 0.0351(15) Uani 1 1 d . . .
H6A H 0.4646 0.8161 1.0080 0.053 Uiso 1 1 calc R . .
H6B H 0.3520 0.8262 1.0623 0.053 Uiso 1 1 calc R . .
H6C H 0.5294 0.8093 1.0878 0.053 Uiso 1 1 calc R . .
C7 C 0.3867(6) 0.9301(2) 1.0028(3) 0.0395(16) Uani 1 1 d . . .
H7A H 0.4014 0.9726 1.0089 0.059 Uiso 1 1 calc R . .
H7B H 0.2805 0.9198 1.0073 0.059 Uiso 1 1 calc R . .
H7C H 0.4054 0.9189 0.9574 0.059 Uiso 1 1 calc R . .
C8 C 0.4709(6) 0.9152(3) 1.1292(3) 0.0394(15) Uani 1 1 d . . .
H8A H 0.3598 0.9131 1.1302 0.059 Uiso 1 1 calc R . .
H8B H 0.5073 0.9555 1.1392 0.059 Uiso 1 1 calc R . .
H8C H 0.5264 0.8885 1.1634 0.059 Uiso 1 1 calc R . .
C9 C 0.7488(6) 0.9892(2) 1.0379(2) 0.0233(12) Uani 1 1 d . . .
C10 C 0.6982(6) 1.0097(2) 0.9632(3) 0.0334(14) Uani 1 1 d . . .
H10A H 0.7535 0.9868 0.9332 0.050 Uiso 1 1 calc R . .
H10B H 0.7226 1.0514 0.9595 0.050 Uiso 1 1 calc R . .
H10C H 0.5866 1.0038 0.9496 0.050 Uiso 1 1 calc R . .
C11 C 0.6676(7) 1.0291(2) 1.0843(3) 0.0324(15) Uani 1 1 d . . .
H11A H 0.7025 1.0698 1.0810 0.049 Uiso 1 1 calc R . .
H11B H 0.6936 1.0157 1.1316 0.049 Uiso 1 1 calc R . .
H11C H 0.5553 1.0272 1.0694 0.049 Uiso 1 1 calc R . .
C12 C 0.9236(6) 1.0019(2) 1.0582(3) 0.0354(15) Uani 1 1 d . . .
H12A H 0.9423 1.0440 1.0537 0.053 Uiso 1 1 calc R . .
H12B H 0.9808 0.9799 1.0282 0.053 Uiso 1 1 calc R . .
H12C H 0.9585 0.9898 1.1055 0.053 Uiso 1 1 calc R . .
C13 C 1.0245(6) 0.8570(2) 1.2223(2) 0.0220(13) Uani 1 1 d . . .
C14 C 1.0679(7) 0.8499(3) 1.2926(3) 0.0326(15) Uani 1 1 d . . .
H14 H 1.0125 0.8707 1.3221 0.039 Uiso 1 1 calc R . .
C15 C 1.1887(7) 0.8136(3) 1.3213(3) 0.0418(17) Uani 1 1 d . . .
H15 H 1.2116 0.8084 1.3693 0.050 Uiso 1 1 calc R . .
C16 C 1.2756(7) 0.7850(3) 1.2794(3) 0.0453(18) Uani 1 1 d . . .
H16 H 1.3597 0.7606 1.2985 0.054 Uiso 1 1 calc R . .
C17 C 1.2394(7) 0.7921(3) 1.2100(3) 0.0409(16) Uani 1 1 d . . .
H17 H 1.2994 0.7729 1.1811 0.049 Uiso 1 1 calc R . .
C18 C 1.1163(6) 0.8270(2) 1.1823(3) 0.0323(14) Uani 1 1 d . . .
H18 H 1.0926 0.8308 1.1342 0.039 Uiso 1 1 calc R . .
C19 C 0.3002(6) 0.0590(2) 0.2592(3) 0.0260(13) Uani 1 1 d . . .
C20 C 0.2087(7) 0.0077(2) 0.2823(3) 0.0416(16) Uani 1 1 d . . .
H20A H 0.2162 0.0089 0.3319 0.062 Uiso 1 1 calc R . .
H20B H 0.2513 -0.0295 0.2690 0.062 Uiso 1 1 calc R . .
H20C H 0.0999 0.0108 0.2608 0.062 Uiso 1 1 calc R . .
C21 C 0.4713(6) 0.0468(2) 0.2862(3) 0.0365(15) Uani 1 1 d . . .
H21A H 0.4947 0.0057 0.2775 0.055 Uiso 1 1 calc R . .
H21B H 0.4933 0.0544 0.3353 0.055 Uiso 1 1 calc R . .
H21C H 0.5355 0.0725 0.2630 0.055 Uiso 1 1 calc R . .
C22 C 0.2729(7) 0.0608(3) 0.1793(3) 0.0383(16) Uani 1 1 d . . .
H22A H 0.1659 0.0724 0.1621 0.057 Uiso 1 1 calc R . .
H22B H 0.2921 0.0217 0.1618 0.057 Uiso 1 1 calc R . .
H22C H 0.3437 0.0892 0.1642 0.057 Uiso 1 1 calc R . .
C23 C 0.3177(6) 0.1948(2) 0.2548(3) 0.0258(13) Uani 1 1 d . . .
C24 C 0.2208(6) 0.2126(3) 0.1848(3) 0.0401(16) Uani 1 1 d . . .
H24A H 0.2132 0.1792 0.1536 0.060 Uiso 1 1 calc R . .
H24B H 0.2714 0.2455 0.1657 0.060 Uiso 1 1 calc R . .
H24C H 0.1169 0.2245 0.1913 0.060 Uiso 1 1 calc R . .
C25 C 0.4843(6) 0.1836(2) 0.2440(3) 0.0307(14) Uani 1 1 d . . .
H25A H 0.5308 0.2207 0.2327 0.046 Uiso 1 1 calc R . .
H25B H 0.4838 0.1556 0.2066 0.046 Uiso 1 1 calc R . .
H25C H 0.5447 0.1674 0.2858 0.046 Uiso 1 1 calc R . .
C26 C 0.3256(7) 0.2482(2) 0.3040(3) 0.0396(15) Uani 1 1 d . . .
H26A H 0.2207 0.2592 0.3099 0.059 Uiso 1 1 calc R . .
H26B H 0.3745 0.2814 0.2848 0.059 Uiso 1 1 calc R . .
H26C H 0.3864 0.2376 0.3483 0.059 Uiso 1 1 calc R . .
C27 C 0.0217(6) 0.1350(2) 0.2863(2) 0.0237(12) Uani 1 1 d . . .
C28 C -0.0656(6) 0.1197(3) 0.2144(2) 0.0324(14) Uani 1 1 d . . .
H28A H -0.0244 0.1433 0.1804 0.049 Uiso 1 1 calc R . .
H28B H -0.1759 0.1282 0.2118 0.049 Uiso 1 1 calc R . .
H28C H -0.0518 0.0779 0.2053 0.049 Uiso 1 1 calc R . .
C29 C -0.0229(7) 0.1969(2) 0.3054(3) 0.0383(15) Uani 1 1 d . . .
H29A H 0.0373 0.2076 0.3497 0.057 Uiso 1 1 calc R . .
H29B H -0.1334 0.1980 0.3080 0.057 Uiso 1 1 calc R . .
H29C H -0.0012 0.2248 0.2708 0.057 Uiso 1 1 calc R . .
C30 C -0.0364(6) 0.0933(3) 0.3375(3) 0.0358(15) Uani 1 1 d . . .
H30A H -0.1484 0.0979 0.3344 0.054 Uiso 1 1 calc R . .
H30B H 0.0151 0.1029 0.3838 0.054 Uiso 1 1 calc R . .
H30C H -0.0127 0.0527 0.3269 0.054 Uiso 1 1 calc R . .
C31 C 0.5173(6) 0.1484(2) 0.4834(2) 0.0226(13) Uani 1 1 d . . .
C32 C 0.5554(7) 0.1482(2) 0.5551(3) 0.0319(15) Uani 1 1 d . . .
H32 H 0.4789 0.1372 0.5813 0.038 Uiso 1 1 calc R . .
C33 C 0.7019(7) 0.1636(3) 0.5885(3) 0.0402(16) Uani 1 1 d . . .
H33 H 0.7245 0.1623 0.6368 0.048 Uiso 1 1 calc R . .
C34 C 0.8144(7) 0.1806(3) 0.5524(3) 0.0481(18) Uani 1 1 d . . .
H34 H 0.9139 0.1919 0.5754 0.058 Uiso 1 1 calc R . .
C35 C 0.7809(7) 0.1811(3) 0.4825(3) 0.0494(18) Uani 1 1 d . . .
H35 H 0.8580 0.1927 0.4570 0.059 Uiso 1 1 calc R . .
C36 C 0.6364(6) 0.1649(3) 0.4489(3) 0.0354(15) Uani 1 1 d . . .
H36 H 0.6173 0.1650 0.4005 0.043 Uiso 1 1 calc R . .
C37 C 0.8294(6) -0.0331(2) 0.5019(3) 0.0303(14) Uani 1 1 d . . .
C38 C 0.7537(8) -0.0016(3) 0.4373(3) 0.057(2) Uani 1 1 d . . .
H38A H 0.8190 0.0314 0.4281 0.085 Uiso 1 1 calc R . .
H38B H 0.6520 0.0131 0.4433 0.085 Uiso 1 1 calc R . .
H38C H 0.7415 -0.0291 0.3989 0.085 Uiso 1 1 calc R . .
C39 C 0.9936(7) -0.0516(3) 0.4875(4) 0.072(2) Uani 1 1 d . . .
H39A H 1.0487 -0.0733 0.5268 0.108 Uiso 1 1 calc R . .
H39B H 1.0526 -0.0164 0.4800 0.108 Uiso 1 1 calc R . .
H39C H 0.9817 -0.0766 0.4469 0.108 Uiso 1 1 calc R . .
C40 C 0.8575(11) 0.0090(3) 0.5609(3) 0.088(3) Uani 1 1 d . . .
H40A H 0.7584 0.0242 0.5699 0.132 Uiso 1 1 calc R . .
H40B H 0.9214 0.0418 0.5498 0.132 Uiso 1 1 calc R . .
H40C H 0.9112 -0.0113 0.6015 0.132 Uiso 1 1 calc R . .
C41 C 0.7548(8) -0.1642(3) 0.4699(3) 0.0436(16) Uani 1 1 d U . .
C42 C 0.9138(9) -0.1882(4) 0.4882(4) 0.093(3) Uani 1 1 d U . .
H42A H 0.9890 -0.1578 0.4815 0.140 Uiso 1 1 calc R . .
H42B H 0.9256 -0.2220 0.4590 0.140 Uiso 1 1 calc R . .
H42C H 0.9318 -0.2006 0.5360 0.140 Uiso 1 1 calc R . .
C43 C 0.7208(7) -0.1517(3) 0.3932(3) 0.0531(18) Uani 1 1 d U . .
H43A H 0.7397 -0.1872 0.3681 0.080 Uiso 1 1 calc R . .
H43B H 0.7884 -0.1200 0.3824 0.080 Uiso 1 1 calc R . .
H43C H 0.6125 -0.1397 0.3800 0.080 Uiso 1 1 calc R . .
C44 C 0.6341(10) -0.2138(3) 0.4793(4) 0.091(3) Uani 1 1 d U . .
H44A H 0.6374 -0.2447 0.4453 0.136 Uiso 1 1 calc R . .
H44B H 0.5299 -0.1969 0.4732 0.136 Uiso 1 1 calc R . .
H44C H 0.6602 -0.2306 0.5251 0.136 Uiso 1 1 calc R . .
C45 C 0.5122(6) -0.0850(3) 0.5183(3) 0.0424(16) Uani 1 1 d U . .
C46 C 0.4224(6) -0.0787(3) 0.4456(3) 0.0496(19) Uani 1 1 d U . .
H46A H 0.3173 -0.0650 0.4473 0.074 Uiso 1 1 calc R . .
H46B H 0.4175 -0.1169 0.4226 0.074 Uiso 1 1 calc R . .
H46C H 0.4748 -0.0503 0.4204 0.074 Uiso 1 1 calc R . .
C47 C 0.4384(8) -0.1289(4) 0.5582(4) 0.092(3) Uani 1 1 d U . .
H47A H 0.4241 -0.1660 0.5330 0.138 Uiso 1 1 calc R . .
H47B H 0.3377 -0.1141 0.5656 0.138 Uiso 1 1 calc R . .
H47C H 0.5050 -0.1355 0.6023 0.138 Uiso 1 1 calc R . .
C48 C 0.4926(8) -0.0245(4) 0.5536(3) 0.080(3) Uani 1 1 d U . .
H48A H 0.5509 -0.0250 0.6002 0.120 Uiso 1 1 calc R . .
H48B H 0.3829 -0.0177 0.5550 0.120 Uiso 1 1 calc R . .
H48C H 0.5319 0.0071 0.5277 0.120 Uiso 1 1 calc R . .
C49 C 0.9959(6) -0.1327(2) 0.7125(3) 0.0217(12) Uani 1 1 d . . .
C50 C 1.0238(6) -0.1369(2) 0.7847(3) 0.0244(13) Uani 1 1 d . . .
H50 H 0.9430 -0.1284 0.8095 0.029 Uiso 1 1 calc R . .
C51 C 1.1682(7) -0.1534(2) 0.8193(3) 0.0307(14) Uani 1 1 d . . .
H51 H 1.1859 -0.1554 0.8676 0.037 Uiso 1 1 calc R . .
C52 C 1.2866(6) -0.1668(2) 0.7843(3) 0.0292(14) Uani 1 1 d . . .
H52 H 1.3843 -0.1787 0.8086 0.035 Uiso 1 1 calc R . .
C53 C 1.2632(6) -0.1630(2) 0.7137(3) 0.0313(14) Uani 1 1 d . . .
H53 H 1.3448 -0.1716 0.6895 0.038 Uiso 1 1 calc R . .
C54 C 1.1177(6) -0.1465(2) 0.6790(3) 0.0283(13) Uani 1 1 d . . .
H54 H 1.1014 -0.1446 0.6306 0.034 Uiso 1 1 calc R . .
C59 C 0.7645(6) 0.6787(2) 0.2328(3) 0.0324(14) Uani 1 1 d . . .
C60 C 0.8897(7) 0.6823(3) 0.2978(3) 0.056(2) Uani 1 1 d . . .
H60A H 0.8859 0.7211 0.3188 0.084 Uiso 1 1 calc R . .
H60B H 0.9921 0.6762 0.2855 0.084 Uiso 1 1 calc R . .
H60C H 0.8703 0.6519 0.3301 0.084 Uiso 1 1 calc R . .
C61 C 0.7993(8) 0.7254(2) 0.1814(3) 0.056(2) Uani 1 1 d . . .
H61A H 0.8987 0.7166 0.1674 0.084 Uiso 1 1 calc R . .
H61B H 0.8042 0.7643 0.2028 0.084 Uiso 1 1 calc R . .
H61C H 0.7172 0.7251 0.1413 0.084 Uiso 1 1 calc R . .
C62 C 0.6082(7) 0.6973(3) 0.2523(3) 0.0470(18) Uani 1 1 d . . .
H62A H 0.6155 0.7379 0.2688 0.071 Uiso 1 1 calc R . .
H62B H 0.5837 0.6714 0.2883 0.071 Uiso 1 1 calc R . .
H62C H 0.5266 0.6944 0.2122 0.071 Uiso 1 1 calc R . .
C63 C 0.6359(6) 0.5520(2) 0.2366(3) 0.0267(13) Uani 1 1 d . . .
C64 C 0.6884(7) 0.5526(3) 0.3145(3) 0.0480(18) Uani 1 1 d . . .
H64A H 0.7981 0.5421 0.3253 0.072 Uiso 1 1 calc R . .
H64B H 0.6272 0.5241 0.3355 0.072 Uiso 1 1 calc R . .
H64C H 0.6731 0.5919 0.3321 0.072 Uiso 1 1 calc R . .
C65 C 0.4618(6) 0.5667(3) 0.2199(3) 0.0375(15) Uani 1 1 d . . .
H65A H 0.4429 0.6046 0.2403 0.056 Uiso 1 1 calc R . .
H65B H 0.4026 0.5360 0.2384 0.056 Uiso 1 1 calc R . .
H65C H 0.4296 0.5688 0.1704 0.056 Uiso 1 1 calc R . .
C66 C 0.6495(7) 0.4889(2) 0.2110(3) 0.0447(17) Uani 1 1 d . . .
H66A H 0.5807 0.4631 0.2316 0.067 Uiso 1 1 calc R . .
H66B H 0.7565 0.4753 0.2238 0.067 Uiso 1 1 calc R . .
H66C H 0.6199 0.4879 0.1613 0.067 Uiso 1 1 calc R . .
C67 C 0.9437(6) 0.5738(3) 0.1867(3) 0.0321(14) Uani 1 1 d . . .
C68 C 1.0279(6) 0.5478(3) 0.2547(3) 0.0403(16) Uani 1 1 d . . .
H68A H 1.0404 0.5783 0.2899 0.060 Uiso 1 1 calc R . .
H68B H 1.1298 0.5332 0.2487 0.060 Uiso 1 1 calc R . .
H68C H 0.9668 0.5153 0.2686 0.060 Uiso 1 1 calc R . .
C69 C 1.0449(6) 0.6207(3) 0.1618(3) 0.0506(18) Uani 1 1 d . . .
H69A H 1.1403 0.6027 0.1523 0.076 Uiso 1 1 calc R . .
H69B H 1.0704 0.6509 0.1969 0.076 Uiso 1 1 calc R . .
H69C H 0.9889 0.6387 0.1201 0.076 Uiso 1 1 calc R . .
C70 C 0.9276(7) 0.5236(3) 0.1322(3) 0.0442(17) Uani 1 1 d . . .
H70A H 1.0306 0.5097 0.1269 0.066 Uiso 1 1 calc R . .
H70B H 0.8735 0.5386 0.0885 0.066 Uiso 1 1 calc R . .
H70C H 0.8685 0.4910 0.1472 0.066 Uiso 1 1 calc R . .
C71 C 0.4707(6) 0.6657(2) 0.0155(2) 0.0200(12) Uani 1 1 d . . .
C72 C 0.3489(6) 0.6746(2) 0.0513(3) 0.0229(12) Uani 1 1 d . . .
H72 H 0.3612 0.6630 0.0977 0.027 Uiso 1 1 calc R . .
C73 C 0.2098(7) 0.7001(2) 0.0210(3) 0.0321(14) Uani 1 1 d . . .
H73 H 0.1282 0.7049 0.0464 0.038 Uiso 1 1 calc R . .
C74 C 0.1906(7) 0.7185(2) -0.0461(3) 0.0336(15) Uani 1 1 d . . .
H74 H 0.0963 0.7363 -0.0667 0.040 Uiso 1 1 calc R . .
C75 C 0.3082(7) 0.7110(2) -0.0827(3) 0.0287(14) Uani 1 1 d . . .
H75 H 0.2946 0.7231 -0.1290 0.034 Uiso 1 1 calc R . .
C76 C 0.4469(7) 0.6857(2) -0.0525(3) 0.0274(13) Uani 1 1 d . . .
H76 H 0.5279 0.6816 -0.0784 0.033 Uiso 1 1 calc R . .
N1 N 0.8172(5) 0.88836(16) 1.12055(19) 0.0196(10) Uani 1 1 d . . .
N2 N 0.3183(5) 0.1307(2) 0.3737(2) 0.0280(11) Uani 1 1 d . . .
N3 N 0.8023(5) -0.11659(18) 0.6006(2) 0.0265(11) Uani 1 1 d . . .
N4 N 0.6456(5) 0.61555(17) 0.11747(19) 0.0226(10) Uani 1 1 d . . .
B1 B 0.8807(7) 0.8932(2) 1.1875(3) 0.0217(15) Uani 1 1 d . . .
B2 B 0.3552(7) 0.1321(3) 0.4420(3) 0.0221(14) Uani 1 1 d . . .
B3 B 0.8369(8) -0.1141(3) 0.6698(3) 0.0292(16) Uani 1 1 d . . .
B4 B 0.6236(7) 0.6355(3) 0.0522(3) 0.0226(14) Uani 1 1 d . . .
P1 P 0.71021(15) 0.90943(6) 1.05316(6) 0.0190(3) Uani 1 1 d . . .
P2 P 0.24032(15) 0.12953(6) 0.29693(6) 0.0188(3) Uani 1 1 d . . .
P3 P 0.72488(15) -0.10018(6) 0.52619(7) 0.0221(3) Uani 1 1 d . . .
P4 P 0.74577(15) 0.60486(6) 0.18995(6) 0.0181(3) Uani 1 1 d . . .
Cl1 Cl 0.80405(17) 0.94412(6) 1.24678(7) 0.0342(4) Uani 1 1 d . . .
Cl2 Cl 0.20932(18) 0.11663(9) 0.49728(7) 0.0576(6) Uani 1 1 d . . .
Cl3 Cl 0.69334(16) -0.08719(7) 0.72172(7) 0.0368(4) Uani 1 1 d . . .
Cl4 Cl 0.77149(18) 0.62548(8) -0.00284(7) 0.0510(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
C1 C2 1.531(7) . ?
C1 C3 1.548(7) . ?
C1 C4 1.561(7) . ?
C1 P1 1.898(5) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C7 1.545(7) . ?
C5 C8 1.551(7) . ?
C5 C6 1.552(7) . ?
C5 P1 1.870(5) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C12 1.545(7) . ?
C9 C10 1.551(7) . ?
C9 C11 1.553(7) . ?
C9 P1 1.883(5) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.398(7) . ?
C13 C18 1.403(7) . ?
C13 B1 1.566(8) . ?
C14 C15 1.388(8) . ?
C14 H14 0.9500 . ?
C15 C16 1.385(8) . ?
C15 H15 0.9500 . ?
C16 C17 1.374(8) . ?
C16 H16 0.9500 . ?
C17 C18 1.379(7) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C21 1.532(7) . ?
C19 C20 1.533(7) . ?
C19 C22 1.568(7) . ?
C19 P2 1.885(5) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C25 1.535(7) . ?
C23 C26 1.555(7) . ?
C23 C24 1.558(7) . ?
C23 P2 1.888(5) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C29 1.527(7) . ?
C27 C30 1.543(7) . ?
C27 C28 1.545(6) . ?
C27 P2 1.898(5) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C36 1.396(7) . ?
C31 C32 1.412(7) . ?
C31 B2 1.563(8) . ?
C32 C33 1.388(7) . ?
C32 H32 0.9500 . ?
C33 C34 1.373(8) . ?
C33 H33 0.9500 . ?
C34 C35 1.372(7) . ?
C34 H34 0.9500 . ?
C35 C36 1.379(7) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C40 1.505(8) . ?
C37 C38 1.524(7) . ?
C37 C39 1.573(8) . ?
C37 P3 1.886(5) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C42 1.486(9) . ?
C41 C43 1.534(8) . ?
C41 C44 1.582(9) . ?
C41 P3 1.884(6) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C47 1.493(9) . ?
C45 C46 1.533(7) . ?
C45 C48 1.571(9) . ?
C45 P3 1.878(6) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 C54 1.390(7) . ?
C49 C50 1.420(6) . ?
C49 B3 1.564(8) . ?
C50 C51 1.387(7) . ?
C50 H50 0.9500 . ?
C51 C52 1.379(7) . ?
C51 H51 0.9500 . ?
C52 C53 1.388(7) . ?
C52 H52 0.9500 . ?
C53 C54 1.397(7) . ?
C53 H53 0.9500 . ?
C54 H54 0.9500 . ?
C59 C61 1.543(8) . ?
C59 C62 1.547(8) . ?
C59 C60 1.552(7) . ?
C59 P4 1.879(6) . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 C66 1.536(8) . ?
C63 C64 1.542(7) . ?
C63 C65 1.543(7) . ?
C63 P4 1.883(5) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 C69 1.525(7) . ?
C67 C68 1.546(7) . ?
C67 C70 1.567(8) . ?
C67 P4 1.887(5) . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C69 H69A 0.9800 . ?
C69 H69B 0.9800 . ?
C69 H69C 0.9800 . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
C71 C72 1.397(7) . ?
C71 C76 1.411(7) . ?
C71 B4 1.573(8) . ?
C72 C73 1.393(7) . ?
C72 H72 0.9500 . ?
C73 C74 1.382(7) . ?
C73 H73 0.9500 . ?
C74 C75 1.372(7) . ?
C74 H74 0.9500 . ?
C75 C76 1.388(7) . ?
C75 H75 0.9500 . ?
C76 H76 0.9500 . ?
N1 B1 1.359(7) . ?
N1 P1 1.576(4) . ?
N2 B2 1.345(7) . ?
N2 P2 1.566(4) . ?
N3 B3 1.361(7) . ?
N3 P3 1.567(4) . ?
N4 B4 1.359(6) . ?
N4 P4 1.576(4) . ?
B1 Cl1 1.860(6) . ?
B2 Cl2 1.858(6) . ?
B3 Cl3 1.864(6) . ?
B4 Cl4 1.850(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C3 109.5(4) . . ?
C2 C1 C4 108.8(4) . . ?
C3 C1 C4 105.8(4) . . ?
C2 C1 P1 115.0(4) . . ?
C3 C1 P1 108.9(3) . . ?
C4 C1 P1 108.6(3) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C7 C5 C8 109.2(4) . . ?
C7 C5 C6 108.0(4) . . ?
C8 C5 C6 102.9(4) . . ?
C7 C5 P1 114.9(4) . . ?
C8 C5 P1 109.0(4) . . ?
C6 C5 P1 112.1(4) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C12 C9 C10 107.7(4) . . ?
C12 C9 C11 105.7(4) . . ?
C10 C9 C11 108.0(4) . . ?
C12 C9 P1 109.7(4) . . ?
C10 C9 P1 114.5(3) . . ?
C11 C9 P1 110.8(3) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C18 115.2(5) . . ?
C14 C13 B1 124.5(5) . . ?
C18 C13 B1 120.2(5) . . ?
C15 C14 C13 122.8(6) . . ?
C15 C14 H14 118.6 . . ?
C13 C14 H14 118.6 . . ?
C16 C15 C14 119.5(5) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
C17 C16 C15 119.6(6) . . ?
C17 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C16 C17 C18 120.1(6) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C17 C18 C13 122.7(5) . . ?
C17 C18 H18 118.6 . . ?
C13 C18 H18 118.6 . . ?
C21 C19 C20 106.8(4) . . ?
C21 C19 C22 109.4(5) . . ?
C20 C19 C22 109.0(5) . . ?
C21 C19 P2 109.7(4) . . ?
C20 C19 P2 109.5(4) . . ?
C22 C19 P2 112.2(4) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C25 C23 C26 106.1(4) . . ?
C25 C23 C24 107.8(4) . . ?
C26 C23 C24 108.5(4) . . ?
C25 C23 P2 110.8(4) . . ?
C26 C23 P2 108.5(4) . . ?
C24 C23 P2 114.8(4) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C29 C27 C30 106.0(4) . . ?
C29 C27 C28 109.4(4) . . ?
C30 C27 C28 107.9(4) . . ?
C29 C27 P2 109.3(4) . . ?
C30 C27 P2 109.1(3) . . ?
C28 C27 P2 114.9(3) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C36 C31 C32 115.5(5) . . ?
C36 C31 B2 119.7(5) . . ?
C32 C31 B2 124.8(5) . . ?
C33 C32 C31 121.6(5) . . ?
C33 C32 H32 119.2 . . ?
C31 C32 H32 119.2 . . ?
C34 C33 C32 120.7(5) . . ?
C34 C33 H33 119.6 . . ?
C32 C33 H33 119.6 . . ?
C35 C34 C33 119.0(6) . . ?
C35 C34 H34 120.5 . . ?
C33 C34 H34 120.5 . . ?
C34 C35 C36 120.7(6) . . ?
C34 C35 H35 119.6 . . ?
C36 C35 H35 119.6 . . ?
C35 C36 C31 122.4(5) . . ?
C35 C36 H36 118.8 . . ?
C31 C36 H36 118.8 . . ?
C40 C37 C38 110.5(5) . . ?
C40 C37 C39 106.2(6) . . ?
C38 C37 C39 104.7(5) . . ?
C40 C37 P3 109.8(4) . . ?
C38 C37 P3 115.9(4) . . ?
C39 C37 P3 109.3(4) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C41 C43 109.1(5) . . ?
C42 C41 C44 109.1(6) . . ?
C43 C41 C44 103.3(5) . . ?
C42 C41 P3 111.0(5) . . ?
C43 C41 P3 115.2(4) . . ?
C44 C41 P3 108.7(4) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C47 C45 C46 111.4(5) . . ?
C47 C45 C48 105.0(6) . . ?
C46 C45 C48 105.3(5) . . ?
C47 C45 P3 110.3(5) . . ?
C46 C45 P3 116.2(4) . . ?
C48 C45 P3 107.9(4) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C45 C47 H47A 109.5 . . ?
C45 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C45 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C45 C48 H48A 109.5 . . ?
C45 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C45 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C54 C49 C50 117.2(5) . . ?
C54 C49 B3 119.2(5) . . ?
C50 C49 B3 123.6(5) . . ?
C51 C50 C49 120.5(5) . . ?
C51 C50 H50 119.8 . . ?
C49 C50 H50 119.8 . . ?
C52 C51 C50 120.8(5) . . ?
C52 C51 H51 119.6 . . ?
C50 C51 H51 119.6 . . ?
C51 C52 C53 120.2(5) . . ?
C51 C52 H52 119.9 . . ?
C53 C52 H52 119.9 . . ?
C52 C53 C54 119.0(5) . . ?
C52 C53 H53 120.5 . . ?
C54 C53 H53 120.5 . . ?
C49 C54 C53 122.4(5) . . ?
C49 C54 H54 118.8 . . ?
C53 C54 H54 118.8 . . ?
C61 C59 C62 105.2(5) . . ?
C61 C59 C60 108.9(5) . . ?
C62 C59 C60 107.9(5) . . ?
C61 C59 P4 109.2(4) . . ?
C62 C59 P4 110.3(4) . . ?
C60 C59 P4 114.9(4) . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C59 C61 H61A 109.5 . . ?
C59 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C59 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C59 C62 H62A 109.5 . . ?
C59 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C59 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C66 C63 C64 108.4(5) . . ?
C66 C63 C65 105.2(5) . . ?
C64 C63 C65 109.3(5) . . ?
C66 C63 P4 111.1(4) . . ?
C64 C63 P4 113.6(4) . . ?
C65 C63 P4 109.0(3) . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C63 C65 H65A 109.5 . . ?
C63 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C63 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C63 C66 H66A 109.5 . . ?
C63 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C63 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C69 C67 C68 109.6(5) . . ?
C69 C67 C70 106.0(4) . . ?
C68 C67 C70 107.5(5) . . ?
C69 C67 P4 109.8(4) . . ?
C68 C67 P4 114.8(4) . . ?
C70 C67 P4 108.8(4) . . ?
C67 C68 H68A 109.5 . . ?
C67 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C67 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C67 C69 H69A 109.5 . . ?
C67 C69 H69B 109.5 . . ?
H69A C69 H69B 109.5 . . ?
C67 C69 H69C 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
C67 C70 H70A 109.5 . . ?
C67 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
C67 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C72 C71 C76 116.2(5) . . ?
C72 C71 B4 119.6(4) . . ?
C76 C71 B4 124.2(5) . . ?
C73 C72 C71 122.0(5) . . ?
C73 C72 H72 119.0 . . ?
C71 C72 H72 119.0 . . ?
C74 C73 C72 119.9(5) . . ?
C74 C73 H73 120.0 . . ?
C72 C73 H73 120.0 . . ?
C75 C74 C73 119.8(5) . . ?
C75 C74 H74 120.1 . . ?
C73 C74 H74 120.1 . . ?
C74 C75 C76 120.3(5) . . ?
C74 C75 H75 119.8 . . ?
C76 C75 H75 119.8 . . ?
C75 C76 C71 121.7(5) . . ?
C75 C76 H76 119.2 . . ?
C71 C76 H76 119.2 . . ?
B1 N1 P1 153.7(4) . . ?
B2 N2 P2 168.2(4) . . ?
B3 N3 P3 159.1(4) . . ?
B4 N4 P4 153.4(4) . . ?
N1 B1 C13 123.8(5) . . ?
N1 B1 Cl1 122.7(4) . . ?
C13 B1 Cl1 113.5(4) . . ?
N2 B2 C31 125.4(5) . . ?
N2 B2 Cl2 121.6(4) . . ?
C31 B2 Cl2 113.0(4) . . ?
N3 B3 C49 124.4(5) . . ?
N3 B3 Cl3 121.3(5) . . ?
C49 B3 Cl3 114.3(4) . . ?
N4 B4 C71 124.2(5) . . ?
N4 B4 Cl4 121.7(4) . . ?
C71 B4 Cl4 114.1(4) . . ?
N1 P1 C5 111.2(2) . . ?
N1 P1 C9 109.5(2) . . ?
C5 P1 C9 110.8(2) . . ?
N1 P1 C1 105.5(2) . . ?
C5 P1 C1 109.4(2) . . ?
C9 P1 C1 110.3(2) . . ?
N2 P2 C19 107.4(2) . . ?
N2 P2 C23 106.9(2) . . ?
C19 P2 C23 110.3(2) . . ?
N2 P2 C27 112.0(2) . . ?
C19 P2 C27 110.9(2) . . ?
C23 P2 C27 109.3(2) . . ?
N3 P3 C45 112.9(2) . . ?
N3 P3 C41 107.2(3) . . ?
C45 P3 C41 109.2(3) . . ?
N3 P3 C37 106.5(2) . . ?
C45 P3 C37 110.4(3) . . ?
C41 P3 C37 110.6(3) . . ?
N4 P4 C59 105.6(2) . . ?
N4 P4 C63 107.3(2) . . ?
C59 P4 C63 111.2(3) . . ?
N4 P4 C67 113.6(2) . . ?
C59 P4 C67 109.9(3) . . ?
C63 P4 C67 109.2(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C18 C13 C14 C15 -2.8(8) . . . . ?
B1 C13 C14 C15 174.6(5) . . . . ?
C13 C14 C15 C16 3.0(9) . . . . ?
C14 C15 C16 C17 -1.1(9) . . . . ?
C15 C16 C17 C18 -0.7(10) . . . . ?
C16 C17 C18 C13 0.8(9) . . . . ?
C14 C13 C18 C17 0.9(8) . . . . ?
B1 C13 C18 C17 -176.6(5) . . . . ?
C36 C31 C32 C33 0.1(8) . . . . ?
B2 C31 C32 C33 -179.7(5) . . . . ?
C31 C32 C33 C34 1.2(9) . . . . ?
C32 C33 C34 C35 -1.3(10) . . . . ?
C33 C34 C35 C36 0.2(10) . . . . ?
C34 C35 C36 C31 1.2(10) . . . . ?
C32 C31 C36 C35 -1.3(8) . . . . ?
B2 C31 C36 C35 178.5(6) . . . . ?
C54 C49 C50 C51 1.0(7) . . . . ?
B3 C49 C50 C51 -179.6(5) . . . . ?
C49 C50 C51 C52 -1.1(8) . . . . ?
C50 C51 C52 C53 1.2(8) . . . . ?
C51 C52 C53 C54 -1.1(8) . . . . ?
C50 C49 C54 C53 -1.0(8) . . . . ?
B3 C49 C54 C53 179.6(5) . . . . ?
C52 C53 C54 C49 1.1(9) . . . . ?
C76 C71 C72 C73 1.9(7) . . . . ?
B4 C71 C72 C73 -178.7(5) . . . . ?
C71 C72 C73 C74 -1.3(8) . . . . ?
C72 C73 C74 C75 0.7(8) . . . . ?
C73 C74 C75 C76 -0.8(9) . . . . ?
C74 C75 C76 C71 1.5(8) . . . . ?
C72 C71 C76 C75 -2.0(7) . . . . ?
B4 C71 C76 C75 178.6(5) . . . . ?
P1 N1 B1 C13 -165.1(6) . . . . ?
P1 N1 B1 Cl1 14.7(11) . . . . ?
C14 C13 B1 N1 -163.1(5) . . . . ?
C18 C13 B1 N1 14.2(8) . . . . ?
C14 C13 B1 Cl1 17.1(7) . . . . ?
C18 C13 B1 Cl1 -165.7(4) . . . . ?
P2 N2 B2 C31 -162.2(19) . . . . ?
P2 N2 B2 Cl2 15(3) . . . . ?
C36 C31 B2 N2 2.0(9) . . . . ?
C32 C31 B2 N2 -178.3(5) . . . . ?
C36 C31 B2 Cl2 -175.9(4) . . . . ?
C32 C31 B2 Cl2 3.9(7) . . . . ?
P3 N3 B3 C49 -149.9(9) . . . . ?
P3 N3 B3 Cl3 29.8(15) . . . . ?
C54 C49 B3 N3 7.6(9) . . . . ?
C50 C49 B3 N3 -171.8(5) . . . . ?
C54 C49 B3 Cl3 -172.0(4) . . . . ?
C50 C49 B3 Cl3 8.6(7) . . . . ?
P4 N4 B4 C71 -141.3(7) . . . . ?
P4 N4 B4 Cl4 41.8(11) . . . . ?
C72 C71 B4 N4 1.5(8) . . . . ?
C76 C71 B4 N4 -179.0(5) . . . . ?
C72 C71 B4 Cl4 178.7(4) . . . . ?
C76 C71 B4 Cl4 -1.9(7) . . . . ?
B1 N1 P1 C5 -73.7(9) . . . . ?
B1 N1 P1 C9 49.1(9) . . . . ?
B1 N1 P1 C1 167.8(8) . . . . ?
C7 C5 P1 N1 165.3(4) . . . . ?
C8 C5 P1 N1 42.3(4) . . . . ?
C6 C5 P1 N1 -70.9(4) . . . . ?
C7 C5 P1 C9 43.2(4) . . . . ?
C8 C5 P1 C9 -79.7(4) . . . . ?
C6 C5 P1 C9 167.1(4) . . . . ?
C7 C5 P1 C1 -78.6(4) . . . . ?
C8 C5 P1 C1 158.5(4) . . . . ?
C6 C5 P1 C1 45.2(4) . . . . ?
C12 C9 P1 N1 38.1(4) . . . . ?
C10 C9 P1 N1 159.3(4) . . . . ?
C11 C9 P1 N1 -78.2(4) . . . . ?
C12 C9 P1 C5 161.1(3) . . . . ?
C10 C9 P1 C5 -77.7(4) . . . . ?
C11 C9 P1 C5 44.8(4) . . . . ?
C12 C9 P1 C1 -77.6(4) . . . . ?
C10 C9 P1 C1 43.6(4) . . . . ?
C11 C9 P1 C1 166.1(3) . . . . ?
C2 C1 P1 N1 165.9(4) . . . . ?
C3 C1 P1 N1 -70.9(4) . . . . ?
C4 C1 P1 N1 43.9(4) . . . . ?
C2 C1 P1 C5 46.2(5) . . . . ?
C3 C1 P1 C5 169.4(3) . . . . ?
C4 C1 P1 C5 -75.9(4) . . . . ?
C2 C1 P1 C9 -75.9(5) . . . . ?
C3 C1 P1 C9 47.3(4) . . . . ?
C4 C1 P1 C9 162.0(4) . . . . ?
B2 N2 P2 C19 -119(2) . . . . ?
B2 N2 P2 C23 122(2) . . . . ?
B2 N2 P2 C27 2(2) . . . . ?
C21 C19 P2 N2 -40.8(4) . . . . ?
C20 C19 P2 N2 76.1(4) . . . . ?
C22 C19 P2 N2 -162.6(4) . . . . ?
C21 C19 P2 C23 75.3(4) . . . . ?
C20 C19 P2 C23 -167.8(4) . . . . ?
C22 C19 P2 C23 -46.5(4) . . . . ?
C21 C19 P2 C27 -163.4(4) . . . . ?
C20 C19 P2 C27 -46.5(4) . . . . ?
C22 C19 P2 C27 74.8(4) . . . . ?
C25 C23 P2 N2 75.0(4) . . . . ?
C26 C23 P2 N2 -41.0(4) . . . . ?
C24 C23 P2 N2 -162.6(4) . . . . ?
C25 C23 P2 C19 -41.4(4) . . . . ?
C26 C23 P2 C19 -157.5(4) . . . . ?
C24 C23 P2 C19 80.9(4) . . . . ?
C25 C23 P2 C27 -163.6(3) . . . . ?
C26 C23 P2 C27 80.3(4) . . . . ?
C24 C23 P2 C27 -41.3(4) . . . . ?
C29 C27 P2 N2 70.4(4) . . . . ?
C30 C27 P2 N2 -45.1(4) . . . . ?
C28 C27 P2 N2 -166.3(4) . . . . ?
C29 C27 P2 C19 -169.7(4) . . . . ?
C30 C27 P2 C19 74.8(4) . . . . ?
C28 C27 P2 C19 -46.4(5) . . . . ?
C29 C27 P2 C23 -47.8(4) . . . . ?
C30 C27 P2 C23 -163.3(4) . . . . ?
C28 C27 P2 C23 75.5(4) . . . . ?
B3 N3 P3 C45 -43.7(13) . . . . ?
B3 N3 P3 C41 -164.0(12) . . . . ?
B3 N3 P3 C37 77.6(12) . . . . ?
C47 C45 P3 N3 -42.1(6) . . . . ?
C46 C45 P3 N3 -170.2(5) . . . . ?
C48 C45 P3 N3 72.0(5) . . . . ?
C47 C45 P3 C41 77.0(5) . . . . ?
C46 C45 P3 C41 -51.0(6) . . . . ?
C48 C45 P3 C41 -168.8(4) . . . . ?
C47 C45 P3 C37 -161.2(5) . . . . ?
C46 C45 P3 C37 70.8(6) . . . . ?
C48 C45 P3 C37 -47.0(5) . . . . ?
C42 C41 P3 N3 -41.9(6) . . . . ?
C43 C41 P3 N3 -166.6(4) . . . . ?
C44 C41 P3 N3 78.2(5) . . . . ?
C42 C41 P3 C45 -164.4(5) . . . . ?
C43 C41 P3 C45 70.9(5) . . . . ?
C44 C41 P3 C45 -44.4(5) . . . . ?
C42 C41 P3 C37 73.9(6) . . . . ?
C43 C41 P3 C37 -50.8(5) . . . . ?
C44 C41 P3 C37 -166.1(4) . . . . ?
C40 C37 P3 N3 -42.1(5) . . . . ?
C38 C37 P3 N3 -168.0(4) . . . . ?
C39 C37 P3 N3 74.0(4) . . . . ?
C40 C37 P3 C45 80.8(5) . . . . ?
C38 C37 P3 C45 -45.2(5) . . . . ?
C39 C37 P3 C45 -163.1(4) . . . . ?
C40 C37 P3 C41 -158.2(5) . . . . ?
C38 C37 P3 C41 75.8(5) . . . . ?
C39 C37 P3 C41 -42.1(5) . . . . ?
B4 N4 P4 C59 74.1(9) . . . . ?
B4 N4 P4 C63 -167.3(9) . . . . ?
B4 N4 P4 C67 -46.5(10) . . . . ?
C61 C59 P4 N4 -43.5(4) . . . . ?
C62 C59 P4 N4 71.6(4) . . . . ?
C60 C59 P4 N4 -166.2(4) . . . . ?
C61 C59 P4 C63 -159.6(4) . . . . ?
C62 C59 P4 C63 -44.5(4) . . . . ?
C60 C59 P4 C63 77.7(5) . . . . ?
C61 C59 P4 C67 79.4(4) . . . . ?
C62 C59 P4 C67 -165.5(4) . . . . ?
C60 C59 P4 C67 -43.3(5) . . . . ?
C66 C63 P4 N4 76.8(4) . . . . ?
C64 C63 P4 N4 -160.8(4) . . . . ?
C65 C63 P4 N4 -38.6(4) . . . . ?
C66 C63 P4 C59 -168.2(4) . . . . ?
C64 C63 P4 C59 -45.7(5) . . . . ?
C65 C63 P4 C59 76.4(4) . . . . ?
C66 C63 P4 C67 -46.7(4) . . . . ?
C64 C63 P4 C67 75.7(4) . . . . ?
C65 C63 P4 C67 -162.2(4) . . . . ?
C69 C67 P4 N4 71.2(5) . . . . ?
C68 C67 P4 N4 -164.7(4) . . . . ?
C70 C67 P4 N4 -44.3(4) . . . . ?
C69 C67 P4 C59 -46.9(4) . . . . ?
C68 C67 P4 C59 77.2(5) . . . . ?
C70 C67 P4 C59 -162.4(4) . . . . ?
C69 C67 P4 C63 -169.0(4) . . . . ?
C68 C67 P4 C63 -45.0(5) . . . . ?
C70 C67 P4 C63 75.4(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.46
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.076
_database_code_depnum_ccdc_archive 'CCDC 1018466'
#######################################################################
#
#                 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_7c

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H40 B2 Cl2 N2 P2'
_chemical_formula_sum            'C24 H40 B2 Cl2 N2 P2'
_chemical_formula_weight         511.04

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'


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                   10.1315(4)
_cell_length_b                   10.0647(4)
_cell_length_c                   13.7696(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.606(2)
_cell_angle_gamma                90.00
_cell_volume                     1391.74(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8389
_cell_measurement_theta_min      4.707
_cell_measurement_theta_max      54.914

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             536
_exptl_absorpt_coefficient_mu    0.362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6778
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
'SADABS. Area-Detector Integration Software. (Siemens Industrial Automation, 1995, Inc.: Madison, WI)'

_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  'Bruker Apex II CCD 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            12135
_diffrn_reflns_av_R_equivalents  0.0193
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.35
_diffrn_reflns_theta_max         27.47
_reflns_number_total             3182
_reflns_number_gt                2794
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'Bruker SMART. Area-Detector Software Package. (Siemens Industrial Automation, 1993, Inc.: Madison, WI)'
_computing_cell_refinement       
'Bruker SMART. Area-Detector Software Package. (Siemens Industrial Automation, 1993, Inc.: Madison, WI)'
_computing_data_reduction        
'Bruker SAINT. Area-Detector Integration Software. (Siemens Industrial Automation, 1995, Inc.: Madison, WI)'
_computing_structure_solution    
'SHELX-97. Programs for Crystal Structure Analysis. (G. M. Sheldrick, 1997, Release 97-2, University of Gttingen, Germany)'
_computing_structure_refinement  
'SHELX-97. Programs for Crystal Structure Analysis. (G. M. Sheldrick, 1997, Release 97-2, University of Gttingen, Germany)'
_computing_molecular_graphics    
'Ortep for Windows (L. J. Farrugia, J. Appl. Cryst. 1997, 30, 565)'
_computing_publication_material  
'WinGX v1.70.01 (L. J. Farrugia, J. Appl. Cryst. 1999, 32, 837)'

_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)+(0.0397P)²+0.5770P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3182
_refine_ls_number_parameters     148
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0289
_refine_ls_wR_factor_ref         0.0803
_refine_ls_wR_factor_gt          0.0762
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_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
C1 C -0.11869(12) 0.79890(12) 0.04696(9) 0.0195(3) Uani 1 1 d . . .
C2 C -0.17792(14) 0.85197(15) 0.12477(11) 0.0286(3) Uani 1 1 d . . .
H2 H -0.1677 0.9440 0.1390 0.034 Uiso 1 1 calc R . .
C3 C -0.25112(15) 0.77440(17) 0.18187(12) 0.0346(4) Uani 1 1 d . . .
H3 H -0.2892 0.8135 0.2345 0.041 Uiso 1 1 calc R . .
C4 C -0.26841(16) 0.64063(18) 0.16215(12) 0.0400(4) Uani 1 1 d . . .
H4 H -0.3202 0.5875 0.1999 0.048 Uiso 1 1 calc R . .
C5 C -0.2099(2) 0.58522(18) 0.08740(13) 0.0490(5) Uani 1 1 d . . .
H5 H -0.2201 0.4929 0.0742 0.059 Uiso 1 1 calc R . .
C6 C -0.13551(17) 0.66307(15) 0.03042(11) 0.0340(3) Uani 1 1 d . . .
H6 H -0.0955 0.6224 -0.0207 0.041 Uiso 1 1 calc R . .
C7 C 0.18263(14) 0.83858(16) 0.22448(11) 0.0323(3) Uani 1 1 d . . .
H7A H 0.1156 0.7673 0.2099 0.039 Uiso 1 1 calc R . .
H7B H 0.2649 0.7968 0.2577 0.039 Uiso 1 1 calc R . .
C8 C 0.13156(19) 0.9358(2) 0.29553(12) 0.0486(5) Uani 1 1 d . . .
H8A H 0.1997 1.0033 0.3149 0.073 Uiso 1 1 calc R . .
H8B H 0.1117 0.8878 0.3538 0.073 Uiso 1 1 calc R . .
H8C H 0.0504 0.9789 0.2637 0.073 Uiso 1 1 calc R . .
C9 C 0.33371(13) 1.04230(14) 0.13507(11) 0.0269(3) Uani 1 1 d . . .
H9A H 0.3599 1.0739 0.0723 0.032 Uiso 1 1 calc R . .
H9B H 0.2878 1.1165 0.1639 0.032 Uiso 1 1 calc R . .
C10 C 0.45999(15) 1.00828(19) 0.20433(14) 0.0428(4) Uani 1 1 d . . .
H10A H 0.4358 0.9797 0.2677 0.064 Uiso 1 1 calc R . .
H10B H 0.5173 1.0869 0.2137 0.064 Uiso 1 1 calc R . .
H10C H 0.5078 0.9364 0.1759 0.064 Uiso 1 1 calc R . .
C11 C 0.29852(15) 0.77197(15) 0.05537(12) 0.0337(3) Uani 1 1 d . . .
H11A H 0.3675 0.7341 0.1053 0.040 Uiso 1 1 calc R . .
H11B H 0.2316 0.7017 0.0368 0.040 Uiso 1 1 calc R . .
C12 C 0.36309(17) 0.80888(18) -0.03431(14) 0.0441(4) Uani 1 1 d . . .
H12A H 0.2957 0.8458 -0.0847 0.066 Uiso 1 1 calc R . .
H12B H 0.4024 0.7294 -0.0600 0.066 Uiso 1 1 calc R . .
H12C H 0.4328 0.8752 -0.0162 0.066 Uiso 1 1 calc R . .
N1 N 0.09232(10) 0.96285(10) 0.03982(7) 0.0173(2) Uani 1 1 d . . .
B1 B -0.03450(13) 0.89789(14) -0.01353(10) 0.0172(3) Uani 1 1 d . . .
P1 P 0.21829(3) 0.90796(3) 0.10994(2) 0.01998(10) Uani 1 1 d . . .
Cl1 Cl 0.00731(3) 0.80276(3) -0.13103(2) 0.02500(10) 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
C1 C6 1.3927(19) . ?
C1 C2 1.4013(19) . ?
C1 B1 1.6131(18) . ?
C2 C3 1.390(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.380(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.372(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.398(2) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.522(2) . ?
C7 P1 1.8046(15) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.5299(19) . ?
C9 P1 1.7911(14) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.518(2) . ?
C11 P1 1.8057(15) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N1 B1 1.5388(16) . ?
N1 B1 1.5436(17) 3_575 ?
N1 P1 1.5937(10) . ?
B1 N1 1.5436(17) 3_575 ?
B1 Cl1 1.9737(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 C1 C2 116.34(12) . . ?
C6 C1 B1 125.70(12) . . ?
C2 C1 B1 117.94(11) . . ?
C3 C2 C1 122.21(14) . . ?
C3 C2 H2 118.9 . . ?
C1 C2 H2 118.9 . . ?
C4 C3 C2 120.00(15) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C5 C4 C3 119.20(14) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C4 C5 C6 120.77(16) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C1 C6 C5 121.45(15) . . ?
C1 C6 H6 119.3 . . ?
C5 C6 H6 119.3 . . ?
C8 C7 P1 115.94(11) . . ?
C8 C7 H7A 108.3 . . ?
P1 C7 H7A 108.3 . . ?
C8 C7 H7B 108.3 . . ?
P1 C7 H7B 108.3 . . ?
H7A C7 H7B 107.4 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 P1 114.98(11) . . ?
C10 C9 H9A 108.5 . . ?
P1 C9 H9A 108.5 . . ?
C10 C9 H9B 108.5 . . ?
P1 C9 H9B 108.5 . . ?
H9A C9 H9B 107.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 P1 114.78(11) . . ?
C12 C11 H11A 108.6 . . ?
P1 C11 H11A 108.6 . . ?
C12 C11 H11B 108.6 . . ?
P1 C11 H11B 108.6 . . ?
H11A C11 H11B 107.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
B1 N1 B1 90.39(9) . 3_575 ?
B1 N1 P1 133.87(9) . . ?
B1 N1 P1 134.87(9) 3_575 . ?
N1 B1 N1 89.61(9) . 3_575 ?
N1 B1 C1 118.76(10) . . ?
N1 B1 C1 118.15(10) 3_575 . ?
N1 B1 Cl1 109.95(8) . . ?
N1 B1 Cl1 111.36(8) 3_575 . ?
C1 B1 Cl1 108.01(8) . . ?
N1 P1 C9 107.78(6) . . ?
N1 P1 C11 112.28(7) . . ?
C9 P1 C11 109.53(7) . . ?
N1 P1 C7 115.26(6) . . ?
C9 P1 C7 108.93(7) . . ?
C11 P1 C7 102.92(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -0.8(2) . . . . ?
B1 C1 C2 C3 -179.27(13) . . . . ?
C1 C2 C3 C4 -0.6(2) . . . . ?
C2 C3 C4 C5 1.6(2) . . . . ?
C3 C4 C5 C6 -1.1(3) . . . . ?
C2 C1 C6 C5 1.3(2) . . . . ?
B1 C1 C6 C5 179.59(15) . . . . ?
C4 C5 C6 C1 -0.3(3) . . . . ?
B1 N1 B1 N1 0.0 3_575 . . 3_575 ?
P1 N1 B1 N1 170.10(12) . . . 3_575 ?
B1 N1 B1 C1 -122.30(13) 3_575 . . . ?
P1 N1 B1 C1 47.80(16) . . . . ?
B1 N1 B1 Cl1 112.64(10) 3_575 . . . ?
P1 N1 B1 Cl1 -77.26(13) . . . . ?
C6 C1 B1 N1 -114.10(15) . . . . ?
C2 C1 B1 N1 64.18(16) . . . . ?
C6 C1 B1 N1 139.35(14) . . . 3_575 ?
C2 C1 B1 N1 -42.37(16) . . . 3_575 ?
C6 C1 B1 Cl1 11.88(16) . . . . ?
C2 C1 B1 Cl1 -169.83(10) . . . . ?
B1 N1 P1 C9 174.94(11) . . . . ?
B1 N1 P1 C9 -19.10(13) 3_575 . . . ?
B1 N1 P1 C11 54.22(13) . . . . ?
B1 N1 P1 C11 -139.82(12) 3_575 . . . ?
B1 N1 P1 C7 -63.19(13) . . . . ?
B1 N1 P1 C7 102.77(13) 3_575 . . . ?
C10 C9 P1 N1 178.32(11) . . . . ?
C10 C9 P1 C11 -59.25(14) . . . . ?
C10 C9 P1 C7 52.61(13) . . . . ?
C12 C11 P1 N1 66.14(13) . . . . ?
C12 C11 P1 C9 -53.56(14) . . . . ?
C12 C11 P1 C7 -169.31(12) . . . . ?
C8 C7 P1 N1 -65.82(14) . . . . ?
C8 C7 P1 C9 55.43(13) . . . . ?
C8 C7 P1 C11 171.62(12) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.046
_database_code_depnum_ccdc_archive 'CCDC 1018467'
#######################################################################
#
#                 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_7d

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H40 B2 Cl2 N2 P2, 3(C H2 Cl2)'
_chemical_formula_sum            'C51 H46 B2 Cl8 N2 P2'
_chemical_formula_weight         1054.06

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
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'
Cl Cl 0.1484 0.1585 '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'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   11.9742(5)
_cell_length_b                   13.0899(5)
_cell_length_c                   18.0121(7)
_cell_angle_alpha                78.766(2)
_cell_angle_beta                 85.796(2)
_cell_angle_gamma                65.463(2)
_cell_volume                     2518.98(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9956
_cell_measurement_theta_min      4.376
_cell_measurement_theta_max      54.486

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1084
_exptl_absorpt_coefficient_mu    0.549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7050
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
'SADABS. Area-Detector Integration Software. (Siemens Industrial Automation, 1995, Inc.: Madison, WI)'

_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  'Bruker Apex II CCD 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            42323
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_unetI/netI     0.0920
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.74
_diffrn_reflns_theta_max         27.50
_reflns_number_total             11463
_reflns_number_gt                6960
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'Bruker SMART. Area-Detector Software Package. (Siemens Industrial Automation, 1993, Inc.: Madison, WI)'
_computing_cell_refinement       
'Bruker SMART. Area-Detector Software Package. (Siemens Industrial Automation, 1993, Inc.: Madison, WI)'
_computing_data_reduction        
'Bruker SAINT. Area-Detector Integration Software. (Siemens Industrial Automation, 1995, Inc.: Madison, WI)'
_computing_structure_solution    
'SHELX-97. Programs for Crystal Structure Analysis. (G. M. Sheldrick, 1997, Release 97-2, University of Gttingen, Germany)'
_computing_structure_refinement  
'SHELX-97. Programs for Crystal Structure Analysis. (G. M. Sheldrick, 1997, Release 97-2, University of Gttingen, Germany)'
_computing_molecular_graphics    
'Ortep for Windows (L. J. Farrugia, J. Appl. Cryst. 1997, 30, 565)'
_computing_publication_material  
'WinGX v1.70.01 (L. J. Farrugia, J. Appl. Cryst. 1999, 32, 837)'

_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)+(0.0446P)²+2.3670P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11463
_refine_ls_number_parameters     614
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.0582
_refine_ls_wR_factor_ref         0.1340
_refine_ls_wR_factor_gt          0.1142
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_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
C1 C 0.6934(3) 0.6268(3) 0.37497(16) 0.0189(7) Uani 1 1 d . . .
C2 C 0.6544(3) 0.7025(3) 0.42475(18) 0.0252(7) Uani 1 1 d . . .
H2 H 0.6174 0.6853 0.4712 0.030 Uiso 1 1 calc R . .
C3 C 0.6696(4) 0.8040(3) 0.4065(2) 0.0362(9) Uani 1 1 d . . .
H3 H 0.6423 0.8563 0.4407 0.043 Uiso 1 1 calc R . .
C4 C 0.7239(4) 0.8300(3) 0.3393(2) 0.0379(10) Uani 1 1 d . . .
H4 H 0.7339 0.8997 0.3273 0.045 Uiso 1 1 calc R . .
C5 C 0.7635(4) 0.7538(3) 0.28984(19) 0.0368(9) Uani 1 1 d . . .
H5 H 0.8013 0.7708 0.2437 0.044 Uiso 1 1 calc R . .
C6 C 0.7481(3) 0.6526(3) 0.30722(18) 0.0276(8) Uani 1 1 d . . .
H6 H 0.7750 0.6007 0.2728 0.033 Uiso 1 1 calc R . .
C7 C 0.6542(3) 0.4621(3) 0.31008(16) 0.0173(7) Uani 1 1 d . . .
C8 C 0.5556(3) 0.5442(3) 0.26565(17) 0.0248(7) Uani 1 1 d . . .
H8 H 0.5050 0.6131 0.2828 0.030 Uiso 1 1 calc R . .
C9 C 0.5309(3) 0.5261(3) 0.19648(18) 0.0308(8) Uani 1 1 d . . .
H9 H 0.4636 0.5824 0.1663 0.037 Uiso 1 1 calc R . .
C10 C 0.6045(3) 0.4260(3) 0.17168(19) 0.0341(9) Uani 1 1 d . . .
H10 H 0.5876 0.4135 0.1243 0.041 Uiso 1 1 calc R . .
C11 C 0.7019(3) 0.3444(3) 0.21497(19) 0.0345(9) Uani 1 1 d . . .
H11 H 0.7524 0.2760 0.1973 0.041 Uiso 1 1 calc R . .
C12 C 0.7270(3) 0.3614(3) 0.28465(18) 0.0276(8) Uani 1 1 d . . .
H12 H 0.7937 0.3042 0.3148 0.033 Uiso 1 1 calc R . .
C13 C 0.8284(3) 0.3887(3) 0.43582(16) 0.0189(7) Uani 1 1 d . . .
C14 C 0.8459(3) 0.2745(3) 0.46045(17) 0.0246(7) Uani 1 1 d . . .
H14 H 0.7807 0.2523 0.4567 0.030 Uiso 1 1 calc R . .
C15 C 0.9588(3) 0.1941(3) 0.49027(19) 0.0344(9) Uani 1 1 d . . .
H15 H 0.9706 0.1169 0.5072 0.041 Uiso 1 1 calc R . .
C16 C 1.0539(3) 0.2258(3) 0.4953(2) 0.0380(9) Uani 1 1 d . . .
H16 H 1.1308 0.1703 0.5159 0.046 Uiso 1 1 calc R . .
C17 C 1.0380(3) 0.3376(3) 0.4708(2) 0.0386(9) Uani 1 1 d . . .
H17 H 1.1040 0.3589 0.4745 0.046 Uiso 1 1 calc R . .
C18 C 0.9258(3) 0.4193(3) 0.44056(18) 0.0293(8) Uani 1 1 d . . .
H18 H 0.9154 0.4961 0.4231 0.035 Uiso 1 1 calc R . .
C19 C 0.3761(3) 0.4771(3) 0.40487(15) 0.0195(7) Uani 1 1 d . . .
C20 C 0.2535(3) 0.5299(3) 0.38037(18) 0.0305(8) Uani 1 1 d . . .
H20 H 0.2031 0.6041 0.3901 0.037 Uiso 1 1 calc R . .
C21 C 0.2042(4) 0.4752(4) 0.3419(2) 0.0423(10) Uani 1 1 d . . .
H21 H 0.1206 0.5116 0.3261 0.051 Uiso 1 1 calc R . .
C22 C 0.2774(4) 0.3677(4) 0.3267(2) 0.0453(11) Uani 1 1 d . . .
H22 H 0.2445 0.3306 0.2999 0.054 Uiso 1 1 calc R . .
C23 C 0.3982(4) 0.3146(3) 0.35049(19) 0.0379(9) Uani 1 1 d . . .
H23 H 0.4485 0.2406 0.3403 0.045 Uiso 1 1 calc R . .
C24 C 0.4463(3) 0.3687(3) 0.38899(17) 0.0254(8) Uani 1 1 d . . .
H24 H 0.5296 0.3308 0.4051 0.031 Uiso 1 1 calc R . .
C25 C 0.7844(3) 0.8485(3) 0.02400(16) 0.0180(7) Uani 1 1 d . . .
C26 C 0.7125(3) 0.8210(3) 0.08234(17) 0.0257(8) Uani 1 1 d . . .
H26 H 0.6620 0.8768 0.1111 0.031 Uiso 1 1 calc R . .
C27 C 0.7149(3) 0.7116(3) 0.09825(19) 0.0338(9) Uani 1 1 d . . .
H27 H 0.6659 0.6930 0.1379 0.041 Uiso 1 1 calc R . .
C28 C 0.7877(3) 0.6304(3) 0.0571(2) 0.0355(9) Uani 1 1 d . . .
H28 H 0.7901 0.5555 0.0687 0.043 Uiso 1 1 calc R . .
C29 C 0.8574(3) 0.6578(3) -0.0015(2) 0.0320(8) Uani 1 1 d . . .
H29 H 0.9066 0.6018 -0.0305 0.038 Uiso 1 1 calc R . .
C30 C 0.8565(3) 0.7660(3) -0.01821(18) 0.0244(7) Uani 1 1 d . . .
H30 H 0.9050 0.7839 -0.0584 0.029 Uiso 1 1 calc R . .
C31 C 0.6723(3) 1.0780(3) 0.06177(16) 0.0189(7) Uani 1 1 d . . .
C32 C 0.7027(3) 1.0571(3) 0.13868(17) 0.0229(7) Uani 1 1 d . . .
H32 H 0.7788 0.9979 0.1576 0.027 Uiso 1 1 calc R . .
C33 C 0.6213(3) 1.1229(3) 0.18686(19) 0.0288(8) Uani 1 1 d . . .
H33 H 0.6419 1.1089 0.2389 0.035 Uiso 1 1 calc R . .
C34 C 0.5101(3) 1.2091(3) 0.1600(2) 0.0329(9) Uani 1 1 d . . .
H34 H 0.4549 1.2541 0.1933 0.040 Uiso 1 1 calc R . .
C35 C 0.4796(3) 1.2294(3) 0.0845(2) 0.0311(8) Uani 1 1 d . . .
H35 H 0.4029 1.2881 0.0662 0.037 Uiso 1 1 calc R . .
C36 C 0.5598(3) 1.1648(3) 0.03530(18) 0.0227(7) Uani 1 1 d . . .
H36 H 0.5381 1.1796 -0.0166 0.027 Uiso 1 1 calc R . .
C37 C 0.7087(3) 1.0454(3) -0.09338(16) 0.0173(7) Uani 1 1 d . . .
C38 C 0.6273(3) 1.0055(3) -0.11558(17) 0.0219(7) Uani 1 1 d . . .
H38 H 0.6114 0.9470 -0.0826 0.026 Uiso 1 1 calc R . .
C39 C 0.5693(3) 1.0515(3) -0.18616(18) 0.0258(8) Uani 1 1 d . . .
H39 H 0.5145 1.0237 -0.2014 0.031 Uiso 1 1 calc R . .
C40 C 0.5914(3) 1.1371(3) -0.23381(17) 0.0248(8) Uani 1 1 d . . .
H40 H 0.5514 1.1685 -0.2817 0.030 Uiso 1 1 calc R . .
C41 C 0.6714(3) 1.1773(3) -0.21211(17) 0.0260(8) Uani 1 1 d . . .
H41 H 0.6862 1.2365 -0.2451 0.031 Uiso 1 1 calc R . .
C42 C 0.7305(3) 1.1316(3) -0.14203(17) 0.0224(7) Uani 1 1 d . . .
H42 H 0.7859 1.1593 -0.1274 0.027 Uiso 1 1 calc R . .
C43 C 0.8915(3) 1.2123(3) -0.02669(16) 0.0172(7) Uani 1 1 d . . .
C44 C 0.7896(3) 1.2957(3) 0.00012(19) 0.0281(8) Uani 1 1 d . . .
H44 H 0.7591 1.2774 0.0488 0.034 Uiso 1 1 calc R . .
C45 C 0.7307(3) 1.4048(3) -0.0416(2) 0.0396(10) Uani 1 1 d . . .
H45 H 0.6614 1.4596 -0.0212 0.048 Uiso 1 1 calc R . .
C46 C 0.7724(4) 1.4340(3) -0.1127(2) 0.0418(10) Uani 1 1 d . . .
H46 H 0.7320 1.5085 -0.1416 0.050 Uiso 1 1 calc R . .
C47 C 0.8746(3) 1.3525(3) -0.1412(2) 0.0345(9) Uani 1 1 d . . .
H47 H 0.9049 1.3714 -0.1898 0.041 Uiso 1 1 calc R . .
C48 C 0.9322(3) 1.2442(3) -0.09900(17) 0.0255(8) Uani 1 1 d . . .
H48 H 1.0016 1.1896 -0.1195 0.031 Uiso 1 1 calc R . .
C49 C 0.0684(4) 0.9334(3) 0.3057(2) 0.0428(10) Uani 1 1 d . . .
H49A H 0.0953 0.9641 0.2564 0.051 Uiso 1 1 calc R . .
H49B H 0.1410 0.8942 0.3397 0.051 Uiso 1 1 calc R . .
C50 C 0.0372(4) 0.2727(4) 0.2455(3) 0.0550(12) Uani 1 1 d . . .
H50A H 0.0267 0.2696 0.3008 0.066 Uiso 1 1 calc R . .
H50B H -0.0232 0.2493 0.2274 0.066 Uiso 1 1 calc R . .
N1 N 0.5764(2) 0.4864(2) 0.45929(13) 0.0163(5) Uani 1 1 d . . .
N2 N 0.9109(2) 0.9924(2) 0.00742(13) 0.0159(5) Uani 1 1 d . . .
B1 B 0.4346(3) 0.5345(3) 0.45263(18) 0.0171(7) Uani 1 1 d . . .
B2 B 0.9583(3) 1.0836(3) 0.01812(18) 0.0179(8) Uani 1 1 d . . .
P1 P 0.68045(7) 0.49127(7) 0.39971(4) 0.01675(18) Uani 1 1 d . . .
P2 P 0.77925(7) 0.99151(7) -0.00036(4) 0.01617(18) Uani 1 1 d . . .
Cl1 Cl 0.36802(7) 0.69918(6) 0.41110(4) 0.02314(18) Uani 1 1 d . . .
Cl2 Cl 0.96245(7) 1.09063(7) 0.12574(4) 0.02280(18) Uani 1 1 d . . .
Cl3 Cl 0.01350(13) 0.83545(11) 0.29245(7) 0.0672(4) Uani 1 1 d . . .
Cl4 Cl -0.0402(2) 1.04584(11) 0.34405(7) 0.1216(8) Uani 1 1 d . . .
Cl5 Cl 0.18466(10) 0.17668(10) 0.22784(7) 0.0620(3) Uani 1 1 d . . .
Cl6 Cl 0.00658(11) 0.41428(10) 0.20113(7) 0.0607(3) Uani 1 1 d . . .
Cl7A Cl 0.6578(4) 0.9813(5) 0.5842(2) 0.0827(14) Uani 0.496(8) 1 d P A 1
Cl8A Cl 0.7128(3) 1.0695(3) 0.4314(2) 0.0443(9) Uani 0.496(8) 1 d P A 1
C51A C 0.6001(7) 1.0882(7) 0.5072(5) 0.038(2) Uani 0.504(8) 1 d P A 1
H51A H 0.5782 1.1631 0.5221 0.045 Uiso 0.504(8) 1 calc PR A 1
H51B H 0.5246 1.0874 0.4888 0.045 Uiso 0.504(8) 1 calc PR A 1
Cl7B Cl 0.6436(4) 0.9285(5) 0.5970(3) 0.0759(12) Uani 0.504(8) 1 d P A 2
Cl8B Cl 0.6693(8) 1.0734(3) 0.4635(4) 0.0987(18) Uani 0.504(8) 1 d P A 2
C51B C 0.6865(12) 1.0350(11) 0.5624(8) 0.074(4) Uani 0.496(8) 1 d P A 2
H51C H 0.7735 1.0110 0.5761 0.089 Uiso 0.496(8) 1 calc PR A 2
H51D H 0.6363 1.1022 0.5857 0.089 Uiso 0.496(8) 1 calc PR A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.380(4) . ?
C1 C6 1.393(4) . ?
C1 P1 1.811(3) . ?
C2 C3 1.388(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.384(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.381(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.385(5) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.390(4) . ?
C7 C8 1.393(4) . ?
C7 P1 1.807(3) . ?
C8 C9 1.387(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.380(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.373(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.391(5) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C18 1.394(4) . ?
C13 C14 1.403(4) . ?
C13 P1 1.794(3) . ?
C14 C15 1.389(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.378(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.380(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.390(5) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C24 1.391(4) . ?
C19 C20 1.400(4) . ?
C19 B1 1.605(5) . ?
C20 C21 1.395(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.383(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.379(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.379(5) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C30 1.393(4) . ?
C25 C26 1.397(4) . ?
C25 P2 1.813(3) . ?
C26 C27 1.393(5) . ?
C26 H26 0.9500 . ?
C27 C28 1.372(5) . ?
C27 H27 0.9500 . ?
C28 C29 1.382(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.385(4) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C36 1.395(4) . ?
C31 C32 1.403(4) . ?
C31 P2 1.804(3) . ?
C32 C33 1.385(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.383(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.379(5) . ?
C34 H34 0.9500 . ?
C35 C36 1.384(5) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C42 1.392(4) . ?
C37 C38 1.393(4) . ?
C37 P2 1.809(3) . ?
C38 C39 1.395(4) . ?
C38 H38 0.9500 . ?
C39 C40 1.379(4) . ?
C39 H39 0.9500 . ?
C40 C41 1.379(4) . ?
C40 H40 0.9500 . ?
C41 C42 1.392(4) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 C44 1.388(4) . ?
C43 C48 1.404(4) . ?
C43 B2 1.605(4) . ?
C44 C45 1.387(5) . ?
C44 H44 0.9500 . ?
C45 C46 1.381(5) . ?
C45 H45 0.9500 . ?
C46 C47 1.392(5) . ?
C46 H46 0.9500 . ?
C47 C48 1.381(4) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
C49 Cl3 1.725(4) . ?
C49 Cl4 1.735(4) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 Cl5 1.740(4) . ?
C50 Cl6 1.763(4) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
N1 B1 1.551(4) . ?
N1 B1 1.562(4) 2_666 ?
N1 P1 1.597(2) . ?
N2 B2 1.560(4) 2_775 ?
N2 B2 1.566(4) . ?
N2 P2 1.598(2) . ?
B1 N1 1.562(4) 2_666 ?
B1 Cl1 1.968(3) . ?
B2 N2 1.560(4) 2_775 ?
B2 Cl2 1.964(3) . ?
Cl7A C51A 1.715(10) . ?
Cl8A C51A 1.824(9) . ?
C51A H51A 0.9900 . ?
C51A H51B 0.9900 . ?
Cl7B C51B 1.674(12) . ?
Cl8B C51B 1.756(15) . ?
C51B H51C 0.9900 . ?
C51B H51D 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 119.7(3) . . ?
C2 C1 P1 120.1(2) . . ?
C6 C1 P1 120.1(3) . . ?
C1 C2 C3 119.6(3) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
C4 C3 C2 120.9(3) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C5 C4 C3 119.3(3) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 120.3(3) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C5 C6 C1 120.2(3) . . ?
C5 C6 H6 119.9 . . ?
C1 C6 H6 119.9 . . ?
C12 C7 C8 119.3(3) . . ?
C12 C7 P1 122.8(2) . . ?
C8 C7 P1 118.0(2) . . ?
C9 C8 C7 120.4(3) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C10 C9 C8 119.7(3) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C11 C10 C9 120.5(3) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C10 C11 C12 120.3(3) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C7 C12 C11 119.9(3) . . ?
C7 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C18 C13 C14 119.3(3) . . ?
C18 C13 P1 121.9(2) . . ?
C14 C13 P1 118.8(2) . . ?
C15 C14 C13 119.8(3) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C16 C15 C14 120.3(3) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C15 C16 C17 120.4(3) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
C16 C17 C18 120.2(3) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C17 C18 C13 120.0(3) . . ?
C17 C18 H18 120.0 . . ?
C13 C18 H18 120.0 . . ?
C24 C19 C20 117.3(3) . . ?
C24 C19 B1 120.0(3) . . ?
C20 C19 B1 122.6(3) . . ?
C21 C20 C19 121.0(4) . . ?
C21 C20 H20 119.5 . . ?
C19 C20 H20 119.5 . . ?
C22 C21 C20 119.8(4) . . ?
C22 C21 H21 120.1 . . ?
C20 C21 H21 120.1 . . ?
C23 C22 C21 119.9(4) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C22 C23 C24 120.1(4) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C23 C24 C19 121.9(3) . . ?
C23 C24 H24 119.1 . . ?
C19 C24 H24 119.1 . . ?
C30 C25 C26 119.2(3) . . ?
C30 C25 P2 119.7(2) . . ?
C26 C25 P2 121.0(3) . . ?
C27 C26 C25 119.9(3) . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C28 C27 C26 120.4(3) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C27 C28 C29 119.8(3) . . ?
C27 C28 H28 120.1 . . ?
C29 C28 H28 120.1 . . ?
C28 C29 C30 120.7(3) . . ?
C28 C29 H29 119.7 . . ?
C30 C29 H29 119.7 . . ?
C29 C30 C25 119.9(3) . . ?
C29 C30 H30 120.0 . . ?
C25 C30 H30 120.0 . . ?
C36 C31 C32 119.2(3) . . ?
C36 C31 P2 121.6(2) . . ?
C32 C31 P2 119.2(2) . . ?
C33 C32 C31 119.7(3) . . ?
C33 C32 H32 120.2 . . ?
C31 C32 H32 120.2 . . ?
C34 C33 C32 120.6(3) . . ?
C34 C33 H33 119.7 . . ?
C32 C33 H33 119.7 . . ?
C35 C34 C33 119.8(3) . . ?
C35 C34 H34 120.1 . . ?
C33 C34 H34 120.1 . . ?
C34 C35 C36 120.5(3) . . ?
C34 C35 H35 119.7 . . ?
C36 C35 H35 119.7 . . ?
C35 C36 C31 120.1(3) . . ?
C35 C36 H36 119.9 . . ?
C31 C36 H36 119.9 . . ?
C42 C37 C38 119.4(3) . . ?
C42 C37 P2 120.0(2) . . ?
C38 C37 P2 120.6(2) . . ?
C37 C38 C39 120.0(3) . . ?
C37 C38 H38 120.0 . . ?
C39 C38 H38 120.0 . . ?
C40 C39 C38 120.1(3) . . ?
C40 C39 H39 120.0 . . ?
C38 C39 H39 120.0 . . ?
C39 C40 C41 120.2(3) . . ?
C39 C40 H40 119.9 . . ?
C41 C40 H40 119.9 . . ?
C40 C41 C42 120.2(3) . . ?
C40 C41 H41 119.9 . . ?
C42 C41 H41 119.9 . . ?
C37 C42 C41 120.1(3) . . ?
C37 C42 H42 120.0 . . ?
C41 C42 H42 120.0 . . ?
C44 C43 C48 116.3(3) . . ?
C44 C43 B2 123.8(3) . . ?
C48 C43 B2 119.8(3) . . ?
C45 C44 C43 122.3(3) . . ?
C45 C44 H44 118.8 . . ?
C43 C44 H44 118.8 . . ?
C46 C45 C44 120.3(4) . . ?
C46 C45 H45 119.8 . . ?
C44 C45 H45 119.8 . . ?
C45 C46 C47 118.8(3) . . ?
C45 C46 H46 120.6 . . ?
C47 C46 H46 120.6 . . ?
C48 C47 C46 120.2(3) . . ?
C48 C47 H47 119.9 . . ?
C46 C47 H47 119.9 . . ?
C47 C48 C43 122.1(3) . . ?
C47 C48 H48 119.0 . . ?
C43 C48 H48 119.0 . . ?
Cl3 C49 Cl4 112.7(2) . . ?
Cl3 C49 H49A 109.0 . . ?
Cl4 C49 H49A 109.0 . . ?
Cl3 C49 H49B 109.0 . . ?
Cl4 C49 H49B 109.0 . . ?
H49A C49 H49B 107.8 . . ?
Cl5 C50 Cl6 112.7(2) . . ?
Cl5 C50 H50A 109.0 . . ?
Cl6 C50 H50A 109.0 . . ?
Cl5 C50 H50B 109.0 . . ?
Cl6 C50 H50B 109.0 . . ?
H50A C50 H50B 107.8 . . ?
B1 N1 B1 89.4(2) . 2_666 ?
B1 N1 P1 132.6(2) . . ?
B1 N1 P1 136.1(2) 2_666 . ?
B2 N2 B2 89.7(2) 2_775 . ?
B2 N2 P2 132.5(2) 2_775 . ?
B2 N2 P2 135.4(2) . . ?
N1 B1 N1 90.6(2) . 2_666 ?
N1 B1 C19 118.6(3) . . ?
N1 B1 C19 118.7(2) 2_666 . ?
N1 B1 Cl1 109.7(2) . . ?
N1 B1 Cl1 110.6(2) 2_666 . ?
C19 B1 Cl1 107.7(2) . . ?
N2 B2 N2 90.3(2) 2_775 . ?
N2 B2 C43 118.4(2) 2_775 . ?
N2 B2 C43 119.4(2) . . ?
N2 B2 Cl2 109.6(2) 2_775 . ?
N2 B2 Cl2 110.8(2) . . ?
C43 B2 Cl2 107.3(2) . . ?
N1 P1 C13 110.09(13) . . ?
N1 P1 C7 111.31(13) . . ?
C13 P1 C7 108.91(14) . . ?
N1 P1 C1 116.20(14) . . ?
C13 P1 C1 105.86(14) . . ?
C7 P1 C1 104.06(13) . . ?
N2 P2 C31 109.52(13) . . ?
N2 P2 C37 116.46(13) . . ?
C31 P2 C37 105.92(14) . . ?
N2 P2 C25 112.06(13) . . ?
C31 P2 C25 108.37(14) . . ?
C37 P2 C25 104.04(14) . . ?
Cl7A C51A Cl8A 110.6(5) . . ?
Cl7A C51A H51A 109.5 . . ?
Cl8A C51A H51A 109.5 . . ?
Cl7A C51A H51B 109.5 . . ?
Cl8A C51A H51B 109.5 . . ?
H51A C51A H51B 108.1 . . ?
Cl7B C51B Cl8B 111.8(6) . . ?
Cl7B C51B H51C 109.2 . . ?
Cl8B C51B H51C 109.2 . . ?
Cl7B C51B H51D 109.2 . . ?
Cl8B C51B H51D 109.2 . . ?
H51C C51B H51D 107.9 . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.907
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.077
_database_code_depnum_ccdc_archive 'CCDC 1018468'
#######################################################################
#
#                 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_8d

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H32 B N P, C F3 O3 S'
_chemical_formula_sum            'C28 H32 B F3 N O3 P S'
_chemical_formula_weight         561.39

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'


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                   13.6726(6)
_cell_length_b                   13.0411(6)
_cell_length_c                   15.1399(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.961(2)
_cell_angle_gamma                90.00
_cell_volume                     2666.6(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9990
_cell_measurement_theta_min      5.369
_cell_measurement_theta_max      54.729

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1176
_exptl_absorpt_coefficient_mu    0.234
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7171
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
'SADABS. Area-Detector Integration Software. (Siemens Industrial Automation, 1995, Inc.: Madison, WI)'

_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  'Bruker Apex II CCD 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            43894
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         27.52
_reflns_number_total             6097
_reflns_number_gt                4410
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'Bruker SMART. Area-Detector Software Package. (Siemens Industrial Automation, 1993, Inc.: Madison, WI)'
_computing_cell_refinement       
'Bruker SMART. Area-Detector Software Package. (Siemens Industrial Automation, 1993, Inc.: Madison, WI)'
_computing_data_reduction        
'Bruker SAINT. Area-Detector Integration Software. (Siemens Industrial Automation, 1995, Inc.: Madison, WI)'
_computing_structure_solution    
'SHELX-97. Programs for Crystal Structure Analysis. (G. M. Sheldrick, 1997, Release 97-2, University of Gttingen, Germany)'
_computing_structure_refinement  
'SHELX-97. Programs for Crystal Structure Analysis. (G. M. Sheldrick, 1997, Release 97-2, University of Gttingen, Germany)'
_computing_molecular_graphics    
'Ortep for Windows (L. J. Farrugia, J. Appl. Cryst. 1997, 30, 565)'
_computing_publication_material  
'WinGX v1.70.01 (L. J. Farrugia, J. Appl. Cryst. 1999, 32, 837)'

_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)+(0.0451P)²+1.6106P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6097
_refine_ls_number_parameters     344
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0432
_refine_ls_wR_factor_ref         0.1109
_refine_ls_wR_factor_gt          0.0975
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_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
C1 C 0.42307(14) 0.84965(16) 0.17291(14) 0.0220(4) Uani 1 1 d . . .
H1 H 0.3500 0.8474 0.1734 0.026 Uiso 1 1 calc R . .
C2 C 0.45149(15) 0.95301(16) 0.13497(15) 0.0275(5) Uani 1 1 d . . .
H2A H 0.4083 0.9649 0.0771 0.033 Uiso 1 1 calc R . .
H2B H 0.4379 1.0082 0.1763 0.033 Uiso 1 1 calc R . .
C3 C 0.55933(15) 0.96144(17) 0.12057(15) 0.0284(5) Uani 1 1 d . . .
H3A H 0.6014 0.9720 0.1793 0.034 Uiso 1 1 calc R . .
H3B H 0.5664 1.0228 0.0835 0.034 Uiso 1 1 calc R . .
C4 C 0.59778(16) 0.86799(18) 0.07540(15) 0.0318(5) Uani 1 1 d . . .
H4A H 0.6710 0.8714 0.0843 0.038 Uiso 1 1 calc R . .
H4B H 0.5742 0.8728 0.0103 0.038 Uiso 1 1 calc R . .
C5 C 0.56737(14) 0.76192(17) 0.10819(14) 0.0253(5) Uani 1 1 d . . .
H5 H 0.5826 0.7078 0.0655 0.030 Uiso 1 1 calc R . .
C6 C 0.61796(17) 0.7340(2) 0.20355(16) 0.0384(6) Uani 1 1 d . . .
H6A H 0.5998 0.6628 0.2169 0.046 Uiso 1 1 calc R . .
H6B H 0.6906 0.7362 0.2054 0.046 Uiso 1 1 calc R . .
C7 C 0.59053(18) 0.80425(19) 0.27564(16) 0.0367(6) Uani 1 1 d . . .
H7A H 0.6264 0.8699 0.2733 0.044 Uiso 1 1 calc R . .
H7B H 0.6137 0.7727 0.3347 0.044 Uiso 1 1 calc R . .
C8 C 0.47948(16) 0.82727(18) 0.26860(14) 0.0305(5) Uani 1 1 d . . .
H8A H 0.4714 0.8872 0.3069 0.037 Uiso 1 1 calc R . .
H8B H 0.4474 0.7680 0.2933 0.037 Uiso 1 1 calc R . .
C9 C 0.44159(16) 0.57673(17) 0.05662(16) 0.0311(5) Uani 1 1 d . . .
H9A H 0.4467 0.5813 -0.0071 0.047 Uiso 1 1 calc R . .
H9B H 0.4021 0.5165 0.0670 0.047 Uiso 1 1 calc R . .
H9C H 0.5080 0.5704 0.0915 0.047 Uiso 1 1 calc R . .
C10 C 0.20528(13) 0.77202(14) 0.04128(12) 0.0157(4) Uani 1 1 d . . .
C11 C 0.10457(13) 0.78025(15) 0.04862(13) 0.0199(4) Uani 1 1 d . . .
H11 H 0.0764 0.7359 0.0876 0.024 Uiso 1 1 calc R . .
C12 C 0.04637(14) 0.85310(16) -0.00110(14) 0.0228(4) Uani 1 1 d . . .
H12 H -0.0217 0.8592 0.0042 0.027 Uiso 1 1 calc R . .
C13 C 0.08736(15) 0.91727(16) -0.05868(13) 0.0235(4) Uani 1 1 d . . .
H13 H 0.0470 0.9666 -0.0932 0.028 Uiso 1 1 calc R . .
C14 C 0.18723(15) 0.90974(16) -0.06608(13) 0.0223(4) Uani 1 1 d . . .
H14 H 0.2151 0.9544 -0.1051 0.027 Uiso 1 1 calc R . .
C15 C 0.24616(14) 0.83695(15) -0.01649(13) 0.0187(4) Uani 1 1 d . . .
H15 H 0.3143 0.8313 -0.0219 0.022 Uiso 1 1 calc R . .
C16 C 0.26176(13) 0.65730(15) 0.21184(12) 0.0163(4) Uani 1 1 d . . .
C17 C 0.21512(13) 0.73093(16) 0.25732(13) 0.0204(4) Uani 1 1 d . . .
H17 H 0.1820 0.7873 0.2261 0.025 Uiso 1 1 calc R . .
C18 C 0.21763(15) 0.72085(18) 0.34902(14) 0.0290(5) Uani 1 1 d . . .
H18 H 0.1862 0.7708 0.3806 0.035 Uiso 1 1 calc R . .
C19 C 0.26554(15) 0.63865(19) 0.39488(14) 0.0301(5) Uani 1 1 d . . .
H19 H 0.2669 0.6326 0.4576 0.036 Uiso 1 1 calc R . .
C20 C 0.31141(15) 0.56523(18) 0.34950(14) 0.0276(5) Uani 1 1 d . . .
H20 H 0.3437 0.5086 0.3810 0.033 Uiso 1 1 calc R . .
C21 C 0.31026(14) 0.57425(16) 0.25833(13) 0.0220(4) Uani 1 1 d . . .
H21 H 0.3423 0.5242 0.2273 0.026 Uiso 1 1 calc R . .
C22 C 0.21961(13) 0.55436(15) 0.03731(13) 0.0179(4) Uani 1 1 d . . .
C23 C 0.16418(16) 0.48372(17) 0.07675(15) 0.0302(5) Uani 1 1 d . . .
H23 H 0.1539 0.4927 0.1369 0.036 Uiso 1 1 calc R . .
C24 C 0.12387(19) 0.39978(19) 0.02767(16) 0.0394(6) Uani 1 1 d . . .
H24 H 0.0849 0.3518 0.0542 0.047 Uiso 1 1 calc R . .
C25 C 0.13984(19) 0.38541(18) -0.05912(16) 0.0367(6) Uani 1 1 d . . .
H25 H 0.1138 0.3265 -0.0915 0.044 Uiso 1 1 calc R . .
C26 C 0.19369(18) 0.45673(19) -0.09894(15) 0.0347(5) Uani 1 1 d . . .
H26 H 0.2038 0.4474 -0.1591 0.042 Uiso 1 1 calc R . .
C27 C 0.23291(16) 0.54162(17) -0.05156(14) 0.0281(5) Uani 1 1 d . . .
H27 H 0.2689 0.5912 -0.0794 0.034 Uiso 1 1 calc R . .
C28 C 0.43406(15) 0.74720(18) -0.19805(14) 0.0295(5) Uani 1 1 d . . .
N1 N 0.39265(11) 0.67139(12) 0.08473(11) 0.0170(3) Uani 1 1 d . . .
O1 O 0.37037(14) 0.56220(14) -0.20602(12) 0.0492(5) Uani 1 1 d . . .
O2 O 0.52955(12) 0.59745(13) -0.25118(14) 0.0480(5) Uani 1 1 d . . .
O3 O 0.37915(13) 0.65084(12) -0.34510(10) 0.0388(4) Uani 1 1 d . . .
B1 B 0.45419(16) 0.75812(18) 0.11554(15) 0.0184(5) Uani 1 1 d . . .
F1 F 0.48377(11) 0.81702(10) -0.23813(10) 0.0443(4) Uani 1 1 d . . .
F2 F 0.34468(10) 0.78684(13) -0.19498(11) 0.0572(5) Uani 1 1 d . . .
F3 F 0.47993(11) 0.73917(14) -0.11389(9) 0.0541(4) Uani 1 1 d . . .
P1 P 0.27307(3) 0.66581(4) 0.09559(3) 0.01459(12) Uani 1 1 d . . .
S1 S 0.42738(4) 0.62488(4) -0.25648(4) 0.02486(14) 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
C1 C2 1.539(3) . ?
C1 C8 1.559(3) . ?
C1 B1 1.573(3) . ?
C1 H1 1.0000 . ?
C2 C3 1.528(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.530(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.548(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.544(3) . ?
C5 B1 1.569(3) . ?
C5 H5 1.0000 . ?
C6 C7 1.516(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.535(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 N1 1.497(2) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C15 1.395(3) . ?
C10 C11 1.403(2) . ?
C10 P1 1.7934(19) . ?
C11 C12 1.384(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.388(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.391(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.388(3) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.393(3) . ?
C16 C21 1.401(3) . ?
C16 P1 1.7941(19) . ?
C17 C18 1.390(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.385(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.384(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.383(3) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C23 1.386(3) . ?
C22 C27 1.395(3) . ?
C22 P1 1.796(2) . ?
C23 C24 1.388(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.378(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.382(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.381(3) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 F3 1.334(3) . ?
C28 F2 1.334(2) . ?
C28 F1 1.337(3) . ?
C28 S1 1.819(2) . ?
N1 B1 1.443(3) . ?
N1 P1 1.6701(15) . ?
O1 S1 1.4298(16) . ?
O2 S1 1.4321(16) . ?
O3 S1 1.4402(17) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C8 113.19(17) . . ?
C2 C1 B1 110.66(16) . . ?
C8 C1 B1 103.52(17) . . ?
C2 C1 H1 109.8 . . ?
C8 C1 H1 109.8 . . ?
B1 C1 H1 109.8 . . ?
C3 C2 C1 114.95(18) . . ?
C3 C2 H2A 108.5 . . ?
C1 C2 H2A 108.5 . . ?
C3 C2 H2B 108.5 . . ?
C1 C2 H2B 108.5 . . ?
H2A C2 H2B 107.5 . . ?
C2 C3 C4 114.39(17) . . ?
C2 C3 H3A 108.7 . . ?
C4 C3 H3A 108.7 . . ?
C2 C3 H3B 108.7 . . ?
C4 C3 H3B 108.7 . . ?
H3A C3 H3B 107.6 . . ?
C3 C4 C5 116.11(17) . . ?
C3 C4 H4A 108.3 . . ?
C5 C4 H4A 108.3 . . ?
C3 C4 H4B 108.3 . . ?
C5 C4 H4B 108.3 . . ?
H4A C4 H4B 107.4 . . ?
C6 C5 C4 114.01(19) . . ?
C6 C5 B1 103.25(17) . . ?
C4 C5 B1 111.59(17) . . ?
C6 C5 H5 109.3 . . ?
C4 C5 H5 109.3 . . ?
B1 C5 H5 109.3 . . ?
C7 C6 C5 113.93(19) . . ?
C7 C6 H6A 108.8 . . ?
C5 C6 H6A 108.8 . . ?
C7 C6 H6B 108.8 . . ?
C5 C6 H6B 108.8 . . ?
H6A C6 H6B 107.7 . . ?
C6 C7 C8 114.90(19) . . ?
C6 C7 H7A 108.5 . . ?
C8 C7 H7A 108.5 . . ?
C6 C7 H7B 108.5 . . ?
C8 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
C7 C8 C1 116.23(17) . . ?
C7 C8 H8A 108.2 . . ?
C1 C8 H8A 108.2 . . ?
C7 C8 H8B 108.2 . . ?
C1 C8 H8B 108.2 . . ?
H8A C8 H8B 107.4 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C15 C10 C11 119.82(17) . . ?
C15 C10 P1 121.82(14) . . ?
C11 C10 P1 117.80(14) . . ?
C12 C11 C10 119.85(18) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C11 C12 C13 120.08(18) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C12 C13 C14 120.37(19) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
C15 C14 C13 119.95(18) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C10 119.93(17) . . ?
C14 C15 H15 120.0 . . ?
C10 C15 H15 120.0 . . ?
C17 C16 C21 120.13(18) . . ?
C17 C16 P1 123.95(15) . . ?
C21 C16 P1 115.74(14) . . ?
C18 C17 C16 119.13(19) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
C19 C18 C17 120.7(2) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C20 C19 C18 120.13(19) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C21 C20 C19 120.1(2) . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C20 C21 C16 119.87(19) . . ?
C20 C21 H21 120.1 . . ?
C16 C21 H21 120.1 . . ?
C23 C22 C27 119.89(19) . . ?
C23 C22 P1 122.31(15) . . ?
C27 C22 P1 117.77(15) . . ?
C22 C23 C24 119.46(19) . . ?
C22 C23 H23 120.3 . . ?
C24 C23 H23 120.3 . . ?
C25 C24 C23 120.6(2) . . ?
C25 C24 H24 119.7 . . ?
C23 C24 H24 119.7 . . ?
C24 C25 C26 119.9(2) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C27 C26 C25 120.2(2) . . ?
C27 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C26 C27 C22 119.9(2) . . ?
C26 C27 H27 120.1 . . ?
C22 C27 H27 120.1 . . ?
F3 C28 F2 107.10(17) . . ?
F3 C28 F1 106.88(18) . . ?
F2 C28 F1 106.56(19) . . ?
F3 C28 S1 112.10(17) . . ?
F2 C28 S1 112.32(15) . . ?
F1 C28 S1 111.53(14) . . ?
B1 N1 C9 118.31(16) . . ?
B1 N1 P1 122.19(13) . . ?
C9 N1 P1 118.67(13) . . ?
N1 B1 C5 122.24(18) . . ?
N1 B1 C1 125.37(17) . . ?
C5 B1 C1 111.69(17) . . ?
N1 P1 C10 111.42(8) . . ?
N1 P1 C16 109.55(8) . . ?
C10 P1 C16 112.34(9) . . ?
N1 P1 C22 108.46(8) . . ?
C10 P1 C22 104.96(9) . . ?
C16 P1 C22 109.96(9) . . ?
O1 S1 O2 115.82(11) . . ?
O1 S1 O3 115.06(11) . . ?
O2 S1 O3 114.33(11) . . ?
O1 S1 C28 103.40(11) . . ?
O2 S1 C28 102.54(10) . . ?
O3 S1 C28 103.17(10) . . ?

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
C8 C1 C2 C3 63.7(2) . . . . ?
B1 C1 C2 C3 -51.9(2) . . . . ?
C1 C2 C3 C4 45.3(3) . . . . ?
C2 C3 C4 C5 -42.3(3) . . . . ?
C3 C4 C5 C6 -70.5(2) . . . . ?
C3 C4 C5 B1 46.0(3) . . . . ?
C4 C5 C6 C7 64.1(2) . . . . ?
B1 C5 C6 C7 -57.2(2) . . . . ?
C5 C6 C7 C8 46.0(3) . . . . ?
C6 C7 C8 C1 -42.5(3) . . . . ?
C2 C1 C8 C7 -70.0(2) . . . . ?
B1 C1 C8 C7 49.8(2) . . . . ?
C15 C10 C11 C12 -0.3(3) . . . . ?
P1 C10 C11 C12 -171.92(15) . . . . ?
C10 C11 C12 C13 0.6(3) . . . . ?
C11 C12 C13 C14 -0.8(3) . . . . ?
C12 C13 C14 C15 0.7(3) . . . . ?
C13 C14 C15 C10 -0.5(3) . . . . ?
C11 C10 C15 C14 0.3(3) . . . . ?
P1 C10 C15 C14 171.56(15) . . . . ?
C21 C16 C17 C18 0.1(3) . . . . ?
P1 C16 C17 C18 -174.79(15) . . . . ?
C16 C17 C18 C19 -0.2(3) . . . . ?
C17 C18 C19 C20 -0.2(3) . . . . ?
C18 C19 C20 C21 0.6(3) . . . . ?
C19 C20 C21 C16 -0.6(3) . . . . ?
C17 C16 C21 C20 0.3(3) . . . . ?
P1 C16 C21 C20 175.59(15) . . . . ?
C27 C22 C23 C24 1.2(3) . . . . ?
P1 C22 C23 C24 179.22(18) . . . . ?
C22 C23 C24 C25 1.0(4) . . . . ?
C23 C24 C25 C26 -2.1(4) . . . . ?
C24 C25 C26 C27 1.0(4) . . . . ?
C25 C26 C27 C22 1.2(4) . . . . ?
C23 C22 C27 C26 -2.3(3) . . . . ?
P1 C22 C27 C26 179.58(18) . . . . ?
C9 N1 B1 C5 8.5(3) . . . . ?
P1 N1 B1 C5 177.98(15) . . . . ?
C9 N1 B1 C1 -161.12(19) . . . . ?
P1 N1 B1 C1 8.3(3) . . . . ?
C6 C5 B1 N1 -100.4(2) . . . . ?
C4 C5 B1 N1 136.7(2) . . . . ?
C6 C5 B1 C1 70.5(2) . . . . ?
C4 C5 B1 C1 -52.4(2) . . . . ?
C2 C1 B1 N1 -134.0(2) . . . . ?
C8 C1 B1 N1 104.4(2) . . . . ?
C2 C1 B1 C5 55.4(2) . . . . ?
C8 C1 B1 C5 -66.2(2) . . . . ?
B1 N1 P1 C10 57.95(17) . . . . ?
C9 N1 P1 C10 -132.63(15) . . . . ?
B1 N1 P1 C16 -66.98(17) . . . . ?
C9 N1 P1 C16 102.44(16) . . . . ?
B1 N1 P1 C22 172.99(15) . . . . ?
C9 N1 P1 C22 -17.59(17) . . . . ?
C15 C10 P1 N1 11.70(19) . . . . ?
C11 C10 P1 N1 -176.91(15) . . . . ?
C15 C10 P1 C16 135.05(16) . . . . ?
C11 C10 P1 C16 -53.56(18) . . . . ?
C15 C10 P1 C22 -105.49(17) . . . . ?
C11 C10 P1 C22 65.90(17) . . . . ?
C17 C16 P1 N1 117.62(16) . . . . ?
C21 C16 P1 N1 -57.49(16) . . . . ?
C17 C16 P1 C10 -6.77(19) . . . . ?
C21 C16 P1 C10 178.11(14) . . . . ?
C17 C16 P1 C22 -123.27(16) . . . . ?
C21 C16 P1 C22 61.62(16) . . . . ?
C23 C22 P1 N1 129.65(18) . . . . ?
C27 C22 P1 N1 -52.24(18) . . . . ?
C23 C22 P1 C10 -111.16(18) . . . . ?
C27 C22 P1 C10 66.95(17) . . . . ?
C23 C22 P1 C16 9.9(2) . . . . ?
C27 C22 P1 C16 -172.01(16) . . . . ?
F3 C28 S1 O1 61.65(17) . . . . ?
F2 C28 S1 O1 -58.99(19) . . . . ?
F1 C28 S1 O1 -178.54(15) . . . . ?
F3 C28 S1 O2 -59.12(17) . . . . ?
F2 C28 S1 O2 -179.77(17) . . . . ?
F1 C28 S1 O2 60.69(18) . . . . ?
F3 C28 S1 O3 -178.17(15) . . . . ?
F2 C28 S1 O3 61.19(19) . . . . ?
F1 C28 S1 O3 -58.35(17) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.52
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.060
_database_code_depnum_ccdc_archive 'CCDC 1018469'
#######################################################################
#
#                 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_9c

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H18 B F10 N P, C F3 O3 S'
_chemical_formula_sum            'C20 H18 B F13 N O3 P S'
_chemical_formula_weight         641.19

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
O O 0.0106 0.0060 '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'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   9.6201(5)
_cell_length_b                   10.6974(6)
_cell_length_c                   13.7275(8)
_cell_angle_alpha                70.229(3)
_cell_angle_beta                 79.114(2)
_cell_angle_gamma                73.445(2)
_cell_volume                     1267.60(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9897
_cell_measurement_theta_min      5.185
_cell_measurement_theta_max      54.970

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             644
_exptl_absorpt_coefficient_mu    0.312
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7031
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
'SADABS. Area-Detector Integration Software. (Siemens Industrial Automation, 1995, Inc.: Madison, WI)'

_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  'Bruker Apex II CCD 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            21505
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.58
_diffrn_reflns_theta_max         27.53
_reflns_number_total             5787
_reflns_number_gt                4571
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'Bruker SMART. Area-Detector Software Package. (Siemens Industrial Automation, 1993, Inc.: Madison, WI)'
_computing_cell_refinement       
'Bruker SMART. Area-Detector Software Package. (Siemens Industrial Automation, 1993, Inc.: Madison, WI)'
_computing_data_reduction        
'Bruker SAINT. Area-Detector Integration Software. (Siemens Industrial Automation, 1995, Inc.: Madison, WI)'
_computing_structure_solution    
'SHELX-97. Programs for Crystal Structure Analysis. (G. M. Sheldrick, 1997, Release 97-2, University of Gttingen, Germany)'
_computing_structure_refinement  
'SHELX-97. Programs for Crystal Structure Analysis. (G. M. Sheldrick, 1997, Release 97-2, University of Gttingen, Germany)'
_computing_molecular_graphics    
'Ortep for Windows (L. J. Farrugia, J. Appl. Cryst. 1997, 30, 565)'
_computing_publication_material  
'WinGX v1.70.01 (L. J. Farrugia, J. Appl. Cryst. 1999, 32, 837)'

_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)+(0.0458P)²+0.8934P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5787
_refine_ls_number_parameters     361
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0387
_refine_ls_wR_factor_ref         0.1005
_refine_ls_wR_factor_gt          0.0927
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_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
C1 C 0.3414(2) 0.7089(2) 0.10786(15) 0.0204(4) Uani 1 1 d . . .
C2 C 0.2639(2) 0.8061(2) 0.02875(16) 0.0247(4) Uani 1 1 d . . .
C3 C 0.2180(2) 0.7741(3) -0.04742(17) 0.0325(5) Uani 1 1 d . . .
C4 C 0.2454(2) 0.6393(3) -0.04317(18) 0.0349(6) Uani 1 1 d . . .
C5 C 0.3203(2) 0.5387(2) 0.03426(19) 0.0318(5) Uani 1 1 d . . .
C6 C 0.3702(2) 0.5747(2) 0.10673(16) 0.0239(4) Uani 1 1 d . . .
C7 C 0.5651(2) 0.71551(19) 0.19433(14) 0.0169(4) Uani 1 1 d . . .
C8 C 0.6512(2) 0.7653(2) 0.10388(14) 0.0195(4) Uani 1 1 d . . .
C9 C 0.8014(2) 0.7233(2) 0.09423(15) 0.0219(4) Uani 1 1 d . . .
C10 C 0.8703(2) 0.6261(2) 0.17692(16) 0.0213(4) Uani 1 1 d . . .
C11 C 0.7899(2) 0.57258(19) 0.26817(15) 0.0192(4) Uani 1 1 d . . .
C12 C 0.6401(2) 0.61869(19) 0.27508(14) 0.0182(4) Uani 1 1 d . . .
C13 C 0.1303(2) 0.7940(2) 0.26706(16) 0.0231(4) Uani 1 1 d . . .
H13A H 0.0682 0.8342 0.3195 0.035 Uiso 1 1 calc R . .
H13B H 0.1258 0.6984 0.2844 0.035 Uiso 1 1 calc R . .
H13C H 0.0959 0.8454 0.1985 0.035 Uiso 1 1 calc R . .
C14 C 0.4693(2) 0.9219(2) 0.33297(15) 0.0213(4) Uani 1 1 d . . .
H14A H 0.4732 0.9554 0.3911 0.026 Uiso 1 1 calc R . .
H14B H 0.5496 0.8388 0.3374 0.026 Uiso 1 1 calc R . .
C15 C 0.5018(3) 1.0302(2) 0.23181(19) 0.0354(5) Uani 1 1 d . . .
H15A H 0.5971 1.0468 0.2310 0.053 Uiso 1 1 calc R . .
H15B H 0.4263 1.1153 0.2267 0.053 Uiso 1 1 calc R . .
H15C H 0.5028 0.9981 0.1727 0.053 Uiso 1 1 calc R . .
C16 C 0.1479(2) 1.0134(2) 0.35380(15) 0.0213(4) Uani 1 1 d . . .
H16A H 0.0589 0.9778 0.3774 0.026 Uiso 1 1 calc R . .
H16B H 0.1574 1.0558 0.4053 0.026 Uiso 1 1 calc R . .
C17 C 0.1255(3) 1.1256(2) 0.24933(18) 0.0345(5) Uani 1 1 d . . .
H17A H 0.0387 1.1976 0.2577 0.052 Uiso 1 1 calc R . .
H17B H 0.1124 1.0863 0.1977 0.052 Uiso 1 1 calc R . .
H17C H 0.2110 1.1647 0.2258 0.052 Uiso 1 1 calc R . .
C18 C 0.2936(2) 0.7454(2) 0.48081(15) 0.0220(4) Uani 1 1 d . . .
H18A H 0.2059 0.7100 0.4899 0.026 Uiso 1 1 calc R . .
H18B H 0.3799 0.6678 0.4825 0.026 Uiso 1 1 calc R . .
C19 C 0.2886(3) 0.7980(2) 0.57239(16) 0.0320(5) Uani 1 1 d . . .
H19A H 0.2845 0.7236 0.6377 0.048 Uiso 1 1 calc R . .
H19B H 0.2019 0.8731 0.5728 0.048 Uiso 1 1 calc R . .
H19C H 0.3763 0.8310 0.5653 0.048 Uiso 1 1 calc R . .
C20 C -0.2266(3) 0.6171(2) 0.58035(19) 0.0342(5) Uani 1 1 d . . .
N1 N 0.28552(16) 0.80038(16) 0.26505(12) 0.0173(3) Uani 1 1 d . . .
B1 B 0.3933(2) 0.7479(2) 0.19505(16) 0.0173(4) Uani 1 1 d . . .
F1 F 0.23183(14) 0.93899(13) 0.02409(10) 0.0345(3) Uani 1 1 d . . .
F2 F 0.14563(16) 0.87255(17) -0.12349(11) 0.0481(4) Uani 1 1 d . . .
F3 F 0.19799(17) 0.60604(19) -0.11480(12) 0.0562(5) Uani 1 1 d . . .
F4 F 0.34486(16) 0.40658(15) 0.03958(13) 0.0473(4) Uani 1 1 d . . .
F5 F 0.44857(14) 0.47478(13) 0.17919(10) 0.0318(3) Uani 1 1 d . . .
F6 F 0.58644(13) 0.85709(12) 0.02082(9) 0.0272(3) Uani 1 1 d . . .
F7 F 0.88089(13) 0.77231(14) 0.00503(9) 0.0345(3) Uani 1 1 d . . .
F8 F 1.01569(12) 0.58294(13) 0.16759(10) 0.0303(3) Uani 1 1 d . . .
F9 F 0.85699(12) 0.47734(12) 0.34721(9) 0.0276(3) Uani 1 1 d . . .
F10 F 0.56482(12) 0.56306(12) 0.36538(9) 0.0263(3) Uani 1 1 d . . .
F11 F -0.22106(18) 0.62106(18) 0.67575(11) 0.0536(4) Uani 1 1 d . . .
F12 F -0.35501(17) 0.59442(18) 0.57885(14) 0.0587(5) Uani 1 1 d . . .
F13 F -0.12413(18) 0.50998(15) 0.56614(14) 0.0564(4) Uani 1 1 d . . .
P1 P 0.30167(5) 0.87116(5) 0.35525(4) 0.01555(11) Uani 1 1 d . . .
S1 S -0.20355(5) 0.77682(5) 0.48258(4) 0.01982(12) Uani 1 1 d . . .
O1 O -0.20700(16) 0.75434(16) 0.38546(11) 0.0304(4) Uani 1 1 d . . .
O2 O -0.06404(15) 0.78859(15) 0.49838(11) 0.0261(3) Uani 1 1 d . . .
O3 O -0.32696(16) 0.87528(16) 0.51207(12) 0.0317(4) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.385(3) . ?
C1 C6 1.387(3) . ?
C1 B1 1.593(3) . ?
C2 F1 1.347(2) . ?
C2 C3 1.382(3) . ?
C3 F2 1.341(3) . ?
C3 C4 1.372(4) . ?
C4 F3 1.342(2) . ?
C4 C5 1.371(4) . ?
C5 F4 1.344(3) . ?
C5 C6 1.383(3) . ?
C6 F5 1.344(2) . ?
C7 C12 1.386(3) . ?
C7 C8 1.388(3) . ?
C7 B1 1.587(3) . ?
C8 F6 1.347(2) . ?
C8 C9 1.380(3) . ?
C9 F7 1.342(2) . ?
C9 C10 1.379(3) . ?
C10 F8 1.338(2) . ?
C10 C11 1.377(3) . ?
C11 F9 1.332(2) . ?
C11 C12 1.380(3) . ?
C12 F10 1.350(2) . ?
C13 N1 1.509(2) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.524(3) . ?
C14 P1 1.7854(19) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.533(3) . ?
C16 P1 1.7922(19) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.530(3) . ?
C18 P1 1.797(2) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 F13 1.326(3) . ?
C20 F12 1.330(3) . ?
C20 F11 1.336(3) . ?
C20 S1 1.823(2) . ?
N1 B1 1.404(3) . ?
N1 P1 1.7044(15) . ?
S1 O1 1.4403(14) . ?
S1 O3 1.4412(15) . ?
S1 O2 1.4453(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 115.56(18) . . ?
C2 C1 B1 122.37(17) . . ?
C6 C1 B1 122.07(18) . . ?
F1 C2 C3 117.58(19) . . ?
F1 C2 C1 119.30(17) . . ?
C3 C2 C1 123.1(2) . . ?
F2 C3 C4 120.29(19) . . ?
F2 C3 C2 120.7(2) . . ?
C4 C3 C2 119.0(2) . . ?
F3 C4 C5 120.0(2) . . ?
F3 C4 C3 119.8(2) . . ?
C5 C4 C3 120.25(19) . . ?
F4 C5 C4 120.3(2) . . ?
F4 C5 C6 120.4(2) . . ?
C4 C5 C6 119.3(2) . . ?
F5 C6 C5 118.21(19) . . ?
F5 C6 C1 119.12(17) . . ?
C5 C6 C1 122.7(2) . . ?
C12 C7 C8 115.42(17) . . ?
C12 C7 B1 123.04(17) . . ?
C8 C7 B1 120.54(16) . . ?
F6 C8 C9 117.98(17) . . ?
F6 C8 C7 119.13(17) . . ?
C9 C8 C7 122.88(17) . . ?
F7 C9 C10 119.54(17) . . ?
F7 C9 C8 121.20(18) . . ?
C10 C9 C8 119.23(18) . . ?
F8 C10 C11 120.15(18) . . ?
F8 C10 C9 119.64(18) . . ?
C11 C10 C9 120.21(18) . . ?
F9 C11 C10 119.94(17) . . ?
F9 C11 C12 121.34(17) . . ?
C10 C11 C12 118.72(17) . . ?
F10 C12 C11 117.09(17) . . ?
F10 C12 C7 119.38(16) . . ?
C11 C12 C7 123.52(17) . . ?
N1 C13 H13A 109.5 . . ?
N1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 P1 119.09(15) . . ?
C15 C14 H14A 107.5 . . ?
P1 C14 H14A 107.5 . . ?
C15 C14 H14B 107.5 . . ?
P1 C14 H14B 107.5 . . ?
H14A C14 H14B 107.0 . . ?
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 . . ?
C17 C16 P1 116.60(15) . . ?
C17 C16 H16A 108.1 . . ?
P1 C16 H16A 108.1 . . ?
C17 C16 H16B 108.1 . . ?
P1 C16 H16B 108.1 . . ?
H16A C16 H16B 107.3 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 P1 114.53(14) . . ?
C19 C18 H18A 108.6 . . ?
P1 C18 H18A 108.6 . . ?
C19 C18 H18B 108.6 . . ?
P1 C18 H18B 108.6 . . ?
H18A C18 H18B 107.6 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
F13 C20 F12 107.7(2) . . ?
F13 C20 F11 107.3(2) . . ?
F12 C20 F11 107.5(2) . . ?
F13 C20 S1 112.39(17) . . ?
F12 C20 S1 110.96(17) . . ?
F11 C20 S1 110.83(16) . . ?
B1 N1 C13 118.96(15) . . ?
B1 N1 P1 129.49(13) . . ?
C13 N1 P1 111.54(12) . . ?
N1 B1 C7 127.73(16) . . ?
N1 B1 C1 117.76(17) . . ?
C7 B1 C1 114.45(16) . . ?
N1 P1 C14 112.65(8) . . ?
N1 P1 C16 107.75(8) . . ?
C14 P1 C16 111.36(9) . . ?
N1 P1 C18 107.82(9) . . ?
C14 P1 C18 108.69(9) . . ?
C16 P1 C18 108.44(10) . . ?
O1 S1 O3 115.51(9) . . ?
O1 S1 O2 114.73(9) . . ?
O3 S1 O2 114.51(9) . . ?
O1 S1 C20 103.91(10) . . ?
O3 S1 C20 102.20(11) . . ?
O2 S1 C20 103.62(10) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 F1 -179.82(17) . . . . ?
B1 C1 C2 F1 0.6(3) . . . . ?
C6 C1 C2 C3 -0.4(3) . . . . ?
B1 C1 C2 C3 -179.95(19) . . . . ?
F1 C2 C3 F2 0.8(3) . . . . ?
C1 C2 C3 F2 -178.71(19) . . . . ?
F1 C2 C3 C4 -178.18(19) . . . . ?
C1 C2 C3 C4 2.4(3) . . . . ?
F2 C3 C4 F3 -0.8(3) . . . . ?
C2 C3 C4 F3 178.16(19) . . . . ?
F2 C3 C4 C5 179.54(19) . . . . ?
C2 C3 C4 C5 -1.5(3) . . . . ?
F3 C4 C5 F4 -0.9(3) . . . . ?
C3 C4 C5 F4 178.81(19) . . . . ?
F3 C4 C5 C6 179.11(19) . . . . ?
C3 C4 C5 C6 -1.2(3) . . . . ?
F4 C5 C6 F5 2.8(3) . . . . ?
C4 C5 C6 F5 -177.23(18) . . . . ?
F4 C5 C6 C1 -176.67(18) . . . . ?
C4 C5 C6 C1 3.3(3) . . . . ?
C2 C1 C6 F5 178.07(17) . . . . ?
B1 C1 C6 F5 -2.3(3) . . . . ?
C2 C1 C6 C5 -2.5(3) . . . . ?
B1 C1 C6 C5 177.07(18) . . . . ?
C12 C7 C8 F6 178.30(16) . . . . ?
B1 C7 C8 F6 9.4(3) . . . . ?
C12 C7 C8 C9 -0.6(3) . . . . ?
B1 C7 C8 C9 -169.57(18) . . . . ?
F6 C8 C9 F7 0.1(3) . . . . ?
C7 C8 C9 F7 179.07(17) . . . . ?
F6 C8 C9 C10 -177.95(17) . . . . ?
C7 C8 C9 C10 1.0(3) . . . . ?
F7 C9 C10 F8 0.7(3) . . . . ?
C8 C9 C10 F8 178.76(17) . . . . ?
F7 C9 C10 C11 -178.53(17) . . . . ?
C8 C9 C10 C11 -0.4(3) . . . . ?
F8 C10 C11 F9 -0.2(3) . . . . ?
C9 C10 C11 F9 179.02(17) . . . . ?
F8 C10 C11 C12 -179.61(16) . . . . ?
C9 C10 C11 C12 -0.4(3) . . . . ?
F9 C11 C12 F10 0.0(3) . . . . ?
C10 C11 C12 F10 179.45(16) . . . . ?
F9 C11 C12 C7 -178.64(17) . . . . ?
C10 C11 C12 C7 0.8(3) . . . . ?
C8 C7 C12 F10 -178.89(16) . . . . ?
B1 C7 C12 F10 -10.3(3) . . . . ?
C8 C7 C12 C11 -0.3(3) . . . . ?
B1 C7 C12 C11 168.35(17) . . . . ?
C13 N1 B1 C7 -166.36(18) . . . . ?
P1 N1 B1 C7 12.1(3) . . . . ?
C13 N1 B1 C1 10.7(3) . . . . ?
P1 N1 B1 C1 -170.84(14) . . . . ?
C12 C7 B1 N1 62.6(3) . . . . ?
C8 C7 B1 N1 -129.3(2) . . . . ?
C12 C7 B1 C1 -114.5(2) . . . . ?
C8 C7 B1 C1 53.5(2) . . . . ?
C2 C1 B1 N1 66.4(3) . . . . ?
C6 C1 B1 N1 -113.1(2) . . . . ?
C2 C1 B1 C7 -116.1(2) . . . . ?
C6 C1 B1 C7 64.3(2) . . . . ?
B1 N1 P1 C14 17.0(2) . . . . ?
C13 N1 P1 C14 -164.43(13) . . . . ?
B1 N1 P1 C16 140.24(18) . . . . ?
C13 N1 P1 C16 -41.20(15) . . . . ?
B1 N1 P1 C18 -102.91(19) . . . . ?
C13 N1 P1 C18 75.65(15) . . . . ?
C15 C14 P1 N1 61.52(18) . . . . ?
C15 C14 P1 C16 -59.66(18) . . . . ?
C15 C14 P1 C18 -179.06(16) . . . . ?
C17 C16 P1 N1 -57.15(17) . . . . ?
C17 C16 P1 C14 66.85(17) . . . . ?
C17 C16 P1 C18 -173.60(15) . . . . ?
C19 C18 P1 N1 -173.19(15) . . . . ?
C19 C18 P1 C14 64.41(18) . . . . ?
C19 C18 P1 C16 -56.79(18) . . . . ?
F13 C20 S1 O1 58.06(18) . . . . ?
F12 C20 S1 O1 -62.54(19) . . . . ?
F11 C20 S1 O1 178.06(16) . . . . ?
F13 C20 S1 O3 178.55(16) . . . . ?
F12 C20 S1 O3 57.96(19) . . . . ?
F11 C20 S1 O3 -61.45(18) . . . . ?
F13 C20 S1 O2 -62.17(18) . . . . ?
F12 C20 S1 O2 177.23(17) . . . . ?
F11 C20 S1 O2 57.83(18) . . . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.53
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.059
_database_code_depnum_ccdc_archive 'CCDC 1018470'
#######################################################################
#
#                 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_10d

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H40 B N P, C F3 O3 S, C H2 Cl2'
_chemical_formula_sum            'C39 H42 B Cl2 F3 N O3 P S'
_chemical_formula_weight         774.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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                   20.7145(13)
_cell_length_b                   10.2318(7)
_cell_length_c                   19.1894(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.369(2)
_cell_angle_gamma                90.00
_cell_volume                     3812.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    149(2)
_cell_measurement_reflns_used    9161
_cell_measurement_theta_min      4.528
_cell_measurement_theta_max      54.921

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1616
_exptl_absorpt_coefficient_mu    0.320
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7054
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
'SADABS. Area-Detector Integration Software. (Siemens Industrial Automation, 1995, Inc.: Madison, WI)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      149(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 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            32988
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.10
_diffrn_reflns_theta_max         27.51
_reflns_number_total             8740
_reflns_number_gt                7274
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'Bruker SMART. Area-Detector Software Package. (Siemens Industrial Automation, 1993, Inc.: Madison, WI)'
_computing_cell_refinement       
'Bruker SMART. Area-Detector Software Package. (Siemens Industrial Automation, 1993, Inc.: Madison, WI)'
_computing_data_reduction        
'Bruker SAINT. Area-Detector Integration Software. (Siemens Industrial Automation, 1995, Inc.: Madison, WI)'
_computing_structure_solution    
'SHELX-97. Programs for Crystal Structure Analysis. (G. M. Sheldrick, 1997, Release 97-2, University of Gttingen, Germany)'
_computing_structure_refinement  
'SHELX-97. Programs for Crystal Structure Analysis. (G. M. Sheldrick, 1997, Release 97-2, University of Gttingen, Germany)'
_computing_molecular_graphics    
'Ortep for Windows (L. J. Farrugia, J. Appl. Cryst. 1997, 30, 565)'
_computing_publication_material  
'WinGX v1.70.01 (L. J. Farrugia, J. Appl. Cryst. 1999, 32, 837)'

_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)+(0.0540P)²+3.4548P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8740
_refine_ls_number_parameters     532
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0454
_refine_ls_wR_factor_ref         0.1204
_refine_ls_wR_factor_gt          0.1130
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_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
S1 S 0.27800(2) 0.45243(5) 0.08300(3) 0.02375(11) Uani 1 1 d . . .
P1 P 0.31495(2) 0.92745(4) 0.27495(2) 0.01519(10) Uani 1 1 d . . .
C1 C 0.29402(9) 0.67234(17) 0.29484(10) 0.0211(4) Uani 1 1 d . . .
H1A H 0.2947 0.6496 0.3447 0.032 Uiso 1 1 calc R . .
H1B H 0.3413 0.6751 0.2947 0.032 Uiso 1 1 calc R . .
H1C H 0.2677 0.6065 0.2592 0.032 Uiso 1 1 calc R . .
C8 C 0.21117(10) 0.7521(2) 0.41513(10) 0.0249(4) Uani 1 1 d . . .
H8A H 0.1855 0.7899 0.4446 0.037 Uiso 1 1 calc R . .
H8B H 0.2299 0.8225 0.3932 0.037 Uiso 1 1 calc R . .
H8C H 0.2490 0.6983 0.4473 0.037 Uiso 1 1 calc R . .
C4 C 0.13151(9) 0.56408(18) 0.37582(10) 0.0204(4) Uani 1 1 d . . .
H4 H 0.1404 0.5511 0.4273 0.024 Uiso 1 1 calc R . .
Cl2 Cl 0.46081(4) 0.25700(8) 0.31317(5) 0.0766(3) Uani 1 1 d . A .
C18 C 0.01125(10) 1.2328(2) 0.07084(12) 0.0326(5) Uani 1 1 d . . .
H18A H 0.0358 1.3165 0.0803 0.049 Uiso 1 1 calc R . .
H18B H -0.0302 1.2399 0.0841 0.049 Uiso 1 1 calc R . .
H18C H -0.0019 1.2106 0.0180 0.049 Uiso 1 1 calc R . .
N1 N 0.26089(7) 0.80398(14) 0.27315(8) 0.0157(3) Uani 1 1 d . . .
C23 C 0.37008(11) 0.9353(2) 0.06425(11) 0.0332(5) Uani 1 1 d . . .
H23 H 0.3821 0.9356 0.0208 0.040 Uiso 1 1 calc R . .
C22 C 0.36760(12) 1.0514(2) 0.09975(12) 0.0347(5) Uani 1 1 d . . .
H22 H 0.3780 1.1311 0.0805 0.042 Uiso 1 1 calc R . .
C21 C 0.35001(10) 1.05288(19) 0.16349(11) 0.0263(4) Uani 1 1 d . . .
H21 H 0.3487 1.1329 0.1881 0.032 Uiso 1 1 calc R . .
C20 C 0.33428(9) 0.93529(17) 0.19089(9) 0.0189(3) Uani 1 1 d . . .
B1 B 0.18642(9) 0.81043(19) 0.25173(10) 0.0154(4) Uani 1 1 d . . .
C2 C 0.15026(8) 0.69177(17) 0.27732(9) 0.0166(3) Uani 1 1 d . . .
C3 C 0.16345(9) 0.66805(17) 0.35389(9) 0.0186(3) Uani 1 1 d . . .
C5 C 0.08725(9) 0.47883(17) 0.32528(10) 0.0204(4) Uani 1 1 d . . .
C9 C 0.05509(10) 0.36490(19) 0.35098(12) 0.0281(4) Uani 1 1 d . . .
H9A H 0.0174 0.3291 0.3087 0.042 Uiso 1 1 calc R . .
H9B H 0.0371 0.3945 0.3892 0.042 Uiso 1 1 calc R . .
H9C H 0.0899 0.2971 0.3717 0.042 Uiso 1 1 calc R . .
C29 C 0.51892(10) 0.8386(2) 0.46158(12) 0.0343(5) Uani 1 1 d . . .
H29 H 0.5614 0.8201 0.5000 0.041 Uiso 1 1 calc R . .
C30 C 0.45780(10) 0.8267(2) 0.47535(11) 0.0309(4) Uani 1 1 d . . .
H30 H 0.4585 0.8006 0.5231 0.037 Uiso 1 1 calc R . .
C31 C 0.39552(9) 0.85278(19) 0.41931(10) 0.0245(4) Uani 1 1 d . . .
H31 H 0.3535 0.8446 0.4286 0.029 Uiso 1 1 calc R . .
C26 C 0.39488(8) 0.89123(17) 0.34901(10) 0.0190(3) Uani 1 1 d . . .
C7 C 0.10412(8) 0.60661(17) 0.22558(9) 0.0179(3) Uani 1 1 d . . .
C6 C 0.07453(9) 0.50221(17) 0.25024(10) 0.0205(4) Uani 1 1 d . . .
H6 H 0.0446 0.4449 0.2145 0.025 Uiso 1 1 calc R . .
C10 C 0.08702(10) 0.62231(19) 0.14269(10) 0.0255(4) Uani 1 1 d . . .
H10A H 0.1282 0.6046 0.1301 0.038 Uiso 1 1 calc R . .
H10B H 0.0713 0.7118 0.1281 0.038 Uiso 1 1 calc R . .
H10C H 0.0505 0.5607 0.1162 0.038 Uiso 1 1 calc R . .
C11 C 0.14329(8) 0.92744(17) 0.20427(9) 0.0168(3) Uani 1 1 d . . .
C16 C 0.10636(8) 1.01321(17) 0.23492(10) 0.0184(3) Uani 1 1 d . . .
C15 C 0.06548(9) 1.11153(18) 0.19170(10) 0.0220(4) Uani 1 1 d . . .
H15 H 0.0423 1.1697 0.2137 0.026 Uiso 1 1 calc R . .
C14 C 0.05742(9) 1.12741(18) 0.11710(11) 0.0232(4) Uani 1 1 d . . .
C13 C 0.09266(9) 1.04262(18) 0.08679(10) 0.0221(4) Uani 1 1 d . . .
H13 H 0.0874 1.0516 0.0358 0.026 Uiso 1 1 calc R . .
C12 C 0.13566(8) 0.94421(17) 0.12874(9) 0.0189(3) Uani 1 1 d . . .
C17 C 0.17076(9) 0.8579(2) 0.08876(10) 0.0236(4) Uani 1 1 d . . .
H17A H 0.1360 0.8176 0.0456 0.035 Uiso 1 1 calc R . .
H17B H 0.1969 0.7894 0.1226 0.035 Uiso 1 1 calc R . .
H17C H 0.2022 0.9107 0.0722 0.035 Uiso 1 1 calc R . .
C19 C 0.11237(10) 1.0021(2) 0.31511(10) 0.0248(4) Uani 1 1 d . . .
H19A H 0.0804 1.0636 0.3252 0.037 Uiso 1 1 calc R . .
H19B H 0.1596 1.0228 0.3471 0.037 Uiso 1 1 calc R . .
H19C H 0.1010 0.9128 0.3253 0.037 Uiso 1 1 calc R . .
C32 C 0.28419(8) 1.08245(17) 0.29458(10) 0.0182(3) Uani 1 1 d . . .
C37 C 0.30105(10) 1.11989(19) 0.36909(11) 0.0246(4) Uani 1 1 d . . .
H37 H 0.3267 1.0625 0.4077 0.029 Uiso 1 1 calc R . .
C36 C 0.28026(11) 1.2408(2) 0.38632(12) 0.0312(4) Uani 1 1 d . . .
H36 H 0.2916 1.2662 0.4368 0.037 Uiso 1 1 calc R . .
C35 C 0.24290(10) 1.3246(2) 0.32988(13) 0.0313(5) Uani 1 1 d . . .
H35 H 0.2287 1.4074 0.3418 0.038 Uiso 1 1 calc R . .
C34 C 0.22625(10) 1.28823(19) 0.25642(12) 0.0289(4) Uani 1 1 d . . .
H34 H 0.2009 1.3463 0.2181 0.035 Uiso 1 1 calc R . .
C33 C 0.24633(9) 1.16747(18) 0.23829(11) 0.0233(4) Uani 1 1 d . . .
H33 H 0.2343 1.1426 0.1877 0.028 Uiso 1 1 calc R . .
C24 C 0.35517(10) 0.8185(2) 0.09165(11) 0.0276(4) Uani 1 1 d . . .
H24 H 0.3572 0.7387 0.0672 0.033 Uiso 1 1 calc R . .
C25 C 0.33721(9) 0.81794(18) 0.15475(10) 0.0218(4) Uani 1 1 d . . .
H25 H 0.3269 0.7377 0.1735 0.026 Uiso 1 1 calc R . .
C27 C 0.45671(9) 0.90330(19) 0.33606(11) 0.0252(4) Uani 1 1 d . . .
H27 H 0.4566 0.9294 0.2885 0.030 Uiso 1 1 calc R . .
C28 C 0.51874(10) 0.8770(2) 0.39297(13) 0.0332(5) Uani 1 1 d . . .
H28 H 0.5610 0.8856 0.3843 0.040 Uiso 1 1 calc R . .
C38 C 0.19446(14) 0.3802(3) 0.03462(14) 0.0556(8) Uani 1 1 d . B .
C39 C 0.40982(18) 0.3956(4) 0.3001(2) 0.0780(10) Uani 1 1 d . . .
H39A H 0.3686 0.3832 0.2554 0.094 Uiso 0.492(2) 1 d PR A 1
H39B H 0.3959 0.4085 0.3441 0.094 Uiso 0.492(2) 1 d PR A 1
H39C H 0.4193 0.4555 0.2642 0.094 Uiso 0.508(2) 1 d PR A 2
H39D H 0.3604 0.3731 0.2825 0.094 Uiso 0.508(2) 1 d PR A 2
Cl1A Cl 0.45442(7) 0.53903(14) 0.28736(12) 0.0707(6) Uani 0.492(2) 1 d P A 1
Cl1B Cl 0.43814(7) 0.47128(17) 0.39543(9) 0.0677(6) Uani 0.508(2) 1 d P A 2
F1A F 0.18825(19) 0.3129(5) -0.0233(2) 0.0570(16) Uani 0.576(9) 1 d P B 1
F2A F 0.14801(17) 0.4934(5) 0.0013(2) 0.0533(12) Uani 0.576(9) 1 d P B 1
F3A F 0.1692(10) 0.324(2) 0.0830(10) 0.045(3) Uani 0.576(9) 1 d P B 1
O1A O 0.2963(7) 0.5180(9) 0.0244(8) 0.0353(14) Uani 0.576(9) 1 d P B 1
O2A O 0.2675(5) 0.5345(8) 0.1370(3) 0.0418(16) Uani 0.576(9) 1 d P B 1
O3A O 0.3142(2) 0.3350(4) 0.1081(3) 0.0433(11) Uani 0.576(9) 1 d P B 1
F1B F 0.2173(3) 0.2379(6) 0.0199(5) 0.076(3) Uani 0.424(9) 1 d P B 2
F2B F 0.1597(4) 0.4114(10) -0.0185(3) 0.086(4) Uani 0.424(9) 1 d P B 2
F3B F 0.1606(14) 0.343(3) 0.0763(13) 0.040(3) Uani 0.424(9) 1 d P B 2
O1B O 0.3064(10) 0.4808(14) 0.0291(12) 0.050(3) Uani 0.424(9) 1 d P B 2
O2B O 0.2523(6) 0.5615(11) 0.1129(7) 0.054(3) Uani 0.424(9) 1 d P B 2
O3B O 0.3217(3) 0.3668(8) 0.1432(4) 0.0494(18) Uani 0.424(9) 1 d P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O1B 1.39(2) . ?
S1 O2A 1.408(8) . ?
S1 O3A 1.409(4) . ?
S1 O2B 1.439(11) . ?
S1 O1A 1.467(14) . ?
S1 O3B 1.482(6) . ?
S1 C38 1.813(3) . ?
P1 N1 1.6806(14) . ?
P1 C20 1.7939(18) . ?
P1 C32 1.7974(18) . ?
P1 C26 1.8057(17) . ?
C1 N1 1.503(2) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C8 C3 1.513(2) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C4 C5 1.387(3) . ?
C4 C3 1.393(2) . ?
C4 H4 0.9500 . ?
Cl2 C39 1.733(4) . ?
C18 C14 1.508(3) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
N1 B1 1.453(2) . ?
C23 C22 1.379(3) . ?
C23 C24 1.383(3) . ?
C23 H23 0.9500 . ?
C22 C21 1.393(3) . ?
C22 H22 0.9500 . ?
C21 C20 1.396(3) . ?
C21 H21 0.9500 . ?
C20 C25 1.398(3) . ?
B1 C11 1.579(3) . ?
B1 C2 1.591(2) . ?
C2 C7 1.413(2) . ?
C2 C3 1.419(2) . ?
C5 C6 1.391(3) . ?
C5 C9 1.508(2) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C29 C28 1.373(3) . ?
C29 C30 1.386(3) . ?
C29 H29 0.9500 . ?
C30 C31 1.388(3) . ?
C30 H30 0.9500 . ?
C31 C26 1.401(3) . ?
C31 H31 0.9500 . ?
C26 C27 1.392(2) . ?
C7 C6 1.394(2) . ?
C7 C10 1.513(2) . ?
C6 H6 0.9500 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.413(2) . ?
C11 C16 1.419(2) . ?
C16 C15 1.389(3) . ?
C16 C19 1.504(2) . ?
C15 C14 1.392(3) . ?
C15 H15 0.9500 . ?
C14 C13 1.385(3) . ?
C13 C12 1.399(2) . ?
C13 H13 0.9500 . ?
C12 C17 1.512(2) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C32 C33 1.396(2) . ?
C32 C37 1.402(3) . ?
C37 C36 1.387(3) . ?
C37 H37 0.9500 . ?
C36 C35 1.387(3) . ?
C36 H36 0.9500 . ?
C35 C34 1.381(3) . ?
C35 H35 0.9500 . ?
C34 C33 1.386(3) . ?
C34 H34 0.9500 . ?
C33 H33 0.9500 . ?
C24 C25 1.385(3) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C27 C28 1.393(3) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C38 F2B 1.072(5) . ?
C38 F1A 1.274(4) . ?
C38 F3B 1.29(2) . ?
C38 F3A 1.343(17) . ?
C38 F2A 1.500(5) . ?
C38 F1B 1.586(7) . ?
C39 Cl1A 1.796(4) . ?
C39 Cl1B 1.883(4) . ?
C39 H39A 0.9862 . ?
C39 H39B 0.9906 . ?
C39 H39C 0.9904 . ?
C39 H39D 0.9862 . ?
Cl1A H39C 1.1102 . ?
Cl1B H39B 1.2445 . ?

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
O1B S1 O2A 129.6(8) . . ?
O1B S1 O3A 96.9(5) . . ?
O2A S1 O3A 117.2(3) . . ?
O1B S1 O2B 116.5(7) . . ?
O2A S1 O2B 21.7(4) . . ?
O3A S1 O2B 138.7(4) . . ?
O1B S1 O1A 17.0(8) . . ?
O2A S1 O1A 116.0(5) . . ?
O3A S1 O1A 113.8(4) . . ?
O2B S1 O1A 100.4(6) . . ?
O1B S1 O3B 113.8(7) . . ?
O2A S1 O3B 89.2(4) . . ?
O3A S1 O3B 28.5(3) . . ?
O2B S1 O3B 111.0(4) . . ?
O1A S1 O3B 128.2(5) . . ?
O1B S1 C38 106.3(9) . . ?
O2A S1 C38 104.8(4) . . ?
O3A S1 C38 97.3(2) . . ?
O2B S1 C38 95.8(5) . . ?
O1A S1 C38 104.4(6) . . ?
O3B S1 C38 111.9(3) . . ?
N1 P1 C20 111.77(8) . . ?
N1 P1 C32 112.66(7) . . ?
C20 P1 C32 110.82(8) . . ?
N1 P1 C26 106.49(8) . . ?
C20 P1 C26 106.65(8) . . ?
C32 P1 C26 108.12(8) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 C4 C3 122.48(16) . . ?
C5 C4 H4 118.8 . . ?
C3 C4 H4 118.8 . . ?
C14 C18 H18A 109.5 . . ?
C14 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C14 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
B1 N1 C1 117.16(14) . . ?
B1 N1 P1 127.29(12) . . ?
C1 N1 P1 115.54(11) . . ?
C22 C23 C24 120.33(18) . . ?
C22 C23 H23 119.8 . . ?
C24 C23 H23 119.8 . . ?
C23 C22 C21 120.60(19) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C22 C21 C20 119.23(19) . . ?
C22 C21 H21 120.4 . . ?
C20 C21 H21 120.4 . . ?
C21 C20 C25 119.81(16) . . ?
C21 C20 P1 122.10(14) . . ?
C25 C20 P1 117.99(13) . . ?
N1 B1 C11 121.97(15) . . ?
N1 B1 C2 116.45(15) . . ?
C11 B1 C2 121.57(14) . . ?
C7 C2 C3 117.48(15) . . ?
C7 C2 B1 121.96(15) . . ?
C3 C2 B1 120.56(15) . . ?
C4 C3 C2 120.20(16) . . ?
C4 C3 C8 116.74(15) . . ?
C2 C3 C8 123.06(16) . . ?
C4 C5 C6 117.17(16) . . ?
C4 C5 C9 121.14(17) . . ?
C6 C5 C9 121.68(17) . . ?
C5 C9 H9A 109.5 . . ?
C5 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C5 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C28 C29 C30 120.69(18) . . ?
C28 C29 H29 119.7 . . ?
C30 C29 H29 119.7 . . ?
C29 C30 C31 119.98(19) . . ?
C29 C30 H30 120.0 . . ?
C31 C30 H30 120.0 . . ?
C30 C31 C26 119.66(18) . . ?
C30 C31 H31 120.2 . . ?
C26 C31 H31 120.2 . . ?
C27 C26 C31 119.72(16) . . ?
C27 C26 P1 119.32(14) . . ?
C31 C26 P1 120.95(13) . . ?
C6 C7 C2 120.25(16) . . ?
C6 C7 C10 117.94(16) . . ?
C2 C7 C10 121.78(16) . . ?
C5 C6 C7 122.40(16) . . ?
C5 C6 H6 118.8 . . ?
C7 C6 H6 118.8 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C16 117.78(16) . . ?
C12 C11 B1 121.49(15) . . ?
C16 C11 B1 120.54(15) . . ?
C15 C16 C11 120.34(16) . . ?
C15 C16 C19 118.79(16) . . ?
C11 C16 C19 120.84(16) . . ?
C16 C15 C14 121.92(17) . . ?
C16 C15 H15 119.0 . . ?
C14 C15 H15 119.0 . . ?
C13 C14 C15 117.81(17) . . ?
C13 C14 C18 121.30(18) . . ?
C15 C14 C18 120.88(18) . . ?
C14 C13 C12 122.16(17) . . ?
C14 C13 H13 118.9 . . ?
C12 C13 H13 118.9 . . ?
C13 C12 C11 119.95(16) . . ?
C13 C12 C17 116.81(16) . . ?
C11 C12 C17 123.22(16) . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C33 C32 C37 119.50(17) . . ?
C33 C32 P1 122.16(14) . . ?
C37 C32 P1 118.31(14) . . ?
C36 C37 C32 119.93(18) . . ?
C36 C37 H37 120.0 . . ?
C32 C37 H37 120.0 . . ?
C37 C36 C35 120.04(19) . . ?
C37 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C34 C35 C36 120.23(18) . . ?
C34 C35 H35 119.9 . . ?
C36 C35 H35 119.9 . . ?
C35 C34 C33 120.44(19) . . ?
C35 C34 H34 119.8 . . ?
C33 C34 H34 119.8 . . ?
C34 C33 C32 119.87(18) . . ?
C34 C33 H33 120.1 . . ?
C32 C33 H33 120.1 . . ?
C23 C24 C25 119.94(19) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C24 C25 C20 120.09(17) . . ?
C24 C25 H25 120.0 . . ?
C20 C25 H25 120.0 . . ?
C26 C27 C28 119.86(18) . . ?
C26 C27 H27 120.1 . . ?
C28 C27 H27 120.1 . . ?
C29 C28 C27 120.08(19) . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
F2B C38 F1A 60.1(5) . . ?
F2B C38 F3B 110.3(14) . . ?
F1A C38 F3B 117.9(11) . . ?
F2B C38 F3A 119.4(10) . . ?
F1A C38 F3A 115.2(9) . . ?
F3B C38 F3A 11(2) . . ?
F2B C38 F2A 41.0(6) . . ?
F1A C38 F2A 101.0(3) . . ?
F3B C38 F2A 95.0(15) . . ?
F3A C38 F2A 106.2(10) . . ?
F2B C38 F1B 104.3(6) . . ?
F1A C38 F1B 45.2(3) . . ?
F3B C38 F1B 95.6(14) . . ?
F3A C38 F1B 86.7(10) . . ?
F2A C38 F1B 145.1(4) . . ?
F2B C38 S1 124.8(4) . . ?
F1A C38 S1 117.1(2) . . ?
F3B C38 S1 115.6(11) . . ?
F3A C38 S1 110.6(8) . . ?
F2A C38 S1 105.0(3) . . ?
F1B C38 S1 100.1(3) . . ?
Cl2 C39 Cl1A 111.84(19) . . ?
Cl2 C39 Cl1B 103.2(2) . . ?
Cl1A C39 Cl1B 78.16(17) . . ?
Cl2 C39 H39A 108.7 . . ?
Cl1A C39 H39A 108.6 . . ?
Cl1B C39 H39A 141.4 . . ?
Cl2 C39 H39B 109.2 . . ?
Cl1A C39 H39B 108.8 . . ?
Cl1B C39 H39B 37.1 . . ?
H39A C39 H39B 109.7 . . ?
Cl2 C39 H39C 110.5 . . ?
Cl1A C39 H39C 33.3 . . ?
Cl1B C39 H39C 110.5 . . ?
H39A C39 H39C 78.2 . . ?
H39B C39 H39C 134.1 . . ?
Cl2 C39 H39D 111.5 . . ?
Cl1A C39 H39D 131.7 . . ?
Cl1B C39 H39D 111.4 . . ?
H39A C39 H39D 35.9 . . ?
H39B C39 H39D 75.5 . . ?
H39C C39 H39D 109.8 . . ?
C39 Cl1A H39C 29.3 . . ?
C39 Cl1B H39B 28.7 . . ?

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
C20 P1 N1 B1 -95.13(15) . . . . ?
C32 P1 N1 B1 30.42(16) . . . . ?
C26 P1 N1 B1 148.78(14) . . . . ?
C20 P1 N1 C1 83.55(13) . . . . ?
C32 P1 N1 C1 -150.90(12) . . . . ?
C26 P1 N1 C1 -32.55(14) . . . . ?
C24 C23 C22 C21 -0.1(3) . . . . ?
C23 C22 C21 C20 -0.5(3) . . . . ?
C22 C21 C20 C25 0.8(3) . . . . ?
C22 C21 C20 P1 177.10(15) . . . . ?
N1 P1 C20 C21 150.42(15) . . . . ?
C32 P1 C20 C21 23.86(18) . . . . ?
C26 P1 C20 C21 -93.58(16) . . . . ?
N1 P1 C20 C25 -33.23(16) . . . . ?
C32 P1 C20 C25 -159.79(13) . . . . ?
C26 P1 C20 C25 82.76(15) . . . . ?
C1 N1 B1 C11 -160.01(15) . . . . ?
P1 N1 B1 C11 18.6(2) . . . . ?
C1 N1 B1 C2 18.9(2) . . . . ?
P1 N1 B1 C2 -162.47(12) . . . . ?
N1 B1 C2 C7 -115.47(17) . . . . ?
C11 B1 C2 C7 63.4(2) . . . . ?
N1 B1 C2 C3 64.7(2) . . . . ?
C11 B1 C2 C3 -116.46(18) . . . . ?
C5 C4 C3 C2 1.3(3) . . . . ?
C5 C4 C3 C8 -179.23(16) . . . . ?
C7 C2 C3 C4 0.0(2) . . . . ?
B1 C2 C3 C4 179.91(15) . . . . ?
C7 C2 C3 C8 -179.45(16) . . . . ?
B1 C2 C3 C8 0.4(3) . . . . ?
C3 C4 C5 C6 -1.1(3) . . . . ?
C3 C4 C5 C9 178.22(17) . . . . ?
C28 C29 C30 C31 0.4(3) . . . . ?
C29 C30 C31 C26 0.0(3) . . . . ?
C30 C31 C26 C27 -0.2(3) . . . . ?
C30 C31 C26 P1 -179.45(15) . . . . ?
N1 P1 C26 C27 133.15(15) . . . . ?
C20 P1 C26 C27 13.67(17) . . . . ?
C32 P1 C26 C27 -105.55(16) . . . . ?
N1 P1 C26 C31 -47.60(17) . . . . ?
C20 P1 C26 C31 -167.09(15) . . . . ?
C32 P1 C26 C31 73.70(17) . . . . ?
C3 C2 C7 C6 -1.4(2) . . . . ?
B1 C2 C7 C6 178.72(15) . . . . ?
C3 C2 C7 C10 -179.37(16) . . . . ?
B1 C2 C7 C10 0.8(2) . . . . ?
C4 C5 C6 C7 -0.3(3) . . . . ?
C9 C5 C6 C7 -179.65(16) . . . . ?
C2 C7 C6 C5 1.6(3) . . . . ?
C10 C7 C6 C5 179.64(16) . . . . ?
N1 B1 C11 C12 69.6(2) . . . . ?
C2 B1 C11 C12 -109.23(19) . . . . ?
N1 B1 C11 C16 -115.45(18) . . . . ?
C2 B1 C11 C16 65.7(2) . . . . ?
C12 C11 C16 C15 -1.3(2) . . . . ?
B1 C11 C16 C15 -176.45(15) . . . . ?
C12 C11 C16 C19 -179.45(16) . . . . ?
B1 C11 C16 C19 5.4(2) . . . . ?
C11 C16 C15 C14 2.0(3) . . . . ?
C19 C16 C15 C14 -179.86(16) . . . . ?
C16 C15 C14 C13 -1.0(3) . . . . ?
C16 C15 C14 C18 178.40(17) . . . . ?
C15 C14 C13 C12 -0.5(3) . . . . ?
C18 C14 C13 C12 -179.95(17) . . . . ?
C14 C13 C12 C11 1.1(3) . . . . ?
C14 C13 C12 C17 179.66(16) . . . . ?
C16 C11 C12 C13 -0.2(2) . . . . ?
B1 C11 C12 C13 174.91(15) . . . . ?
C16 C11 C12 C17 -178.63(16) . . . . ?
B1 C11 C12 C17 -3.5(3) . . . . ?
N1 P1 C32 C33 -94.15(15) . . . . ?
C20 P1 C32 C33 31.91(17) . . . . ?
C26 P1 C32 C33 148.45(15) . . . . ?
N1 P1 C32 C37 87.97(15) . . . . ?
C20 P1 C32 C37 -145.97(14) . . . . ?
C26 P1 C32 C37 -29.43(16) . . . . ?
C33 C32 C37 C36 -0.2(3) . . . . ?
P1 C32 C37 C36 177.74(15) . . . . ?
C32 C37 C36 C35 -0.1(3) . . . . ?
C37 C36 C35 C34 0.0(3) . . . . ?
C36 C35 C34 C33 0.3(3) . . . . ?
C35 C34 C33 C32 -0.6(3) . . . . ?
C37 C32 C33 C34 0.5(3) . . . . ?
P1 C32 C33 C34 -177.33(14) . . . . ?
C22 C23 C24 C25 0.4(3) . . . . ?
C23 C24 C25 C20 -0.1(3) . . . . ?
C21 C20 C25 C24 -0.5(3) . . . . ?
P1 C20 C25 C24 -176.92(14) . . . . ?
C31 C26 C27 C28 0.1(3) . . . . ?
P1 C26 C27 C28 179.32(16) . . . . ?
C30 C29 C28 C27 -0.6(3) . . . . ?
C26 C27 C28 C29 0.3(3) . . . . ?
O1B S1 C38 F2B -38.9(9) . . . . ?
O2A S1 C38 F2B 101.0(8) . . . . ?
O3A S1 C38 F2B -138.3(8) . . . . ?
O2B S1 C38 F2B 80.9(8) . . . . ?
O1A S1 C38 F2B -21.4(9) . . . . ?
O3B S1 C38 F2B -163.7(8) . . . . ?
O1B S1 C38 F1A 32.1(6) . . . . ?
O2A S1 C38 F1A 172.0(4) . . . . ?
O3A S1 C38 F1A -67.4(4) . . . . ?
O2B S1 C38 F1A 151.9(5) . . . . ?
O1A S1 C38 F1A 49.5(5) . . . . ?
O3B S1 C38 F1A -92.8(5) . . . . ?
O1B S1 C38 F3B 177.8(17) . . . . ?
O2A S1 C38 F3B -42.3(16) . . . . ?
O3A S1 C38 F3B 78.4(16) . . . . ?
O2B S1 C38 F3B -62.4(17) . . . . ?
O1A S1 C38 F3B -164.7(16) . . . . ?
O3B S1 C38 F3B 53.0(16) . . . . ?
O1B S1 C38 F3A 166.8(12) . . . . ?
O2A S1 C38 F3A -53.3(11) . . . . ?
O3A S1 C38 F3A 67.4(11) . . . . ?
O2B S1 C38 F3A -73.4(12) . . . . ?
O1A S1 C38 F3A -175.7(11) . . . . ?
O3B S1 C38 F3A 42.0(11) . . . . ?
O1B S1 C38 F2A -79.0(6) . . . . ?
O2A S1 C38 F2A 61.0(3) . . . . ?
O3A S1 C38 F2A -178.4(3) . . . . ?
O2B S1 C38 F2A 40.8(5) . . . . ?
O1A S1 C38 F2A -61.5(4) . . . . ?
O3B S1 C38 F2A 156.2(4) . . . . ?
O1B S1 C38 F1B 76.6(6) . . . . ?
O2A S1 C38 F1B -143.5(4) . . . . ?
O3A S1 C38 F1B -22.9(3) . . . . ?
O2B S1 C38 F1B -163.6(4) . . . . ?
O1A S1 C38 F1B 94.0(5) . . . . ?
O3B S1 C38 F1B -48.2(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.943
_refine_diff_density_min         -0.941
_refine_diff_density_rms         0.056
_database_code_depnum_ccdc_archive 'CCDC 1018471'
