# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013


#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material 
#  of the CCDC or of third parties, and may not be copied or further 
#  disseminated in any form, whether machine-readable or not,  
#  except for the purpose of generating routine backup copies 
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and 
#  data retrieval see:
#                         www.ccdc.cam.ac.uk 
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively. 
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data_compound_1b
_database_code_depnum_ccdc_archive 'CCDC 929289'
#TrackingRef 'cif_revised.txt'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H49 B N P'
_chemical_formula_sum            'C24 H49 B N P'
_chemical_formula_weight         393.42
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                   8.5008(4)
_cell_length_b                   10.7942(5)
_cell_length_c                   14.9113(6)
_cell_angle_alpha                97.788(2)
_cell_angle_beta                 100.943(2)
_cell_angle_gamma                106.893(2)
_cell_volume                     1258.65(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9996
_cell_measurement_theta_min      2.58
_cell_measurement_theta_max      27.50
_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    1.038
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             440
_exptl_absorpt_coefficient_mu    0.118
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9768
_exptl_absorpt_correction_T_max  0.9883
_exptl_absorpt_process_details   sadabs
_exptl_special_details           
;
APEX2, Bruker AXS, Madison, WI, USA.
;
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21428
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.01
_diffrn_reflns_theta_max         27.50
_reflns_number_total             5713
_reflns_number_gt                4675
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SHELXTL XPREP'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Mercury v3.0'
_computing_publication_material  'Bruker SHELXTL XCIF'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
Structure solved by direct methods to reveal all non-H atoms. All non-H
atoms refined aniostropically. H atoms added at calculated positions and
refined with a riding model.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+0.4071P] where P=(Fo^2^+2Fc^2^)/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         5713
_refine_ls_number_parameters     253
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0387
_refine_ls_wR_factor_ref         0.1025
_refine_ls_wR_factor_gt          0.0956
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_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
P1 P 0.20192(4) 1.09536(3) 0.27898(2) 0.01473(9) Uani 1 1 d . . .
N1 N 0.17536(13) 0.94541(10) 0.25750(7) 0.0181(2) Uani 1 1 d . . .
C44 C 0.2989(2) 1.13057(15) 0.47522(9) 0.0305(3) Uani 1 1 d . . .
H44A H 0.3914 1.1574 0.5316 0.046 Uiso 1 1 calc R . .
H44B H 0.2445 1.0345 0.4624 0.046 Uiso 1 1 calc R . .
H44C H 0.2153 1.1743 0.4845 0.046 Uiso 1 1 calc R . .
C41 C 0.37009(17) 1.17074(13) 0.39220(9) 0.0219(3) Uani 1 1 d . . .
B1 B 0.18179(17) 0.82258(14) 0.22009(9) 0.0165(3) Uani 1 1 d . . .
C21 C 0.09264(16) 0.69768(12) 0.26169(8) 0.0177(3) Uani 1 1 d . . .
H21 H 0.1291 0.6221 0.2377 0.021 Uiso 1 1 calc R . .
C26 C 0.14661(18) 0.72681(13) 0.36891(9) 0.0235(3) Uani 1 1 d . . .
H26A H 0.2705 0.7453 0.3887 0.028 Uiso 1 1 calc R . .
H26B H 0.1220 0.8072 0.3935 0.028 Uiso 1 1 calc R . .
C25 C 0.0575(2) 0.61363(14) 0.41134(9) 0.0299(3) Uani 1 1 d . . .
H25A H 0.0933 0.5362 0.3937 0.036 Uiso 1 1 calc R . .
H25B H 0.0909 0.6407 0.4802 0.036 Uiso 1 1 calc R . .
C24 C -0.1335(2) 0.57530(16) 0.37807(10) 0.0351(4) Uani 1 1 d . . .
H24A H -0.1705 0.6494 0.4023 0.042 Uiso 1 1 calc R . .
H24B H -0.1878 0.4978 0.4033 0.042 Uiso 1 1 calc R . .
C34 C 0.45628(18) 1.19021(15) 0.18629(10) 0.0300(3) Uani 1 1 d . . .
H34A H 0.4866 1.2191 0.1305 0.045 Uiso 1 1 calc R . .
H34B H 0.4675 1.1026 0.1878 0.045 Uiso 1 1 calc R . .
H34C H 0.5321 1.2534 0.2421 0.045 Uiso 1 1 calc R . .
C31 C 0.27174(18) 1.18313(13) 0.18383(9) 0.0227(3) Uani 1 1 d . . .
C11 C 0.26994(17) 0.79462(13) 0.13687(9) 0.0205(3) Uani 1 1 d . . .
H11 H 0.3184 0.8804 0.1180 0.025 Uiso 1 1 calc R . .
C12 C 0.13940(17) 0.69846(14) 0.05130(9) 0.0228(3) Uani 1 1 d . . .
H12A H 0.0842 0.6150 0.0699 0.027 Uiso 1 1 calc R . .
H12B H 0.0506 0.7375 0.0296 0.027 Uiso 1 1 calc R . .
C13 C 0.21932(19) 0.66774(15) -0.02912(9) 0.0272(3) Uani 1 1 d . . .
H13A H 0.1317 0.6025 -0.0811 0.033 Uiso 1 1 calc R . .
H13B H 0.2647 0.7494 -0.0522 0.033 Uiso 1 1 calc R . .
C14 C 0.3613(2) 0.61292(15) 0.00246(10) 0.0298(3) Uani 1 1 d . . .
H14A H 0.4147 0.5978 -0.0497 0.036 Uiso 1 1 calc R . .
H14B H 0.3140 0.5269 0.0199 0.036 Uiso 1 1 calc R . .
C16 C 0.41522(18) 0.73929(16) 0.16623(10) 0.0297(3) Uani 1 1 d . . .
H16A H 0.5039 0.8047 0.2177 0.036 Uiso 1 1 calc R . .
H16B H 0.3714 0.6578 0.1899 0.036 Uiso 1 1 calc R . .
C22 C -0.10153(17) 0.65548(13) 0.22934(9) 0.0223(3) Uani 1 1 d . . .
H22A H -0.1387 0.7323 0.2469 0.027 Uiso 1 1 calc R . .
H22B H -0.1356 0.6282 0.1605 0.027 Uiso 1 1 calc R . .
C23 C -0.19084(19) 0.54172(14) 0.27173(10) 0.0303(3) Uani 1 1 d . . .
H23A H -0.3149 0.5229 0.2525 0.036 Uiso 1 1 calc R . .
H23B H -0.1657 0.4612 0.2478 0.036 Uiso 1 1 calc R . .
C51 C -0.00598(17) 1.11554(13) 0.29314(10) 0.0235(3) Uani 1 1 d . . .
C54 C 0.0068(2) 1.25601(15) 0.33815(12) 0.0348(4) Uani 1 1 d . . .
H54A H -0.1068 1.2594 0.3392 0.052 Uiso 1 1 calc R . .
H54B H 0.0583 1.3188 0.3018 0.052 Uiso 1 1 calc R . .
H54C H 0.0771 1.2794 0.4021 0.052 Uiso 1 1 calc R . .
C53 C -0.08463(19) 1.01905(15) 0.35208(12) 0.0323(3) Uani 1 1 d . . .
H53A H -0.2025 1.0151 0.3479 0.048 Uiso 1 1 calc R . .
H53B H -0.0203 1.0498 0.4173 0.048 Uiso 1 1 calc R . .
H53C H -0.0812 0.9308 0.3286 0.048 Uiso 1 1 calc R . .
C52 C -0.13066(19) 1.07483(17) 0.19673(12) 0.0378(4) Uani 1 1 d . . .
H52A H -0.1285 0.9904 0.1641 0.057 Uiso 1 1 calc R . .
H52B H -0.0977 1.1428 0.1602 0.057 Uiso 1 1 calc R . .
H52C H -0.2453 1.0653 0.2044 0.057 Uiso 1 1 calc R . .
C43 C 0.51269(18) 1.10989(15) 0.38986(10) 0.0305(3) Uani 1 1 d . . .
H43A H 0.5716 1.1400 0.3423 0.046 Uiso 1 1 calc R . .
H43B H 0.4640 1.0132 0.3747 0.046 Uiso 1 1 calc R . .
H43C H 0.5933 1.1377 0.4510 0.046 Uiso 1 1 calc R . .
C42 C 0.4455(2) 1.32231(14) 0.41261(11) 0.0332(3) Uani 1 1 d . . .
H42A H 0.3546 1.3609 0.4137 0.050 Uiso 1 1 calc R . .
H42B H 0.5025 1.3500 0.3639 0.050 Uiso 1 1 calc R . .
H42C H 0.5276 1.3527 0.4733 0.050 Uiso 1 1 calc R . .
C33 C 0.2589(2) 1.32288(14) 0.18629(11) 0.0340(4) Uani 1 1 d . . .
H33A H 0.3212 1.3791 0.2475 0.051 Uiso 1 1 calc R . .
H33B H 0.1396 1.3179 0.1753 0.051 Uiso 1 1 calc R . .
H33C H 0.3076 1.3607 0.1376 0.051 Uiso 1 1 calc R . .
C32 C 0.1656(2) 1.09603(15) 0.08849(9) 0.0310(3) Uani 1 1 d . . .
H32A H 0.0511 1.1024 0.0773 0.046 Uiso 1 1 calc R . .
H32B H 0.1592 1.0039 0.0884 0.046 Uiso 1 1 calc R . .
H32C H 0.2190 1.1264 0.0392 0.046 Uiso 1 1 calc R . .
C15 C 0.4943(2) 0.70762(18) 0.08532(11) 0.0361(4) Uani 1 1 d . . .
H15A H 0.5495 0.7905 0.0661 0.043 Uiso 1 1 calc R . .
H15B H 0.5823 0.6677 0.1064 0.043 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.01473(16) 0.01263(16) 0.01690(15) 0.00301(11) 0.00409(12) 0.00437(12)
N1 0.0193(5) 0.0155(5) 0.0198(5) 0.0033(4) 0.0056(4) 0.0057(4)
C44 0.0413(9) 0.0305(8) 0.0193(6) 0.0032(6) 0.0065(6) 0.0125(7)
C41 0.0225(7) 0.0194(7) 0.0192(6) 0.0000(5) 0.0005(5) 0.0047(5)
B1 0.0147(6) 0.0165(7) 0.0161(6) 0.0024(5) 0.0014(5) 0.0038(6)
C21 0.0203(6) 0.0138(6) 0.0184(6) 0.0015(5) 0.0045(5) 0.0054(5)
C26 0.0294(7) 0.0186(7) 0.0188(6) 0.0031(5) 0.0017(5) 0.0050(6)
C25 0.0462(9) 0.0214(7) 0.0202(6) 0.0067(5) 0.0077(6) 0.0076(7)
C24 0.0427(9) 0.0303(8) 0.0314(8) 0.0091(6) 0.0184(7) 0.0031(7)
C34 0.0272(8) 0.0297(8) 0.0345(8) 0.0107(6) 0.0160(6) 0.0039(6)
C31 0.0262(7) 0.0197(7) 0.0228(6) 0.0083(5) 0.0073(5) 0.0055(6)
C11 0.0241(7) 0.0155(6) 0.0235(6) 0.0034(5) 0.0097(5) 0.0065(5)
C12 0.0244(7) 0.0282(7) 0.0183(6) 0.0043(5) 0.0056(5) 0.0124(6)
C13 0.0349(8) 0.0301(8) 0.0194(6) 0.0047(6) 0.0090(6) 0.0135(7)
C14 0.0413(9) 0.0294(8) 0.0283(7) 0.0064(6) 0.0178(6) 0.0195(7)
C16 0.0214(7) 0.0424(9) 0.0245(7) -0.0005(6) 0.0039(5) 0.0135(7)
C22 0.0213(7) 0.0186(7) 0.0228(6) 0.0028(5) 0.0034(5) 0.0022(5)
C23 0.0274(8) 0.0237(7) 0.0330(8) 0.0051(6) 0.0084(6) -0.0024(6)
C51 0.0191(7) 0.0202(7) 0.0342(7) 0.0044(6) 0.0092(6) 0.0098(6)
C54 0.0375(9) 0.0258(8) 0.0518(9) 0.0081(7) 0.0211(7) 0.0195(7)
C53 0.0249(7) 0.0280(8) 0.0505(9) 0.0091(7) 0.0220(7) 0.0097(6)
C52 0.0199(7) 0.0458(10) 0.0467(9) 0.0072(8) 0.0015(7) 0.0144(7)
C43 0.0220(7) 0.0361(8) 0.0289(7) 0.0032(6) -0.0034(6) 0.0104(6)
C42 0.0333(8) 0.0227(7) 0.0317(7) -0.0033(6) 0.0002(6) -0.0002(6)
C33 0.0462(9) 0.0231(7) 0.0372(8) 0.0163(6) 0.0129(7) 0.0116(7)
C32 0.0396(9) 0.0344(8) 0.0195(6) 0.0084(6) 0.0050(6) 0.0132(7)
C15 0.0272(8) 0.0517(10) 0.0346(8) 0.0033(7) 0.0117(6) 0.0202(7)
_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 1.5469(11) . ?
P1 C51 1.8890(13) . ?
P1 C41 1.8951(13) . ?
P1 C31 1.9026(13) . ?
N1 B1 1.3876(17) . ?
C44 C41 1.5376(19) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C41 C42 1.5368(19) . ?
C41 C43 1.5410(19) . ?
B1 C11 1.6048(18) . ?
B1 C21 1.6088(19) . ?
C21 C22 1.5381(18) . ?
C21 C26 1.5385(17) . ?
C21 H21 1.0000 . ?
C26 C25 1.5233(19) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C25 C24 1.517(2) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C24 C23 1.527(2) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C34 C31 1.541(2) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C31 C33 1.5399(19) . ?
C31 C32 1.5418(19) . ?
C11 C16 1.5388(19) . ?
C11 C12 1.5397(18) . ?
C11 H11 1.0000 . ?
C12 C13 1.5303(18) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.518(2) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.518(2) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C16 C15 1.5341(19) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C22 C23 1.5279(19) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C51 C54 1.5369(19) . ?
C51 C52 1.537(2) . ?
C51 C53 1.540(2) . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C15 H15A 0.9900 . ?
C15 H15B 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 C51 107.54(6) . . ?
N1 P1 C41 107.67(6) . . ?
C51 P1 C41 110.08(6) . . ?
N1 P1 C31 113.35(6) . . ?
C51 P1 C31 109.14(6) . . ?
C41 P1 C31 109.02(6) . . ?
B1 N1 P1 162.80(10) . . ?
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 . . ?
C42 C41 C44 107.86(11) . . ?
C42 C41 C43 109.55(12) . . ?
C44 C41 C43 105.56(11) . . ?
C42 C41 P1 115.08(9) . . ?
C44 C41 P1 110.40(9) . . ?
C43 C41 P1 107.97(9) . . ?
N1 B1 C11 124.88(12) . . ?
N1 B1 C21 118.12(11) . . ?
C11 B1 C21 116.99(11) . . ?
C22 C21 C26 109.71(11) . . ?
C22 C21 B1 111.17(10) . . ?
C26 C21 B1 111.59(10) . . ?
C22 C21 H21 108.1 . . ?
C26 C21 H21 108.1 . . ?
B1 C21 H21 108.1 . . ?
C25 C26 C21 113.23(11) . . ?
C25 C26 H26A 108.9 . . ?
C21 C26 H26A 108.9 . . ?
C25 C26 H26B 108.9 . . ?
C21 C26 H26B 108.9 . . ?
H26A C26 H26B 107.7 . . ?
C24 C25 C26 111.08(12) . . ?
C24 C25 H25A 109.4 . . ?
C26 C25 H25A 109.4 . . ?
C24 C25 H25B 109.4 . . ?
C26 C25 H25B 109.4 . . ?
H25A C25 H25B 108.0 . . ?
C25 C24 C23 111.56(12) . . ?
C25 C24 H24A 109.3 . . ?
C23 C24 H24A 109.3 . . ?
C25 C24 H24B 109.3 . . ?
C23 C24 H24B 109.3 . . ?
H24A C24 H24B 108.0 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C31 C34 108.62(12) . . ?
C33 C31 C32 108.01(11) . . ?
C34 C31 C32 105.66(11) . . ?
C33 C31 P1 117.09(10) . . ?
C34 C31 P1 108.59(9) . . ?
C32 C31 P1 108.29(9) . . ?
C16 C11 C12 109.21(10) . . ?
C16 C11 B1 112.55(11) . . ?
C12 C11 B1 111.04(11) . . ?
C16 C11 H11 108.0 . . ?
C12 C11 H11 108.0 . . ?
B1 C11 H11 108.0 . . ?
C13 C12 C11 112.56(11) . . ?
C13 C12 H12A 109.1 . . ?
C11 C12 H12A 109.1 . . ?
C13 C12 H12B 109.1 . . ?
C11 C12 H12B 109.1 . . ?
H12A C12 H12B 107.8 . . ?
C14 C13 C12 110.77(11) . . ?
C14 C13 H13A 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 108.1 . . ?
C13 C14 C15 111.03(12) . . ?
C13 C14 H14A 109.4 . . ?
C15 C14 H14A 109.4 . . ?
C13 C14 H14B 109.4 . . ?
C15 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C15 C16 C11 112.28(12) . . ?
C15 C16 H16A 109.1 . . ?
C11 C16 H16A 109.1 . . ?
C15 C16 H16B 109.1 . . ?
C11 C16 H16B 109.1 . . ?
H16A C16 H16B 107.9 . . ?
C23 C22 C21 112.66(11) . . ?
C23 C22 H22A 109.1 . . ?
C21 C22 H22A 109.1 . . ?
C23 C22 H22B 109.1 . . ?
C21 C22 H22B 109.1 . . ?
H22A C22 H22B 107.8 . . ?
C24 C23 C22 111.20(11) . . ?
C24 C23 H23A 109.4 . . ?
C22 C23 H23A 109.4 . . ?
C24 C23 H23B 109.4 . . ?
C22 C23 H23B 109.4 . . ?
H23A C23 H23B 108.0 . . ?
C54 C51 C52 108.90(12) . . ?
C54 C51 C53 108.57(12) . . ?
C52 C51 C53 106.18(12) . . ?
C54 C51 P1 114.62(10) . . ?
C52 C51 P1 108.69(10) . . ?
C53 C51 P1 109.55(9) . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 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 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 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C14 C15 C16 111.19(12) . . ?
C14 C15 H15A 109.4 . . ?
C16 C15 H15A 109.4 . . ?
C14 C15 H15B 109.4 . . ?
C16 C15 H15B 109.4 . . ?
H15A C15 H15B 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
C51 P1 N1 B1 140.2(3) . . . . ?
C41 P1 N1 B1 -101.2(3) . . . . ?
C31 P1 N1 B1 19.5(3) . . . . ?
N1 P1 C41 C42 165.44(10) . . . . ?
C51 P1 C41 C42 -77.60(12) . . . . ?
C31 P1 C41 C42 42.08(12) . . . . ?
N1 P1 C41 C44 -72.19(10) . . . . ?
C51 P1 C41 C44 44.76(11) . . . . ?
C31 P1 C41 C44 164.45(9) . . . . ?
N1 P1 C41 C43 42.74(11) . . . . ?
C51 P1 C41 C43 159.69(10) . . . . ?
C31 P1 C41 C43 -80.62(11) . . . . ?
P1 N1 B1 C11 -5.0(4) . . . . ?
P1 N1 B1 C21 175.8(3) . . . . ?
N1 B1 C21 C22 73.44(14) . . . . ?
C11 B1 C21 C22 -105.79(12) . . . . ?
N1 B1 C21 C26 -49.40(15) . . . . ?
C11 B1 C21 C26 131.37(12) . . . . ?
C22 C21 C26 C25 53.16(15) . . . . ?
B1 C21 C26 C25 176.83(11) . . . . ?
C21 C26 C25 C24 -54.95(16) . . . . ?
C26 C25 C24 C23 55.19(16) . . . . ?
N1 P1 C31 C33 165.23(10) . . . . ?
C51 P1 C31 C33 45.41(12) . . . . ?
C41 P1 C31 C33 -74.87(12) . . . . ?
N1 P1 C31 C34 -71.37(10) . . . . ?
C51 P1 C31 C34 168.81(9) . . . . ?
C41 P1 C31 C34 48.53(11) . . . . ?
N1 P1 C31 C32 42.90(11) . . . . ?
C51 P1 C31 C32 -76.92(10) . . . . ?
C41 P1 C31 C32 162.81(9) . . . . ?
N1 B1 C11 C16 119.31(14) . . . . ?
C21 B1 C11 C16 -61.51(15) . . . . ?
N1 B1 C11 C12 -117.91(13) . . . . ?
C21 B1 C11 C12 61.27(14) . . . . ?
C16 C11 C12 C13 -54.46(15) . . . . ?
B1 C11 C12 C13 -179.15(11) . . . . ?
C11 C12 C13 C14 56.45(16) . . . . ?
C12 C13 C14 C15 -56.43(17) . . . . ?
C12 C11 C16 C15 53.93(16) . . . . ?
B1 C11 C16 C15 177.73(12) . . . . ?
C26 C21 C22 C23 -53.00(14) . . . . ?
B1 C21 C22 C23 -176.91(11) . . . . ?
C25 C24 C23 C22 -55.42(17) . . . . ?
C21 C22 C23 C24 54.94(16) . . . . ?
N1 P1 C51 C54 165.61(10) . . . . ?
C41 P1 C51 C54 48.57(12) . . . . ?
C31 P1 C51 C54 -71.04(12) . . . . ?
N1 P1 C51 C52 -72.30(11) . . . . ?
C41 P1 C51 C52 170.66(10) . . . . ?
C31 P1 C51 C52 51.04(11) . . . . ?
N1 P1 C51 C53 43.30(11) . . . . ?
C41 P1 C51 C53 -73.73(11) . . . . ?
C31 P1 C51 C53 166.65(9) . . . . ?
C13 C14 C15 C16 56.30(18) . . . . ?
C11 C16 C15 C14 -55.84(18) . . . . ?
_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.042


data_compound_1c
_database_code_depnum_ccdc_archive 'CCDC 929290'
#TrackingRef 'cif_revised.txt'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H55 B N P'
_chemical_formula_sum            'C30 H55 B N P'
_chemical_formula_weight         471.53
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                   10.639(4)
_cell_length_b                   20.992(7)
_cell_length_c                   22.501(8)
_cell_angle_alpha                63.106(9)
_cell_angle_beta                 80.088(11)
_cell_angle_gamma                88.865(10)
_cell_volume                     4405(3)
_cell_formula_units_Z            6
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9690
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      27.45
_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    1.067
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1572
_exptl_absorpt_coefficient_mu    0.111
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9674
_exptl_absorpt_correction_T_max  0.9781
_exptl_absorpt_process_details   sadabs
_exptl_special_details           
;
APEX2, Bruker AXS, Winsconsin, USA
;
_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  'APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            75864
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.81
_diffrn_reflns_theta_max         27.50
_reflns_number_total             20005
_reflns_number_gt                13873
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The structure was solved by direct methods with remaining non-H atoms
located in subsequent difference maps. Residual electron density maps
revealed many of the cyclohexyl rings were disordered (peaks > 1e^-^/A^3^)
and each ring was either; (i) modelled over two sites with common U(iso)
for chemically equivalent C atoms and their geometry restrained to a
cyclohexyl ring (SAME); or (ii) if there was no evident disorder then the
C atoms were refined anisotropically. H atoms were added at calculated
positions and refined with a riding model.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+5.2035P] where P=(Fo^2^+2Fc^2^)/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         20005
_refine_ls_number_parameters     801
_refine_ls_number_restraints     1260
_refine_ls_R_factor_all          0.1058
_refine_ls_R_factor_gt           0.0694
_refine_ls_wR_factor_ref         0.1668
_refine_ls_wR_factor_gt          0.1484
_refine_ls_goodness_of_fit_ref   1.011
_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
P1 P 0.39223(6) 0.38344(3) 0.81562(3) 0.01946(13) Uani 1 1 d . . .
B1 B 0.2693(2) 0.48077(14) 0.85231(14) 0.0224(5) Uani 1 1 d . . .
N1 N 0.32216(19) 0.45322(10) 0.80770(10) 0.0255(4) Uani 1 1 d . A .
C11 C 0.4170(8) 0.3817(5) 0.7323(4) 0.0214(6) Uiso 0.531(5) 1 d PD A 1
H11 H 0.4672 0.3397 0.7360 0.026 Uiso 0.531(5) 1 calc PR A 1
C12 C 0.2880(8) 0.3731(4) 0.7141(4) 0.0262(5) Uiso 0.531(5) 1 d PD A 1
H12A H 0.2434 0.3269 0.7486 0.031 Uiso 0.531(5) 1 calc PR A 1
H12B H 0.2341 0.4119 0.7146 0.031 Uiso 0.531(5) 1 calc PR A 1
C13 C 0.3041(8) 0.3755(5) 0.6447(4) 0.0297(6) Uiso 0.531(5) 1 d PD A 1
H13A H 0.3484 0.3332 0.6457 0.036 Uiso 0.531(5) 1 calc PR A 1
H13B H 0.2188 0.3735 0.6334 0.036 Uiso 0.531(5) 1 calc PR A 1
C14 C 0.3802(5) 0.4428(3) 0.5906(3) 0.0306(8) Uiso 0.531(5) 1 d PD A 1
H14A H 0.3317 0.4850 0.5863 0.037 Uiso 0.531(5) 1 calc PR A 1
H14B H 0.3929 0.4417 0.5465 0.037 Uiso 0.531(5) 1 calc PR A 1
C15 C 0.5108(5) 0.4502(3) 0.6079(2) 0.0297(6) Uiso 0.531(5) 1 d PD A 1
H15A H 0.5575 0.4955 0.5726 0.036 Uiso 0.531(5) 1 calc PR A 1
H15B H 0.5622 0.4100 0.6087 0.036 Uiso 0.531(5) 1 calc PR A 1
C16 C 0.4931(5) 0.4498(3) 0.6772(2) 0.0262(5) Uiso 0.531(5) 1 d PD A 1
H16A H 0.5780 0.4529 0.6885 0.031 Uiso 0.531(5) 1 calc PR A 1
H16B H 0.4476 0.4921 0.6751 0.031 Uiso 0.531(5) 1 calc PR A 1
C11A C 0.4236(9) 0.3770(6) 0.7372(5) 0.0214(6) Uiso 0.469(5) 1 d PD A 2
H11A H 0.4534 0.3281 0.7481 0.026 Uiso 0.469(5) 1 calc PR A 2
C12A C 0.2965(8) 0.3821(5) 0.7101(4) 0.0262(5) Uiso 0.469(5) 1 d PD A 2
H12C H 0.2332 0.3439 0.7448 0.031 Uiso 0.469(5) 1 calc PR A 2
H12D H 0.2610 0.4289 0.7013 0.031 Uiso 0.469(5) 1 calc PR A 2
C13A C 0.3199(9) 0.3743(6) 0.6437(5) 0.0297(6) Uiso 0.469(5) 1 d PD A 2
H13C H 0.3465 0.3255 0.6537 0.036 Uiso 0.469(5) 1 calc PR A 2
H13D H 0.2390 0.3803 0.6261 0.036 Uiso 0.469(5) 1 calc PR A 2
C14A C 0.4213(6) 0.4287(3) 0.5901(3) 0.0306(8) Uiso 0.469(5) 1 d PD A 2
H14C H 0.3919 0.4775 0.5770 0.037 Uiso 0.469(5) 1 calc PR A 2
H14D H 0.4361 0.4209 0.5493 0.037 Uiso 0.469(5) 1 calc PR A 2
C15A C 0.5462(6) 0.4222(4) 0.6169(3) 0.0297(6) Uiso 0.469(5) 1 d PD A 2
H15C H 0.5792 0.3748 0.6260 0.036 Uiso 0.469(5) 1 calc PR A 2
H15D H 0.6106 0.4594 0.5819 0.036 Uiso 0.469(5) 1 calc PR A 2
C16A C 0.5269(6) 0.4306(3) 0.6818(3) 0.0262(5) Uiso 0.469(5) 1 d PD A 2
H16C H 0.6086 0.4237 0.6987 0.031 Uiso 0.469(5) 1 calc PR A 2
H16D H 0.5027 0.4798 0.6715 0.031 Uiso 0.469(5) 1 calc PR A 2
C21 C 0.2997(4) 0.3007(2) 0.8808(2) 0.0220(7) Uiso 0.602(2) 1 d PD A 1
H21 H 0.3234 0.2925 0.9247 0.026 Uiso 0.602(2) 1 calc PR A 1
C22 C 0.1532(5) 0.3063(3) 0.8902(3) 0.0264(5) Uiso 0.602(2) 1 d PD A 1
H22A H 0.1319 0.3502 0.8948 0.032 Uiso 0.602(2) 1 calc PR A 1
H22B H 0.1226 0.3099 0.8497 0.032 Uiso 0.602(2) 1 calc PR A 1
C23 C 0.0860(4) 0.2411(2) 0.9530(2) 0.0333(6) Uiso 0.602(2) 1 d PD A 1
H23A H -0.0077 0.2441 0.9561 0.040 Uiso 0.602(2) 1 calc PR A 1
H23B H 0.1084 0.2413 0.9939 0.040 Uiso 0.602(2) 1 calc PR A 1
C24 C 0.1231(4) 0.1708(2) 0.9518(2) 0.0369(9) Uiso 0.602(2) 1 d PD A 1
H24A H 0.0866 0.1301 0.9960 0.044 Uiso 0.602(2) 1 calc PR A 1
H24B H 0.0861 0.1663 0.9163 0.044 Uiso 0.602(2) 1 calc PR A 1
C25 C 0.2672(4) 0.1668(2) 0.9379(2) 0.0333(6) Uiso 0.602(2) 1 d PD A 1
H25A H 0.2868 0.1229 0.9330 0.040 Uiso 0.602(2) 1 calc PR A 1
H25B H 0.3028 0.1637 0.9769 0.040 Uiso 0.602(2) 1 calc PR A 1
C26 C 0.3313(4) 0.2323(2) 0.8734(2) 0.0264(5) Uiso 0.602(2) 1 d PD A 1
H26A H 0.2999 0.2343 0.8337 0.032 Uiso 0.602(2) 1 calc PR A 1
H26B H 0.4251 0.2285 0.8663 0.032 Uiso 0.602(2) 1 calc PR A 1
C21A C 0.3119(6) 0.2908(4) 0.8727(3) 0.0220(7) Uiso 0.398(2) 1 d PD A 2
H21A H 0.3305 0.2626 0.8466 0.026 Uiso 0.398(2) 1 calc PR A 2
C22A C 0.1651(7) 0.2948(4) 0.8852(4) 0.0264(5) Uiso 0.398(2) 1 d PD A 2
H22C H 0.1419 0.3219 0.9113 0.032 Uiso 0.398(2) 1 calc PR A 2
H22D H 0.1367 0.3208 0.8411 0.032 Uiso 0.398(2) 1 calc PR A 2
C23A C 0.0954(6) 0.2195(3) 0.9244(3) 0.0333(6) Uiso 0.398(2) 1 d PD A 2
H23C H 0.0022 0.2240 0.9341 0.040 Uiso 0.398(2) 1 calc PR A 2
H23D H 0.1106 0.1941 0.8961 0.040 Uiso 0.398(2) 1 calc PR A 2
C24A C 0.1427(6) 0.1767(4) 0.9902(3) 0.0369(9) Uiso 0.398(2) 1 d PD A 2
H24C H 0.1010 0.1277 1.0131 0.044 Uiso 0.398(2) 1 calc PR A 2
H24D H 0.1185 0.1993 1.0204 0.044 Uiso 0.398(2) 1 calc PR A 2
C25A C 0.2875(6) 0.1725(3) 0.9782(3) 0.0333(6) Uiso 0.398(2) 1 d PD A 2
H25C H 0.3110 0.1461 0.9513 0.040 Uiso 0.398(2) 1 calc PR A 2
H25D H 0.3155 0.1456 1.0223 0.040 Uiso 0.398(2) 1 calc PR A 2
C26A C 0.3570(6) 0.2474(3) 0.9404(3) 0.0264(5) Uiso 0.398(2) 1 d PD A 2
H26C H 0.3392 0.2726 0.9687 0.032 Uiso 0.398(2) 1 calc PR A 2
H26D H 0.4504 0.2430 0.9319 0.032 Uiso 0.398(2) 1 calc PR A 2
C31 C 0.5479(2) 0.38242(12) 0.84214(12) 0.0267(5) Uani 1 1 d D A .
H31 H 0.5263 0.3672 0.8919 0.032 Uiso 1 1 calc R . .
C32 C 0.6189(2) 0.45663(13) 0.81109(14) 0.0307(6) Uani 1 1 d D . .
H32A H 0.6463 0.4742 0.7616 0.037 Uiso 1 1 calc R A .
H32B H 0.5603 0.4907 0.8183 0.037 Uiso 1 1 calc R . .
C33 C 0.7362(3) 0.45332(16) 0.84329(16) 0.0429(7) Uani 1 1 d D A .
H33A H 0.7825 0.5011 0.8207 0.051 Uiso 1 1 calc R . .
H33B H 0.7076 0.4409 0.8917 0.051 Uiso 1 1 calc R . .
C34 C 0.8262(3) 0.39890(16) 0.83773(17) 0.0465(8) Uani 1 1 d D . .
H34A H 0.8975 0.3963 0.8617 0.056 Uiso 1 1 calc R A .
H34B H 0.8628 0.4139 0.7895 0.056 Uiso 1 1 calc R . .
C35 C 0.7555(3) 0.32537(16) 0.8686(2) 0.0623(11) Uani 1 1 d D A .
H35A H 0.7265 0.3083 0.9178 0.075 Uiso 1 1 calc R . .
H35B H 0.8146 0.2910 0.8623 0.075 Uiso 1 1 calc R . .
C36 C 0.6389(3) 0.32813(15) 0.8352(2) 0.0535(9) Uani 1 1 d D . .
H36A H 0.6683 0.3415 0.7866 0.064 Uiso 1 1 calc R A .
H36B H 0.5933 0.2802 0.8571 0.064 Uiso 1 1 calc R . .
C41 C 0.2247(2) 0.56118(12) 0.81889(12) 0.0241(5) Uani 1 1 d . A .
H41 H 0.2105 0.5781 0.8544 0.029 Uiso 1 1 calc R . .
C42 C 0.0975(2) 0.56315(14) 0.79406(13) 0.0336(6) Uani 1 1 d . . .
H42A H 0.1085 0.5431 0.7614 0.040 Uiso 1 1 calc R A .
H42B H 0.0309 0.5325 0.8331 0.040 Uiso 1 1 calc R . .
C43 C 0.0525(3) 0.63889(16) 0.76022(14) 0.0427(7) Uani 1 1 d . A .
H43A H -0.0267 0.6376 0.7431 0.051 Uiso 1 1 calc R . .
H43B H 0.0326 0.6572 0.7941 0.051 Uiso 1 1 calc R . .
C44 C 0.1546(3) 0.68924(15) 0.70154(14) 0.0417(7) Uani 1 1 d . . .
H44A H 0.1254 0.7385 0.6828 0.050 Uiso 1 1 calc R A .
H44B H 0.1669 0.6743 0.6651 0.050 Uiso 1 1 calc R . .
C45 C 0.2817(3) 0.68880(14) 0.72462(14) 0.0383(6) Uani 1 1 d . A .
H45A H 0.3474 0.7190 0.6849 0.046 Uiso 1 1 calc R . .
H45B H 0.2719 0.7097 0.7566 0.046 Uiso 1 1 calc R . .
C46 C 0.3264(2) 0.61312(13) 0.75915(13) 0.0304(6) Uani 1 1 d . . .
H46A H 0.4056 0.6149 0.7761 0.036 Uiso 1 1 calc R A .
H46B H 0.3469 0.5947 0.7254 0.036 Uiso 1 1 calc R . .
C51 C 0.2507(2) 0.43869(13) 0.93343(12) 0.0234(5) Uani 1 1 d . A .
H51 H 0.2746 0.3884 0.9462 0.028 Uiso 1 1 calc R . .
C52 C 0.3410(2) 0.47271(14) 0.95975(12) 0.0290(5) Uani 1 1 d . . .
H52A H 0.4306 0.4705 0.9400 0.035 Uiso 1 1 calc R A .
H52B H 0.3238 0.5238 0.9443 0.035 Uiso 1 1 calc R . .
C53 C 0.3246(2) 0.43528(16) 1.03701(13) 0.0348(6) Uani 1 1 d . A .
H53A H 0.3801 0.4611 1.0513 0.042 Uiso 1 1 calc R . .
H53B H 0.3524 0.3859 1.0522 0.042 Uiso 1 1 calc R . .
C54 C 0.1859(3) 0.43243(16) 1.07107(13) 0.0366(6) Uani 1 1 d . . .
H54A H 0.1609 0.4816 1.0603 0.044 Uiso 1 1 calc R A .
H54B H 0.1782 0.4050 1.1209 0.044 Uiso 1 1 calc R . .
C55 C 0.0961(3) 0.39696(15) 1.04672(13) 0.0346(6) Uani 1 1 d . A .
H55A H 0.1155 0.3463 1.0616 0.041 Uiso 1 1 calc R . .
H55B H 0.0065 0.3981 1.0673 0.041 Uiso 1 1 calc R . .
C56 C 0.1112(2) 0.43537(14) 0.96978(12) 0.0291(5) Uani 1 1 d . . .
H56A H 0.0839 0.4847 0.9555 0.035 Uiso 1 1 calc R A .
H56B H 0.0543 0.4103 0.9554 0.035 Uiso 1 1 calc R . .
P2 P 0.79032(6) 0.11473(4) 1.17865(3) 0.02639(15) Uani 1 1 d . . .
N2 N 0.7609(2) 0.08183(12) 1.13206(11) 0.0335(5) Uani 1 1 d . B .
B2 B 0.6882(3) 0.02929(17) 1.12917(15) 0.0300(6) Uani 1 1 d . . .
C61 C 0.9656(5) 0.1304(2) 1.1629(2) 0.0226(7) Uiso 0.608(5) 1 d PD B 1
H61 H 0.9888 0.1635 1.1133 0.027 Uiso 0.608(5) 1 calc PR B 1
C62 C 1.0345(4) 0.0624(2) 1.1720(2) 0.0270(5) Uiso 0.608(5) 1 d PD B 1
H62A H 1.0000 0.0408 1.1466 0.032 Uiso 0.608(5) 1 calc PR B 1
H62B H 1.0185 0.0271 1.2205 0.032 Uiso 0.608(5) 1 calc PR B 1
C63 C 1.1793(4) 0.0799(3) 1.1463(3) 0.0351(6) Uiso 0.608(5) 1 d PD B 1
H63A H 1.2222 0.0350 1.1554 0.042 Uiso 0.608(5) 1 calc PR B 1
H63B H 1.1955 0.1107 1.0966 0.042 Uiso 0.608(5) 1 calc PR B 1
C64 C 1.2361(5) 0.1181(3) 1.1804(3) 0.0385(9) Uiso 0.608(5) 1 d PD B 1
H64A H 1.2278 0.0857 1.2295 0.046 Uiso 0.608(5) 1 calc PR B 1
H64B H 1.3281 0.1309 1.1609 0.046 Uiso 0.608(5) 1 calc PR B 1
C65 C 1.1671(4) 0.1856(3) 1.1701(3) 0.0351(6) Uiso 0.608(5) 1 d PD B 1
H65A H 1.1816 0.2196 1.1212 0.042 Uiso 0.608(5) 1 calc PR B 1
H65B H 1.2031 0.2089 1.1937 0.042 Uiso 0.608(5) 1 calc PR B 1
C66 C 1.0233(4) 0.1690(2) 1.1971(2) 0.0270(5) Uiso 0.608(5) 1 d PD B 1
H66A H 0.9810 0.2141 1.1880 0.032 Uiso 0.608(5) 1 calc PR B 1
H66B H 1.0080 0.1384 1.2468 0.032 Uiso 0.608(5) 1 calc PR B 1
C61A C 0.9611(7) 0.1149(4) 1.1789(4) 0.0226(7) Uiso 0.392(5) 1 d PD B 2
H61A H 1.0005 0.1463 1.1305 0.027 Uiso 0.392(5) 1 calc PR B 2
C62A C 1.0265(6) 0.0445(4) 1.1963(4) 0.0270(5) Uiso 0.392(5) 1 d PD B 2
H62C H 0.9976 0.0208 1.1712 0.032 Uiso 0.392(5) 1 calc PR B 2
H62D H 1.0012 0.0121 1.2454 0.032 Uiso 0.392(5) 1 calc PR B 2
C63A C 1.1727(6) 0.0574(4) 1.1780(4) 0.0351(6) Uiso 0.392(5) 1 d PD B 2
H63C H 1.2125 0.0110 1.1922 0.042 Uiso 0.392(5) 1 calc PR B 2
H63D H 1.1991 0.0857 1.1283 0.042 Uiso 0.392(5) 1 calc PR B 2
C64A C 1.2186(7) 0.0976(4) 1.2131(5) 0.0385(9) Uiso 0.392(5) 1 d PD B 2
H64C H 1.3121 0.1088 1.1981 0.046 Uiso 0.392(5) 1 calc PR B 2
H64D H 1.2019 0.0665 1.2627 0.046 Uiso 0.392(5) 1 calc PR B 2
C65A C 1.1515(7) 0.1673(4) 1.1976(4) 0.0351(6) Uiso 0.392(5) 1 d PD B 2
H65C H 1.1748 0.2005 1.1486 0.042 Uiso 0.392(5) 1 calc PR B 2
H65D H 1.1805 0.1906 1.2230 0.042 Uiso 0.392(5) 1 calc PR B 2
C66A C 1.0050(7) 0.1523(4) 1.2174(4) 0.0270(5) Uiso 0.392(5) 1 d PD B 2
H66C H 0.9807 0.1214 1.2669 0.032 Uiso 0.392(5) 1 calc PR B 2
H66D H 0.9630 0.1978 1.2060 0.032 Uiso 0.392(5) 1 calc PR B 2
C71 C 0.7118(3) 0.06835(14) 1.26903(12) 0.0296(5) Uani 1 1 d . B .
H71 H 0.6224 0.0550 1.2685 0.036 Uiso 1 1 calc R . .
C72 C 0.6972(3) 0.11044(15) 1.31084(13) 0.0381(6) Uani 1 1 d . . .
H72A H 0.7825 0.1217 1.3169 0.046 Uiso 1 1 calc R B .
H72B H 0.6586 0.1562 1.2860 0.046 Uiso 1 1 calc R . .
C73 C 0.6127(3) 0.06697(16) 1.38026(14) 0.0471(8) Uani 1 1 d . B .
H73A H 0.6081 0.0940 1.4069 0.056 Uiso 1 1 calc R . .
H73B H 0.5250 0.0598 1.3742 0.056 Uiso 1 1 calc R . .
C74 C 0.6647(4) -0.00570(17) 1.41921(15) 0.0542(9) Uani 1 1 d . . .
H74A H 0.6044 -0.0338 1.4622 0.065 Uiso 1 1 calc R B .
H74B H 0.7474 0.0014 1.4306 0.065 Uiso 1 1 calc R . .
C75 C 0.6841(3) -0.04783(16) 1.37798(15) 0.0494(8) Uani 1 1 d . B .
H75A H 0.7243 -0.0928 1.4032 0.059 Uiso 1 1 calc R . .
H75B H 0.6001 -0.0604 1.3714 0.059 Uiso 1 1 calc R . .
C76 C 0.7694(3) -0.00319(14) 1.30877(14) 0.0366(6) Uani 1 1 d . . .
H76A H 0.7789 -0.0305 1.2823 0.044 Uiso 1 1 calc R B .
H76B H 0.8554 0.0062 1.3154 0.044 Uiso 1 1 calc R . .
C81 C 0.7357(2) 0.20564(13) 1.14713(12) 0.0271(5) Uani 1 1 d . B .
H81 H 0.7539 0.2257 1.1778 0.032 Uiso 1 1 calc R . .
C82 C 0.5900(2) 0.20315(15) 1.14981(13) 0.0354(6) Uani 1 1 d . . .
H82A H 0.5695 0.1804 1.1222 0.043 Uiso 1 1 calc R B .
H82B H 0.5463 0.1735 1.1972 0.043 Uiso 1 1 calc R . .
C83 C 0.5400(3) 0.27828(16) 1.12316(15) 0.0464(8) Uani 1 1 d . B .
H83A H 0.4469 0.2750 1.1239 0.056 Uiso 1 1 calc R . .
H83B H 0.5537 0.2997 1.1529 0.056 Uiso 1 1 calc R . .
C84 C 0.6090(3) 0.32618(17) 1.05068(15) 0.0502(8) Uani 1 1 d . . .
H84A H 0.5783 0.3750 1.0349 0.060 Uiso 1 1 calc R B .
H84B H 0.5892 0.3070 1.0202 0.060 Uiso 1 1 calc R . .
C85 C 0.7541(3) 0.32973(15) 1.04743(14) 0.0415(7) Uani 1 1 d . B .
H85A H 0.7969 0.3591 0.9998 0.050 Uiso 1 1 calc R . .
H85B H 0.7742 0.3534 1.0744 0.050 Uiso 1 1 calc R . .
C86 C 0.8058(2) 0.25563(15) 1.07444(13) 0.0331(6) Uani 1 1 d . . .
H86A H 0.8983 0.2600 1.0745 0.040 Uiso 1 1 calc R B .
H86B H 0.7955 0.2344 1.0441 0.040 Uiso 1 1 calc R . .
C91 C 0.6864(2) 0.03465(13) 1.05606(12) 0.0266(5) Uani 1 1 d . B .
H91 H 0.6346 -0.0081 1.0629 0.032 Uiso 1 1 calc R . .
C92 C 0.8207(3) 0.03392(18) 1.01836(14) 0.0449(7) Uani 1 1 d . . .
H92A H 0.8755 0.0739 1.0141 0.054 Uiso 1 1 calc R B .
H92B H 0.8584 -0.0113 1.0455 0.054 Uiso 1 1 calc R . .
C93 C 0.8209(3) 0.04072(19) 0.94781(15) 0.0516(8) Uani 1 1 d . B .
H93A H 0.9102 0.0440 0.9245 0.062 Uiso 1 1 calc R . .
H93B H 0.7766 -0.0026 0.9521 0.062 Uiso 1 1 calc R . .
C94 C 0.7550(3) 0.10628(15) 0.90576(13) 0.0434(7) Uani 1 1 d . . .
H94A H 0.8063 0.1499 0.8959 0.052 Uiso 1 1 calc R B .
H94B H 0.7495 0.1068 0.8620 0.052 Uiso 1 1 calc R . .
C95 C 0.6222(3) 0.10684(17) 0.94234(15) 0.0463(8) Uani 1 1 d . B .
H95A H 0.5682 0.0663 0.9472 0.056 Uiso 1 1 calc R . .
H95B H 0.5839 0.1517 0.9149 0.056 Uiso 1 1 calc R . .
C96 C 0.6232(3) 0.10105(16) 1.01238(14) 0.0429(7) Uani 1 1 d . . .
H96A H 0.6697 0.1441 1.0073 0.051 Uiso 1 1 calc R B .
H96B H 0.5342 0.0994 1.0353 0.051 Uiso 1 1 calc R . .
C101 C 0.6020(4) -0.0309(2) 1.1947(2) 0.0229(7) Uiso 0.602(6) 1 d PD B 1
H101 H 0.6059 -0.0218 1.2343 0.027 Uiso 0.602(6) 1 calc PR B 1
C102 C 0.6634(4) -0.1012(3) 1.2058(2) 0.0338(6) Uiso 0.602(6) 1 d PD B 1
H10A H 0.6670 -0.1078 1.1647 0.041 Uiso 0.602(6) 1 calc PR B 1
H10B H 0.7523 -0.0981 1.2124 0.041 Uiso 0.602(6) 1 calc PR B 1
C103 C 0.5902(5) -0.1663(3) 1.2671(3) 0.0429(7) Uiso 0.602(6) 1 d PD B 1
H10C H 0.6362 -0.2097 1.2730 0.051 Uiso 0.602(6) 1 calc PR B 1
H10D H 0.5879 -0.1602 1.3084 0.051 Uiso 0.602(6) 1 calc PR B 1
C104 C 0.4545(5) -0.1769(3) 1.2593(3) 0.0362(9) Uiso 0.602(6) 1 d PD B 1
H10E H 0.4095 -0.2198 1.2990 0.043 Uiso 0.602(6) 1 calc PR B 1
H10F H 0.4538 -0.1823 1.2179 0.043 Uiso 0.602(6) 1 calc PR B 1
C105 C 0.3926(6) -0.1092(3) 1.2543(3) 0.0429(7) Uiso 0.602(6) 1 d PD B 1
H10G H 0.3958 -0.1047 1.2960 0.051 Uiso 0.602(6) 1 calc PR B 1
H10H H 0.3016 -0.1127 1.2510 0.051 Uiso 0.602(6) 1 calc PR B 1
C106 C 0.4615(5) -0.0411(3) 1.1912(3) 0.0338(6) Uiso 0.602(6) 1 d PD B 1
H10I H 0.4572 -0.0454 1.1496 0.041 Uiso 0.602(6) 1 calc PR B 1
H10J H 0.4164 0.0015 1.1885 0.041 Uiso 0.602(6) 1 calc PR B 1
C201 C 0.6193(6) -0.0479(4) 1.1938(4) 0.0229(7) Uiso 0.398(6) 1 d PD B 2
H201 H 0.6466 -0.0514 1.2354 0.027 Uiso 0.398(6) 1 calc PR B 2
C202 C 0.6491(7) -0.1175(4) 1.1914(4) 0.0338(6) Uiso 0.398(6) 1 d PD B 2
H20A H 0.7419 -0.1238 1.1896 0.041 Uiso 0.398(6) 1 calc PR B 2
H20B H 0.6264 -0.1159 1.1500 0.041 Uiso 0.398(6) 1 calc PR B 2
C203 C 0.5737(7) -0.1811(4) 1.2544(4) 0.0429(7) Uiso 0.398(6) 1 d PD B 2
H20C H 0.6099 -0.1895 1.2948 0.051 Uiso 0.398(6) 1 calc PR B 2
H20D H 0.5815 -0.2249 1.2482 0.051 Uiso 0.398(6) 1 calc PR B 2
C204 C 0.4263(7) -0.1651(4) 1.2658(4) 0.0362(9) Uiso 0.398(6) 1 d PD B 2
H20E H 0.3866 -0.1728 1.2327 0.043 Uiso 0.398(6) 1 calc PR B 2
H20F H 0.3859 -0.2019 1.3114 0.043 Uiso 0.398(6) 1 calc PR B 2
C205 C 0.3898(9) -0.0950(4) 1.2607(5) 0.0429(7) Uiso 0.398(6) 1 d PD B 2
H20G H 0.3988 -0.0929 1.3029 0.051 Uiso 0.398(6) 1 calc PR B 2
H20H H 0.2990 -0.0891 1.2558 0.051 Uiso 0.398(6) 1 calc PR B 2
C206 C 0.4721(7) -0.0348(4) 1.2011(4) 0.0338(6) Uiso 0.398(6) 1 d PD B 2
H20I H 0.4596 0.0098 1.2055 0.041 Uiso 0.398(6) 1 calc PR B 2
H20J H 0.4430 -0.0277 1.1591 0.041 Uiso 0.398(6) 1 calc PR B 2
N3 N -0.1215(2) -0.25595(11) 1.47454(11) 0.0317(5) Uani 1 1 d . C .
P3 P -0.21378(6) -0.29910(3) 1.54308(3) 0.02389(14) Uani 1 1 d . . .
B3 B -0.0149(3) -0.21088(16) 1.43199(18) 0.0353(7) Uani 1 1 d . . .
C111 C -0.1616(2) -0.39011(12) 1.58676(13) 0.0252(5) Uani 1 1 d . C .
H111 H -0.2235 -0.4169 1.6301 0.030 Uiso 1 1 calc R . .
C112 C -0.1564(3) -0.43166(14) 1.54496(14) 0.0321(6) Uani 1 1 d . . .
H11C H -0.2423 -0.4353 1.5350 0.038 Uiso 1 1 calc R C .
H11D H -0.0969 -0.4054 1.5013 0.038 Uiso 1 1 calc R . .
C113 C -0.1119(3) -0.50673(14) 1.58347(16) 0.0410(7) Uani 1 1 d . C .
H11E H -0.1750 -0.5341 1.6255 0.049 Uiso 1 1 calc R . .
H11F H -0.1073 -0.5319 1.5552 0.049 Uiso 1 1 calc R . .
C114 C 0.0191(3) -0.50405(15) 1.60167(16) 0.0435(7) Uani 1 1 d . . .
H11G H 0.0426 -0.5534 1.6291 0.052 Uiso 1 1 calc R C .
H11H H 0.0842 -0.4815 1.5596 0.052 Uiso 1 1 calc R . .
C115 C 0.0185(3) -0.46166(15) 1.64149(15) 0.0395(7) Uani 1 1 d . C .
H11I H 0.1061 -0.4573 1.6492 0.047 Uiso 1 1 calc R . .
H11J H -0.0378 -0.4878 1.6863 0.047 Uiso 1 1 calc R . .
C116 C -0.0284(3) -0.38681(14) 1.60411(15) 0.0353(6) Uani 1 1 d . . .
H11K H 0.0334 -0.3586 1.5618 0.042 Uiso 1 1 calc R C .
H11L H -0.0326 -0.3621 1.6328 0.042 Uiso 1 1 calc R . .
C121 C -0.2263(2) -0.26338(12) 1.60534(12) 0.0258(5) Uani 1 1 d . C .
H121 H -0.1363 -0.2557 1.6094 0.031 Uiso 1 1 calc R . .
C122 C -0.2963(3) -0.31199(14) 1.67795(13) 0.0357(6) Uani 1 1 d . . .
H12E H -0.3868 -0.3213 1.6773 0.043 Uiso 1 1 calc R C .
H12F H -0.2565 -0.3585 1.6960 0.043 Uiso 1 1 calc R . .
C123 C -0.2902(3) -0.27679(17) 1.72439(15) 0.0495(8) Uani 1 1 d . C .
H12G H -0.3393 -0.3079 1.7702 0.059 Uiso 1 1 calc R . .
H12H H -0.2002 -0.2719 1.7286 0.059 Uiso 1 1 calc R . .
C124 C -0.3445(3) -0.20333(17) 1.69666(15) 0.0452(7) Uani 1 1 d . . .
H12I H -0.4363 -0.2084 1.6956 0.054 Uiso 1 1 calc R C .
H12J H -0.3370 -0.1814 1.7268 0.054 Uiso 1 1 calc R . .
C125 C -0.2726(3) -0.15515(15) 1.62546(16) 0.0432(7) Uani 1 1 d . C .
H12K H -0.1819 -0.1475 1.6270 0.052 Uiso 1 1 calc R . .
H12L H -0.3100 -0.1080 1.6075 0.052 Uiso 1 1 calc R . .
C126 C -0.2801(3) -0.18915(14) 1.57838(14) 0.0368(6) Uani 1 1 d . . .
H12M H -0.2312 -0.1577 1.5327 0.044 Uiso 1 1 calc R C .
H12N H -0.3704 -0.1935 1.5743 0.044 Uiso 1 1 calc R . .
C131 C -0.3693(5) -0.3102(3) 1.5219(2) 0.0250(8) Uiso 0.531(3) 1 d PD C 1
H131 H -0.3551 -0.3421 1.4995 0.030 Uiso 0.531(3) 1 calc PR C 1
C132 C -0.4158(4) -0.2407(2) 1.4697(2) 0.0280(5) Uiso 0.531(3) 1 d PD C 1
H13E H -0.4321 -0.2067 1.4892 0.034 Uiso 0.531(3) 1 calc PR C 1
H13F H -0.3483 -0.2181 1.4288 0.034 Uiso 0.531(3) 1 calc PR C 1
C133 C -0.5385(5) -0.2557(3) 1.4498(3) 0.0351(6) Uiso 0.531(3) 1 d PD C 1
H13G H -0.5701 -0.2097 1.4195 0.042 Uiso 0.531(3) 1 calc PR C 1
H13H H -0.5189 -0.2839 1.4244 0.042 Uiso 0.531(3) 1 calc PR C 1
C134 C -0.6434(5) -0.2967(3) 1.5116(3) 0.0385(9) Uiso 0.531(3) 1 d PD C 1
H13I H -0.6717 -0.2657 1.5332 0.046 Uiso 0.531(3) 1 calc PR C 1
H13J H -0.7178 -0.3086 1.4965 0.046 Uiso 0.531(3) 1 calc PR C 1
C135 C -0.5984(6) -0.3652(4) 1.5633(3) 0.0351(6) Uiso 0.531(3) 1 d PD C 1
H13K H -0.5804 -0.3990 1.5438 0.042 Uiso 0.531(3) 1 calc PR C 1
H13L H -0.6666 -0.3880 1.6039 0.042 Uiso 0.531(3) 1 calc PR C 1
C136 C -0.4774(5) -0.3490(3) 1.5837(3) 0.0280(5) Uiso 0.531(3) 1 d PD C 1
H13M H -0.4474 -0.3944 1.6160 0.034 Uiso 0.531(3) 1 calc PR C 1
H13N H -0.4980 -0.3188 1.6070 0.034 Uiso 0.531(3) 1 calc PR C 1
C231 C -0.3843(6) -0.3034(3) 1.5354(3) 0.0250(8) Uiso 0.469(3) 1 d PD C 2
H231 H -0.4239 -0.2624 1.5409 0.030 Uiso 0.469(3) 1 calc PR C 2
C232 C -0.3887(5) -0.2897(3) 1.4630(3) 0.0280(5) Uiso 0.469(3) 1 d PD C 2
H23E H -0.3491 -0.3288 1.4548 0.034 Uiso 0.469(3) 1 calc PR C 2
H23F H -0.3394 -0.2442 1.4303 0.034 Uiso 0.469(3) 1 calc PR C 2
C233 C -0.5283(5) -0.2855(3) 1.4518(3) 0.0351(6) Uiso 0.469(3) 1 d PD C 2
H23G H -0.5629 -0.2420 1.4532 0.042 Uiso 0.469(3) 1 calc PR C 2
H23H H -0.5296 -0.2810 1.4062 0.042 Uiso 0.469(3) 1 calc PR C 2
C234 C -0.6139(6) -0.3502(3) 1.5041(3) 0.0385(9) Uiso 0.469(3) 1 d PD C 2
H23I H -0.5882 -0.3927 1.4980 0.046 Uiso 0.469(3) 1 calc PR C 2
H23J H -0.7034 -0.3423 1.4972 0.046 Uiso 0.469(3) 1 calc PR C 2
C235 C -0.6062(7) -0.3643(5) 1.5758(3) 0.0351(6) Uiso 0.469(3) 1 d PD C 2
H23K H -0.6571 -0.4092 1.6086 0.042 Uiso 0.469(3) 1 calc PR C 2
H23L H -0.6430 -0.3247 1.5841 0.042 Uiso 0.469(3) 1 calc PR C 2
C236 C -0.4664(5) -0.3706(3) 1.5868(3) 0.0280(5) Uiso 0.469(3) 1 d PD C 2
H23M H -0.4634 -0.3780 1.6332 0.034 Uiso 0.469(3) 1 calc PR C 2
H23N H -0.4318 -0.4127 1.5822 0.034 Uiso 0.469(3) 1 calc PR C 2
C141 C 0.0275(4) -0.2083(2) 1.3538(2) 0.0232(7) Uiso 0.611(3) 1 d PD C 1
H141 H 0.0863 -0.1649 1.3235 0.028 Uiso 0.611(3) 1 calc PR C 1
C142 C -0.0874(4) -0.2067(2) 1.3201(2) 0.0369(6) Uiso 0.611(3) 1 d PD C 1
H14E H -0.1317 -0.1623 1.3119 0.044 Uiso 0.611(3) 1 calc PR C 1
H14F H -0.1485 -0.2479 1.3512 0.044 Uiso 0.611(3) 1 calc PR C 1
C143 C -0.0460(5) -0.2097(3) 1.2521(2) 0.0397(7) Uiso 0.611(3) 1 d PD C 1
H14G H -0.1229 -0.2115 1.2334 0.048 Uiso 0.611(3) 1 calc PR C 1
H14H H 0.0072 -0.1657 1.2191 0.048 Uiso 0.611(3) 1 calc PR C 1
C144 C 0.0287(5) -0.2741(3) 1.2609(3) 0.0422(10) Uiso 0.611(3) 1 d PD C 1
H14I H 0.0599 -0.2719 1.2159 0.051 Uiso 0.611(3) 1 calc PR C 1
H14J H -0.0286 -0.3180 1.2884 0.051 Uiso 0.611(3) 1 calc PR C 1
C145 C 0.1415(5) -0.2786(3) 1.2951(2) 0.0397(7) Uiso 0.611(3) 1 d PD C 1
H14K H 0.2051 -0.2383 1.2648 0.048 Uiso 0.611(3) 1 calc PR C 1
H14L H 0.1829 -0.3238 1.3035 0.048 Uiso 0.611(3) 1 calc PR C 1
C146 C 0.0991(5) -0.2758(2) 1.3622(2) 0.0369(6) Uiso 0.611(3) 1 d PD C 1
H14M H 0.1752 -0.2767 1.3824 0.044 Uiso 0.611(3) 1 calc PR C 1
H14N H 0.0425 -0.3188 1.3940 0.044 Uiso 0.611(3) 1 calc PR C 1
C241 C 0.0392(7) -0.2093(3) 1.3704(3) 0.0232(7) Uiso 0.389(3) 1 d PD C 2
H241 H 0.1274 -0.1856 1.3556 0.028 Uiso 0.389(3) 1 calc PR C 2
C242 C 0.0454(8) -0.2818(4) 1.3677(4) 0.0369(6) Uiso 0.389(3) 1 d PD C 2
H24E H -0.0397 -0.3080 1.3879 0.044 Uiso 0.389(3) 1 calc PR C 2
H24F H 0.1070 -0.3109 1.3959 0.044 Uiso 0.389(3) 1 calc PR C 2
C243 C 0.0857(8) -0.2748(4) 1.2949(4) 0.0397(7) Uiso 0.389(3) 1 d PD C 2
H24G H 0.1748 -0.2539 1.2762 0.048 Uiso 0.389(3) 1 calc PR C 2
H24H H 0.0825 -0.3228 1.2969 0.048 Uiso 0.389(3) 1 calc PR C 2
C244 C -0.0001(8) -0.2287(4) 1.2495(4) 0.0422(10) Uiso 0.389(3) 1 d PD C 2
H24I H -0.0873 -0.2524 1.2653 0.051 Uiso 0.389(3) 1 calc PR C 2
H24J H 0.0307 -0.2225 1.2030 0.051 Uiso 0.389(3) 1 calc PR C 2
C245 C -0.0047(7) -0.1549(4) 1.2484(3) 0.0397(7) Uiso 0.389(3) 1 d PD C 2
H24K H 0.0810 -0.1293 1.2286 0.048 Uiso 0.389(3) 1 calc PR C 2
H24L H -0.0653 -0.1261 1.2194 0.048 Uiso 0.389(3) 1 calc PR C 2
C246 C -0.0459(7) -0.1618(4) 1.3190(3) 0.0369(6) Uiso 0.389(3) 1 d PD C 2
H24M H -0.1353 -0.1825 1.3364 0.044 Uiso 0.389(3) 1 calc PR C 2
H24N H -0.0444 -0.1134 1.3163 0.044 Uiso 0.389(3) 1 calc PR C 2
C151 C 0.0480(6) -0.1647(3) 1.4655(3) 0.0404(10) Uiso 0.506(3) 1 d PD C 1
H151 H -0.0067 -0.1746 1.5100 0.049 Uiso 0.506(3) 1 calc PR C 1
C152 C 0.1848(5) -0.1878(3) 1.4765(3) 0.0437(7) Uiso 0.506(3) 1 d PD C 1
H15E H 0.2349 -0.1845 1.4337 0.052 Uiso 0.506(3) 1 calc PR C 1
H15F H 0.1795 -0.2384 1.5113 0.052 Uiso 0.506(3) 1 calc PR C 1
C153 C 0.2556(7) -0.1410(3) 1.4995(4) 0.0566(9) Uiso 0.506(3) 1 d PD C 1
H15G H 0.2117 -0.1487 1.5449 0.068 Uiso 0.506(3) 1 calc PR C 1
H15H H 0.3442 -0.1557 1.5028 0.068 Uiso 0.506(3) 1 calc PR C 1
C154 C 0.2587(6) -0.0629(3) 1.4500(3) 0.0512(11) Uiso 0.506(3) 1 d PD C 1
H15I H 0.3099 -0.0545 1.4057 0.061 Uiso 0.506(3) 1 calc PR C 1
H15J H 0.3004 -0.0340 1.4667 0.061 Uiso 0.506(3) 1 calc PR C 1
C155 C 0.1209(6) -0.0385(4) 1.4406(4) 0.0566(9) Uiso 0.506(3) 1 d PD C 1
H15K H 0.0717 -0.0426 1.4839 0.068 Uiso 0.506(3) 1 calc PR C 1
H15L H 0.1254 0.0123 1.4062 0.068 Uiso 0.506(3) 1 calc PR C 1
C156 C 0.0526(6) -0.0856(3) 1.4178(3) 0.0437(7) Uiso 0.506(3) 1 d PD C 1
H15M H -0.0358 -0.0709 1.4141 0.052 Uiso 0.506(3) 1 calc PR C 1
H15N H 0.0974 -0.0770 1.3722 0.052 Uiso 0.506(3) 1 calc PR C 1
C251 C 0.0863(6) -0.1582(3) 1.4360(3) 0.0404(10) Uiso 0.494(3) 1 d PD C 2
H251 H 0.1717 -0.1712 1.4199 0.049 Uiso 0.494(3) 1 calc PR C 2
C252 C 0.0891(6) -0.1715(3) 1.5068(3) 0.0437(7) Uiso 0.494(3) 1 d PD C 2
H25E H 0.1081 -0.2219 1.5333 0.052 Uiso 0.494(3) 1 calc PR C 2
H25F H 0.0028 -0.1651 1.5275 0.052 Uiso 0.494(3) 1 calc PR C 2
C253 C 0.1852(7) -0.1237(3) 1.5132(4) 0.0566(9) Uiso 0.494(3) 1 d PD C 2
H25G H 0.1691 -0.1301 1.5603 0.068 Uiso 0.494(3) 1 calc PR C 2
H25H H 0.2723 -0.1385 1.5039 0.068 Uiso 0.494(3) 1 calc PR C 2
C254 C 0.1788(7) -0.0460(3) 1.4653(3) 0.0512(11) Uiso 0.494(3) 1 d PD C 2
H25I H 0.1023 -0.0281 1.4832 0.061 Uiso 0.494(3) 1 calc PR C 2
H25J H 0.2547 -0.0192 1.4649 0.061 Uiso 0.494(3) 1 calc PR C 2
C255 C 0.1736(7) -0.0298(4) 1.3954(3) 0.0566(9) Uiso 0.494(3) 1 d PD C 2
H25K H 0.2602 -0.0329 1.3727 0.068 Uiso 0.494(3) 1 calc PR C 2
H25L H 0.1501 0.0203 1.3715 0.068 Uiso 0.494(3) 1 calc PR C 2
C256 C 0.0803(6) -0.0781(3) 1.3873(3) 0.0437(7) Uiso 0.494(3) 1 d PD C 2
H25M H 0.0993 -0.0711 1.3400 0.052 Uiso 0.494(3) 1 calc PR C 2
H25N H -0.0077 -0.0638 1.3956 0.052 Uiso 0.494(3) 1 calc PR C 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0203(3) 0.0189(3) 0.0175(3) -0.0074(2) -0.0018(2) 0.0007(2)
B1 0.0149(12) 0.0271(13) 0.0275(14) -0.0150(12) -0.0022(11) -0.0015(10)
N1 0.0267(11) 0.0261(10) 0.0266(11) -0.0150(9) -0.0037(9) 0.0043(8)
C31 0.0247(13) 0.0245(12) 0.0259(13) -0.0067(10) -0.0056(10) -0.0040(10)
C32 0.0320(14) 0.0236(12) 0.0381(15) -0.0136(11) -0.0113(12) -0.0013(10)
C33 0.0362(16) 0.0462(17) 0.0476(18) -0.0206(15) -0.0118(14) -0.0097(13)
C34 0.0289(15) 0.0474(18) 0.0544(19) -0.0126(15) -0.0152(14) -0.0050(13)
C35 0.0312(17) 0.0394(17) 0.092(3) -0.0034(18) -0.0282(18) 0.0042(14)
C36 0.0308(16) 0.0241(14) 0.101(3) -0.0200(16) -0.0244(17) 0.0052(12)
C41 0.0264(13) 0.0262(12) 0.0232(12) -0.0145(10) -0.0045(10) 0.0041(10)
C42 0.0259(14) 0.0412(15) 0.0295(14) -0.0125(12) -0.0056(11) 0.0029(11)
C43 0.0350(16) 0.0516(18) 0.0329(15) -0.0107(14) -0.0115(13) 0.0163(14)
C44 0.0526(19) 0.0392(16) 0.0261(14) -0.0081(12) -0.0100(13) 0.0144(14)
C45 0.0484(18) 0.0293(14) 0.0343(15) -0.0134(12) -0.0025(13) -0.0016(12)
C46 0.0283(14) 0.0288(13) 0.0347(14) -0.0155(11) -0.0038(11) -0.0004(11)
C51 0.0208(12) 0.0260(12) 0.0267(12) -0.0150(10) -0.0037(10) 0.0022(9)
C52 0.0198(12) 0.0405(14) 0.0291(13) -0.0181(12) -0.0038(10) 0.0011(11)
C53 0.0250(13) 0.0524(17) 0.0300(14) -0.0201(13) -0.0088(11) 0.0019(12)
C54 0.0334(15) 0.0557(18) 0.0270(14) -0.0243(13) -0.0058(12) 0.0011(13)
C55 0.0261(14) 0.0485(16) 0.0274(14) -0.0179(13) 0.0022(11) -0.0054(12)
C56 0.0229(13) 0.0433(15) 0.0267(13) -0.0210(12) -0.0032(10) -0.0025(11)
P2 0.0210(3) 0.0386(4) 0.0260(3) -0.0196(3) -0.0060(3) 0.0017(3)
N2 0.0300(12) 0.0470(13) 0.0291(12) -0.0225(11) -0.0036(9) -0.0073(10)
B2 0.0238(15) 0.0400(16) 0.0247(15) -0.0124(13) -0.0067(12) -0.0042(12)
C71 0.0321(14) 0.0350(14) 0.0243(13) -0.0146(11) -0.0095(11) 0.0072(11)
C72 0.0516(18) 0.0376(15) 0.0274(14) -0.0170(12) -0.0079(13) 0.0143(13)
C73 0.067(2) 0.0451(17) 0.0251(14) -0.0142(13) -0.0054(14) 0.0168(15)
C74 0.086(3) 0.0473(18) 0.0242(15) -0.0108(14) -0.0144(16) 0.0151(17)
C75 0.077(2) 0.0357(16) 0.0331(16) -0.0098(13) -0.0237(16) 0.0148(15)
C76 0.0484(17) 0.0364(14) 0.0365(15) -0.0219(13) -0.0224(13) 0.0165(13)
C81 0.0212(12) 0.0382(14) 0.0224(12) -0.0137(11) -0.0057(10) 0.0019(10)
C82 0.0208(13) 0.0422(15) 0.0266(14) -0.0022(12) -0.0011(11) -0.0004(11)
C83 0.0269(15) 0.0494(18) 0.0369(16) 0.0027(14) -0.0062(12) 0.0079(13)
C84 0.0322(16) 0.0514(19) 0.0358(16) 0.0084(14) -0.0103(13) -0.0008(14)
C85 0.0316(15) 0.0448(17) 0.0286(15) 0.0009(13) -0.0068(12) -0.0079(13)
C86 0.0226(13) 0.0449(16) 0.0261(13) -0.0120(12) -0.0013(11) -0.0069(11)
C91 0.0301(13) 0.0246(12) 0.0231(12) -0.0086(10) -0.0057(10) -0.0085(10)
C92 0.0359(16) 0.067(2) 0.0300(15) -0.0196(15) -0.0099(13) 0.0124(15)
C93 0.0485(19) 0.076(2) 0.0301(16) -0.0253(16) -0.0052(14) 0.0176(17)
C94 0.060(2) 0.0400(16) 0.0205(13) -0.0045(12) -0.0066(13) -0.0149(14)
C95 0.061(2) 0.0453(17) 0.0365(16) -0.0167(14) -0.0263(15) 0.0184(15)
C96 0.0526(19) 0.0484(17) 0.0382(16) -0.0251(14) -0.0210(14) 0.0189(14)
N3 0.0301(12) 0.0344(12) 0.0291(12) -0.0142(10) -0.0024(9) 0.0021(9)
P3 0.0224(3) 0.0212(3) 0.0286(3) -0.0120(3) -0.0042(3) 0.0000(2)
B3 0.0270(16) 0.0246(14) 0.057(2) -0.0206(15) -0.0077(14) 0.0019(12)
C111 0.0240(12) 0.0224(11) 0.0301(13) -0.0131(10) -0.0036(10) 0.0008(10)
C112 0.0310(14) 0.0331(14) 0.0400(15) -0.0236(12) -0.0064(12) 0.0029(11)
C113 0.0444(17) 0.0279(14) 0.0579(19) -0.0264(14) -0.0081(14) 0.0071(12)
C114 0.0386(17) 0.0345(15) 0.058(2) -0.0214(14) -0.0101(14) 0.0140(13)
C115 0.0328(15) 0.0388(15) 0.0464(17) -0.0171(14) -0.0137(13) 0.0102(12)
C116 0.0311(15) 0.0313(14) 0.0490(17) -0.0201(13) -0.0163(13) 0.0053(11)
C121 0.0236(12) 0.0241(12) 0.0309(13) -0.0142(11) -0.0035(10) 0.0015(10)
C122 0.0502(17) 0.0334(14) 0.0248(13) -0.0134(11) -0.0089(12) -0.0006(12)
C123 0.072(2) 0.0566(19) 0.0332(16) -0.0286(15) -0.0212(16) 0.0127(17)
C124 0.0458(18) 0.063(2) 0.0503(19) -0.0432(17) -0.0179(15) 0.0173(15)
C125 0.0419(17) 0.0366(15) 0.065(2) -0.0339(15) -0.0129(15) 0.0127(13)
C126 0.0441(17) 0.0284(13) 0.0357(15) -0.0145(12) -0.0027(13) 0.0093(12)
_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 1.581(2) . ?
P1 C11A 1.805(11) . ?
P1 C21 1.845(5) . ?
P1 C31 1.851(2) . ?
P1 C11 1.864(10) . ?
P1 C21A 1.895(7) . ?
B1 N1 1.406(3) . ?
B1 C51 1.605(4) . ?
B1 C41 1.607(4) . ?
C11 C16 1.529(8) . ?
C11 C12 1.535(8) . ?
C11 H11 1.0000 . ?
C12 C13 1.519(8) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.511(8) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.534(6) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.534(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C11A C16A 1.528(9) . ?
C11A C12A 1.559(9) . ?
C11A H11A 1.0000 . ?
C12A C13A 1.554(9) . ?
C12A H12C 0.9900 . ?
C12A H12D 0.9900 . ?
C13A C14A 1.510(9) . ?
C13A H13C 0.9900 . ?
C13A H13D 0.9900 . ?
C14A C15A 1.529(7) . ?
C14A H14C 0.9900 . ?
C14A H14D 0.9900 . ?
C15A C16A 1.528(7) . ?
C15A H15C 0.9900 . ?
C15A H15D 0.9900 . ?
C16A H16C 0.9900 . ?
C16A H16D 0.9900 . ?
C21 C26 1.544(5) . ?
C21 C22 1.546(6) . ?
C21 H21 1.0000 . ?
C22 C23 1.525(6) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.531(6) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.519(6) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.533(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C21A C26A 1.536(8) . ?
C21A C22A 1.546(8) . ?
C21A H21A 1.0000 . ?
C22A C23A 1.545(8) . ?
C22A H22C 0.9900 . ?
C22A H22D 0.9900 . ?
C23A C24A 1.513(8) . ?
C23A H23C 0.9900 . ?
C23A H23D 0.9900 . ?
C24A C25A 1.526(8) . ?
C24A H24C 0.9900 . ?
C24A H24D 0.9900 . ?
C25A C26A 1.537(7) . ?
C25A H25C 0.9900 . ?
C25A H25D 0.9900 . ?
C26A H26C 0.9900 . ?
C26A H26D 0.9900 . ?
C31 C36 1.525(4) . ?
C31 C32 1.538(3) . ?
C31 H31 1.0000 . ?
C32 C33 1.533(3) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.511(4) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.525(4) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.545(4) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C41 C42 1.543(3) . ?
C41 C46 1.545(3) . ?
C41 H41 1.0000 . ?
C42 C43 1.529(4) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.526(4) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.528(4) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C46 1.528(4) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C51 C52 1.545(3) . ?
C51 C56 1.553(3) . ?
C51 H51 1.0000 . ?
C52 C53 1.528(4) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C54 1.530(4) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.531(4) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 C56 1.523(3) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
P2 N2 1.565(2) . ?
P2 C61A 1.818(7) . ?
P2 C81 1.832(3) . ?
P2 C61 1.844(5) . ?
P2 C71 1.854(3) . ?
N2 B2 1.391(3) . ?
B2 C101 1.583(5) . ?
B2 C91 1.601(4) . ?
B2 C201 1.681(7) . ?
C61 C62 1.537(6) . ?
C61 C66 1.540(6) . ?
C61 H61 1.0000 . ?
C62 C63 1.538(6) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 C64 1.528(6) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C64 C65 1.523(6) . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C65 C66 1.530(6) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C61A C62A 1.533(8) . ?
C61A C66A 1.535(8) . ?
C61A H61A 1.0000 . ?
C62A C63A 1.536(8) . ?
C62A H62C 0.9900 . ?
C62A H62D 0.9900 . ?
C63A C64A 1.526(8) . ?
C63A H63C 0.9900 . ?
C63A H63D 0.9900 . ?
C64A C65A 1.534(8) . ?
C64A H64C 0.9900 . ?
C64A H64D 0.9900 . ?
C65A C66A 1.542(8) . ?
C65A H65C 0.9900 . ?
C65A H65D 0.9900 . ?
C66A H66C 0.9900 . ?
C66A H66D 0.9900 . ?
C71 C76 1.539(3) . ?
C71 C72 1.545(3) . ?
C71 H71 1.0000 . ?
C72 C73 1.529(4) . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
C73 C74 1.525(4) . ?
C73 H73A 0.9900 . ?
C73 H73B 0.9900 . ?
C74 C75 1.534(4) . ?
C74 H74A 0.9900 . ?
C74 H74B 0.9900 . ?
C75 C76 1.534(4) . ?
C75 H75A 0.9900 . ?
C75 H75B 0.9900 . ?
C76 H76A 0.9900 . ?
C76 H76B 0.9900 . ?
C81 C82 1.543(3) . ?
C81 C86 1.546(3) . ?
C81 H81 1.0000 . ?
C82 C83 1.533(4) . ?
C82 H82A 0.9900 . ?
C82 H82B 0.9900 . ?
C83 C84 1.531(4) . ?
C83 H83A 0.9900 . ?
C83 H83B 0.9900 . ?
C84 C85 1.534(4) . ?
C84 H84A 0.9900 . ?
C84 H84B 0.9900 . ?
C85 C86 1.523(4) . ?
C85 H85A 0.9900 . ?
C85 H85B 0.9900 . ?
C86 H86A 0.9900 . ?
C86 H86B 0.9900 . ?
C91 C96 1.521(4) . ?
C91 C92 1.535(4) . ?
C91 H91 1.0000 . ?
C92 C93 1.528(4) . ?
C92 H92A 0.9900 . ?
C92 H92B 0.9900 . ?
C93 C94 1.514(4) . ?
C93 H93A 0.9900 . ?
C93 H93B 0.9900 . ?
C94 C95 1.510(4) . ?
C94 H94A 0.9900 . ?
C94 H94B 0.9900 . ?
C95 C96 1.527(4) . ?
C95 H95A 0.9900 . ?
C95 H95B 0.9900 . ?
C96 H96A 0.9900 . ?
C96 H96B 0.9900 . ?
C101 C102 1.534(6) . ?
C101 C106 1.535(6) . ?
C101 H101 1.0000 . ?
C102 C103 1.531(6) . ?
C102 H10A 0.9900 . ?
C102 H10B 0.9900 . ?
C103 C104 1.517(6) . ?
C103 H10C 0.9900 . ?
C103 H10D 0.9900 . ?
C104 C105 1.520(6) . ?
C104 H10E 0.9900 . ?
C104 H10F 0.9900 . ?
C105 C106 1.563(7) . ?
C105 H10G 0.9900 . ?
C105 H10H 0.9900 . ?
C106 H10I 0.9900 . ?
C106 H10J 0.9900 . ?
C201 C202 1.510(8) . ?
C201 C206 1.579(9) . ?
C201 H201 1.0000 . ?
C202 C203 1.541(8) . ?
C202 H20A 0.9900 . ?
C202 H20B 0.9900 . ?
C203 C204 1.600(9) . ?
C203 H20C 0.9900 . ?
C203 H20D 0.9900 . ?
C204 C205 1.474(9) . ?
C204 H20E 0.9900 . ?
C204 H20F 0.9900 . ?
C205 C206 1.506(9) . ?
C205 H20G 0.9900 . ?
C205 H20H 0.9900 . ?
C206 H20I 0.9900 . ?
C206 H20J 0.9900 . ?
N3 B3 1.396(4) . ?
N3 P3 1.553(2) . ?
P3 C111 1.836(2) . ?
P3 C131 1.845(5) . ?
P3 C121 1.850(2) . ?
P3 C231 1.859(6) . ?
B3 C241 1.392(8) . ?
B3 C251 1.600(6) . ?
B3 C151 1.679(7) . ?
B3 C141 1.715(5) . ?
C111 C112 1.539(3) . ?
C111 C116 1.544(3) . ?
C111 H111 1.0000 . ?
C112 C113 1.528(4) . ?
C112 H11C 0.9900 . ?
C112 H11D 0.9900 . ?
C113 C114 1.528(4) . ?
C113 H11E 0.9900 . ?
C113 H11F 0.9900 . ?
C114 C115 1.521(4) . ?
C114 H11G 0.9900 . ?
C114 H11H 0.9900 . ?
C115 C116 1.531(4) . ?
C115 H11I 0.9900 . ?
C115 H11J 0.9900 . ?
C116 H11K 0.9900 . ?
C116 H11L 0.9900 . ?
C121 C126 1.534(3) . ?
C121 C122 1.539(4) . ?
C121 H121 1.0000 . ?
C122 C123 1.538(4) . ?
C122 H12E 0.9900 . ?
C122 H12F 0.9900 . ?
C123 C124 1.523(4) . ?
C123 H12G 0.9900 . ?
C123 H12H 0.9900 . ?
C124 C125 1.522(4) . ?
C124 H12I 0.9900 . ?
C124 H12J 0.9900 . ?
C125 C126 1.534(4) . ?
C125 H12K 0.9900 . ?
C125 H12L 0.9900 . ?
C126 H12M 0.9900 . ?
C126 H12N 0.9900 . ?
C131 C132 1.541(6) . ?
C131 C136 1.544(7) . ?
C131 H131 1.0000 . ?
C132 C133 1.532(6) . ?
C132 H13E 0.9900 . ?
C132 H13F 0.9900 . ?
C133 C134 1.530(7) . ?
C133 H13G 0.9900 . ?
C133 H13H 0.9900 . ?
C134 C135 1.516(8) . ?
C134 H13I 0.9900 . ?
C134 H13J 0.9900 . ?
C135 C136 1.532(7) . ?
C135 H13K 0.9900 . ?
C135 H13L 0.9900 . ?
C136 H13M 0.9900 . ?
C136 H13N 0.9900 . ?
C231 C236 1.522(7) . ?
C231 C232 1.530(7) . ?
C231 H231 1.0000 . ?
C232 C233 1.542(7) . ?
C232 H23E 0.9900 . ?
C232 H23F 0.9900 . ?
C233 C234 1.515(7) . ?
C233 H23G 0.9900 . ?
C233 H23H 0.9900 . ?
C234 C235 1.519(8) . ?
C234 H23I 0.9900 . ?
C234 H23J 0.9900 . ?
C235 C236 1.543(8) . ?
C235 H23K 0.9900 . ?
C235 H23L 0.9900 . ?
C236 H23M 0.9900 . ?
C236 H23N 0.9900 . ?
C141 C142 1.538(6) . ?
C141 C146 1.545(6) . ?
C141 H141 1.0000 . ?
C142 C143 1.548(6) . ?
C142 H14E 0.9900 . ?
C142 H14F 0.9900 . ?
C143 C144 1.506(6) . ?
C143 H14G 0.9900 . ?
C143 H14H 0.9900 . ?
C144 C145 1.513(6) . ?
C144 H14I 0.9900 . ?
C144 H14J 0.9900 . ?
C145 C146 1.528(6) . ?
C145 H14K 0.9900 . ?
C145 H14L 0.9900 . ?
C146 H14M 0.9900 . ?
C146 H14N 0.9900 . ?
C241 C242 1.550(8) . ?
C241 C246 1.561(8) . ?
C241 H241 1.0000 . ?
C242 C243 1.560(9) . ?
C242 H24E 0.9900 . ?
C242 H24F 0.9900 . ?
C243 C244 1.484(9) . ?
C243 H24G 0.9900 . ?
C243 H24H 0.9900 . ?
C244 C245 1.539(9) . ?
C244 H24I 0.9900 . ?
C244 H24J 0.9900 . ?
C245 C246 1.512(8) . ?
C245 H24K 0.9900 . ?
C245 H24L 0.9900 . ?
C246 H24M 0.9900 . ?
C246 H24N 0.9900 . ?
C151 C156 1.511(7) . ?
C151 C152 1.550(7) . ?
C151 H151 1.0000 . ?
C152 C153 1.556(7) . ?
C152 H15E 0.9900 . ?
C152 H15F 0.9900 . ?
C153 C154 1.507(8) . ?
C153 H15G 0.9900 . ?
C153 H15H 0.9900 . ?
C154 C155 1.561(8) . ?
C154 H15I 0.9900 . ?
C154 H15J 0.9900 . ?
C155 C156 1.545(8) . ?
C155 H15K 0.9900 . ?
C155 H15L 0.9900 . ?
C156 H15M 0.9900 . ?
C156 H15N 0.9900 . ?
C251 C252 1.494(7) . ?
C251 C256 1.545(7) . ?
C251 H251 1.0000 . ?
C252 C253 1.513(8) . ?
C252 H25E 0.9900 . ?
C252 H25F 0.9900 . ?
C253 C254 1.503(8) . ?
C253 H25G 0.9900 . ?
C253 H25H 0.9900 . ?
C254 C255 1.462(8) . ?
C254 H25I 0.9900 . ?
C254 H25J 0.9900 . ?
C255 C256 1.522(8) . ?
C255 H25K 0.9900 . ?
C255 H25L 0.9900 . ?
C256 H25M 0.9900 . ?
C256 H25N 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 C11A 111.9(4) . . ?
N1 P1 C21 112.60(15) . . ?
C11A P1 C21 107.7(3) . . ?
N1 P1 C31 111.12(11) . . ?
C11A P1 C31 107.2(3) . . ?
C21 P1 C31 105.99(17) . . ?
N1 P1 C11 108.1(3) . . ?
C21 P1 C11 109.0(3) . . ?
C31 P1 C11 110.0(3) . . ?
N1 P1 C21A 121.6(2) . . ?
C11A P1 C21A 98.2(4) . . ?
C31 P1 C21A 105.4(2) . . ?
C11 P1 C21A 99.9(3) . . ?
N1 B1 C51 125.4(2) . . ?
N1 B1 C41 117.0(2) . . ?
C51 B1 C41 117.68(19) . . ?
B1 N1 P1 134.93(18) . . ?
C16 C11 C12 110.7(6) . . ?
C16 C11 P1 110.2(6) . . ?
C12 C11 P1 110.4(6) . . ?
C16 C11 H11 108.5 . . ?
C12 C11 H11 108.5 . . ?
P1 C11 H11 108.5 . . ?
C13 C12 C11 111.9(7) . . ?
C13 C12 H12A 109.2 . . ?
C11 C12 H12A 109.2 . . ?
C13 C12 H12B 109.2 . . ?
C11 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
C14 C13 C12 111.3(6) . . ?
C14 C13 H13A 109.4 . . ?
C12 C13 H13A 109.4 . . ?
C14 C13 H13B 109.4 . . ?
C12 C13 H13B 109.4 . . ?
H13A C13 H13B 108.0 . . ?
C13 C14 C15 111.2(5) . . ?
C13 C14 H14A 109.4 . . ?
C15 C14 H14A 109.4 . . ?
C13 C14 H14B 109.4 . . ?
C15 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C14 C15 C16 110.1(4) . . ?
C14 C15 H15A 109.6 . . ?
C16 C15 H15A 109.6 . . ?
C14 C15 H15B 109.6 . . ?
C16 C15 H15B 109.6 . . ?
H15A C15 H15B 108.2 . . ?
C11 C16 C15 110.8(5) . . ?
C11 C16 H16A 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C11 C16 H16B 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 108.1 . . ?
C16A C11A C12A 110.4(7) . . ?
C16A C11A P1 115.5(7) . . ?
C12A C11A P1 109.5(7) . . ?
C16A C11A H11A 107.0 . . ?
C12A C11A H11A 107.0 . . ?
P1 C11A H11A 107.0 . . ?
C13A C12A C11A 110.7(8) . . ?
C13A C12A H12C 109.5 . . ?
C11A C12A H12C 109.5 . . ?
C13A C12A H12D 109.5 . . ?
C11A C12A H12D 109.5 . . ?
H12C C12A H12D 108.1 . . ?
C14A C13A C12A 111.8(7) . . ?
C14A C13A H13C 109.3 . . ?
C12A C13A H13C 109.3 . . ?
C14A C13A H13D 109.3 . . ?
C12A C13A H13D 109.3 . . ?
H13C C13A H13D 107.9 . . ?
C13A C14A C15A 110.3(6) . . ?
C13A C14A H14C 109.6 . . ?
C15A C14A H14C 109.6 . . ?
C13A C14A H14D 109.6 . . ?
C15A C14A H14D 109.6 . . ?
H14C C14A H14D 108.1 . . ?
C16A C15A C14A 111.6(5) . . ?
C16A C15A H15C 109.3 . . ?
C14A C15A H15C 109.3 . . ?
C16A C15A H15D 109.3 . . ?
C14A C15A H15D 109.3 . . ?
H15C C15A H15D 108.0 . . ?
C11A C16A C15A 112.2(6) . . ?
C11A C16A H16C 109.2 . . ?
C15A C16A H16C 109.2 . . ?
C11A C16A H16D 109.2 . . ?
C15A C16A H16D 109.2 . . ?
H16C C16A H16D 107.9 . . ?
C26 C21 C22 108.9(3) . . ?
C26 C21 P1 115.5(3) . . ?
C22 C21 P1 114.3(3) . . ?
C26 C21 H21 105.7 . . ?
C22 C21 H21 105.7 . . ?
P1 C21 H21 105.7 . . ?
C23 C22 C21 110.6(4) . . ?
C23 C22 H22A 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 108.1 . . ?
C22 C23 C24 112.2(4) . . ?
C22 C23 H23A 109.2 . . ?
C24 C23 H23A 109.2 . . ?
C22 C23 H23B 109.2 . . ?
C24 C23 H23B 109.2 . . ?
H23A C23 H23B 107.9 . . ?
C25 C24 C23 112.0(4) . . ?
C25 C24 H24A 109.2 . . ?
C23 C24 H24A 109.2 . . ?
C25 C24 H24B 109.2 . . ?
C23 C24 H24B 109.2 . . ?
H24A C24 H24B 107.9 . . ?
C24 C25 C26 111.8(4) . . ?
C24 C25 H25A 109.2 . . ?
C26 C25 H25A 109.2 . . ?
C24 C25 H25B 109.2 . . ?
C26 C25 H25B 109.2 . . ?
H25A C25 H25B 107.9 . . ?
C25 C26 C21 109.2(3) . . ?
C25 C26 H26A 109.8 . . ?
C21 C26 H26A 109.8 . . ?
C25 C26 H26B 109.8 . . ?
C21 C26 H26B 109.8 . . ?
H26A C26 H26B 108.3 . . ?
C26A C21A C22A 110.0(6) . . ?
C26A C21A P1 117.1(4) . . ?
C22A C21A P1 110.1(5) . . ?
C26A C21A H21A 106.3 . . ?
C22A C21A H21A 106.3 . . ?
P1 C21A H21A 106.3 . . ?
C23A C22A C21A 111.6(5) . . ?
C23A C22A H22C 109.3 . . ?
C21A C22A H22C 109.3 . . ?
C23A C22A H22D 109.3 . . ?
C21A C22A H22D 109.3 . . ?
H22C C22A H22D 108.0 . . ?
C24A C23A C22A 110.6(5) . . ?
C24A C23A H23C 109.5 . . ?
C22A C23A H23C 109.5 . . ?
C24A C23A H23D 109.5 . . ?
C22A C23A H23D 109.5 . . ?
H23C C23A H23D 108.1 . . ?
C23A C24A C25A 111.5(5) . . ?
C23A C24A H24C 109.3 . . ?
C25A C24A H24C 109.3 . . ?
C23A C24A H24D 109.3 . . ?
C25A C24A H24D 109.3 . . ?
H24C C24A H24D 108.0 . . ?
C24A C25A C26A 111.5(5) . . ?
C24A C25A H25C 109.3 . . ?
C26A C25A H25C 109.3 . . ?
C24A C25A H25D 109.3 . . ?
C26A C25A H25D 109.3 . . ?
H25C C25A H25D 108.0 . . ?
C21A C26A C25A 110.1(5) . . ?
C21A C26A H26C 109.6 . . ?
C25A C26A H26C 109.6 . . ?
C21A C26A H26D 109.6 . . ?
C25A C26A H26D 109.6 . . ?
H26C C26A H26D 108.1 . . ?
C36 C31 C32 110.2(2) . . ?
C36 C31 P1 116.18(18) . . ?
C32 C31 P1 113.97(16) . . ?
C36 C31 H31 105.1 . . ?
C32 C31 H31 105.1 . . ?
P1 C31 H31 105.1 . . ?
C33 C32 C31 110.9(2) . . ?
C33 C32 H32A 109.5 . . ?
C31 C32 H32A 109.5 . . ?
C33 C32 H32B 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 108.0 . . ?
C34 C33 C32 112.2(2) . . ?
C34 C33 H33A 109.2 . . ?
C32 C33 H33A 109.2 . . ?
C34 C33 H33B 109.2 . . ?
C32 C33 H33B 109.2 . . ?
H33A C33 H33B 107.9 . . ?
C33 C34 C35 110.4(3) . . ?
C33 C34 H34A 109.6 . . ?
C35 C34 H34A 109.6 . . ?
C33 C34 H34B 109.6 . . ?
C35 C34 H34B 109.6 . . ?
H34A C34 H34B 108.1 . . ?
C34 C35 C36 111.2(2) . . ?
C34 C35 H35A 109.4 . . ?
C36 C35 H35A 109.4 . . ?
C34 C35 H35B 109.4 . . ?
C36 C35 H35B 109.4 . . ?
H35A C35 H35B 108.0 . . ?
C31 C36 C35 110.6(3) . . ?
C31 C36 H36A 109.5 . . ?
C35 C36 H36A 109.5 . . ?
C31 C36 H36B 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 108.1 . . ?
C42 C41 C46 109.3(2) . . ?
C42 C41 B1 110.43(19) . . ?
C46 C41 B1 112.17(19) . . ?
C42 C41 H41 108.3 . . ?
C46 C41 H41 108.3 . . ?
B1 C41 H41 108.3 . . ?
C43 C42 C41 112.5(2) . . ?
C43 C42 H42A 109.1 . . ?
C41 C42 H42A 109.1 . . ?
C43 C42 H42B 109.1 . . ?
C41 C42 H42B 109.1 . . ?
H42A C42 H42B 107.8 . . ?
C44 C43 C42 111.2(2) . . ?
C44 C43 H43A 109.4 . . ?
C42 C43 H43A 109.4 . . ?
C44 C43 H43B 109.4 . . ?
C42 C43 H43B 109.4 . . ?
H43A C43 H43B 108.0 . . ?
C43 C44 C45 111.2(2) . . ?
C43 C44 H44A 109.4 . . ?
C45 C44 H44A 109.4 . . ?
C43 C44 H44B 109.4 . . ?
C45 C44 H44B 109.4 . . ?
H44A C44 H44B 108.0 . . ?
C46 C45 C44 111.8(2) . . ?
C46 C45 H45A 109.3 . . ?
C44 C45 H45A 109.3 . . ?
C46 C45 H45B 109.3 . . ?
C44 C45 H45B 109.3 . . ?
H45A C45 H45B 107.9 . . ?
C45 C46 C41 112.5(2) . . ?
C45 C46 H46A 109.1 . . ?
C41 C46 H46A 109.1 . . ?
C45 C46 H46B 109.1 . . ?
C41 C46 H46B 109.1 . . ?
H46A C46 H46B 107.8 . . ?
C52 C51 C56 109.05(19) . . ?
C52 C51 B1 110.68(19) . . ?
C56 C51 B1 113.53(19) . . ?
C52 C51 H51 107.8 . . ?
C56 C51 H51 107.8 . . ?
B1 C51 H51 107.8 . . ?
C53 C52 C51 112.5(2) . . ?
C53 C52 H52A 109.1 . . ?
C51 C52 H52A 109.1 . . ?
C53 C52 H52B 109.1 . . ?
C51 C52 H52B 109.1 . . ?
H52A C52 H52B 107.8 . . ?
C52 C53 C54 112.0(2) . . ?
C52 C53 H53A 109.2 . . ?
C54 C53 H53A 109.2 . . ?
C52 C53 H53B 109.2 . . ?
C54 C53 H53B 109.2 . . ?
H53A C53 H53B 107.9 . . ?
C53 C54 C55 110.7(2) . . ?
C53 C54 H54A 109.5 . . ?
C55 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
C55 C54 H54B 109.5 . . ?
H54A C54 H54B 108.1 . . ?
C56 C55 C54 110.9(2) . . ?
C56 C55 H55A 109.5 . . ?
C54 C55 H55A 109.5 . . ?
C56 C55 H55B 109.5 . . ?
C54 C55 H55B 109.5 . . ?
H55A C55 H55B 108.1 . . ?
C55 C56 C51 112.8(2) . . ?
C55 C56 H56A 109.0 . . ?
C51 C56 H56A 109.0 . . ?
C55 C56 H56B 109.0 . . ?
C51 C56 H56B 109.0 . . ?
H56A C56 H56B 107.8 . . ?
N2 P2 C61A 109.1(2) . . ?
N2 P2 C81 109.08(12) . . ?
C61A P2 C81 111.2(2) . . ?
N2 P2 C61 106.71(17) . . ?
C61A P2 C61 11.1(3) . . ?
C81 P2 C61 102.67(16) . . ?
N2 P2 C71 116.90(12) . . ?
C61A P2 C71 105.7(3) . . ?
C81 P2 C71 104.82(11) . . ?
C61 P2 C71 115.57(17) . . ?
B2 N2 P2 144.6(2) . . ?
N2 B2 C101 121.8(3) . . ?
N2 B2 C91 117.6(2) . . ?
C101 B2 C91 120.4(3) . . ?
N2 B2 C201 128.0(3) . . ?
C91 B2 C201 113.6(3) . . ?
C62 C61 C66 111.3(4) . . ?
C62 C61 P2 111.9(3) . . ?
C66 C61 P2 118.8(3) . . ?
C62 C61 H61 104.4 . . ?
C66 C61 H61 104.4 . . ?
P2 C61 H61 104.4 . . ?
C61 C62 C63 110.8(4) . . ?
C61 C62 H62A 109.5 . . ?
C63 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
C63 C62 H62B 109.5 . . ?
H62A C62 H62B 108.1 . . ?
C64 C63 C62 111.7(4) . . ?
C64 C63 H63A 109.3 . . ?
C62 C63 H63A 109.3 . . ?
C64 C63 H63B 109.3 . . ?
C62 C63 H63B 109.3 . . ?
H63A C63 H63B 107.9 . . ?
C65 C64 C63 110.3(4) . . ?
C65 C64 H64A 109.6 . . ?
C63 C64 H64A 109.6 . . ?
C65 C64 H64B 109.6 . . ?
C63 C64 H64B 109.6 . . ?
H64A C64 H64B 108.1 . . ?
C64 C65 C66 111.7(4) . . ?
C64 C65 H65A 109.3 . . ?
C66 C65 H65A 109.3 . . ?
C64 C65 H65B 109.3 . . ?
C66 C65 H65B 109.3 . . ?
H65A C65 H65B 107.9 . . ?
C65 C66 C61 110.4(4) . . ?
C65 C66 H66A 109.6 . . ?
C61 C66 H66A 109.6 . . ?
C65 C66 H66B 109.6 . . ?
C61 C66 H66B 109.6 . . ?
H66A C66 H66B 108.1 . . ?
C62A C61A C66A 110.0(6) . . ?
C62A C61A P2 118.5(5) . . ?
C66A C61A P2 114.5(5) . . ?
C62A C61A H61A 104.0 . . ?
C66A C61A H61A 104.0 . . ?
P2 C61A H61A 104.0 . . ?
C61A C62A C63A 111.3(5) . . ?
C61A C62A H62C 109.4 . . ?
C63A C62A H62C 109.4 . . ?
C61A C62A H62D 109.4 . . ?
C63A C62A H62D 109.4 . . ?
H62C C62A H62D 108.0 . . ?
C64A C63A C62A 110.2(6) . . ?
C64A C63A H63C 109.6 . . ?
C62A C63A H63C 109.6 . . ?
C64A C63A H63D 109.6 . . ?
C62A C63A H63D 109.6 . . ?
H63C C63A H63D 108.1 . . ?
C63A C64A C65A 111.9(6) . . ?
C63A C64A H64C 109.2 . . ?
C65A C64A H64C 109.2 . . ?
C63A C64A H64D 109.2 . . ?
C65A C64A H64D 109.2 . . ?
H64C C64A H64D 107.9 . . ?
C64A C65A C66A 110.8(6) . . ?
C64A C65A H65C 109.5 . . ?
C66A C65A H65C 109.5 . . ?
C64A C65A H65D 109.5 . . ?
C66A C65A H65D 109.5 . . ?
H65C C65A H65D 108.1 . . ?
C61A C66A C65A 109.1(6) . . ?
C61A C66A H66C 109.9 . . ?
C65A C66A H66C 109.9 . . ?
C61A C66A H66D 109.9 . . ?
C65A C66A H66D 109.9 . . ?
H66C C66A H66D 108.3 . . ?
C76 C71 C72 109.0(2) . . ?
C76 C71 P2 112.52(18) . . ?
C72 C71 P2 118.81(19) . . ?
C76 C71 H71 105.1 . . ?
C72 C71 H71 105.1 . . ?
P2 C71 H71 105.1 . . ?
C73 C72 C71 110.8(2) . . ?
C73 C72 H72A 109.5 . . ?
C71 C72 H72A 109.5 . . ?
C73 C72 H72B 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 108.1 . . ?
C74 C73 C72 111.5(3) . . ?
C74 C73 H73A 109.3 . . ?
C72 C73 H73A 109.3 . . ?
C74 C73 H73B 109.3 . . ?
C72 C73 H73B 109.3 . . ?
H73A C73 H73B 108.0 . . ?
C73 C74 C75 111.7(2) . . ?
C73 C74 H74A 109.3 . . ?
C75 C74 H74A 109.3 . . ?
C73 C74 H74B 109.3 . . ?
C75 C74 H74B 109.3 . . ?
H74A C74 H74B 107.9 . . ?
C76 C75 C74 110.4(3) . . ?
C76 C75 H75A 109.6 . . ?
C74 C75 H75A 109.6 . . ?
C76 C75 H75B 109.6 . . ?
C74 C75 H75B 109.6 . . ?
H75A C75 H75B 108.1 . . ?
C75 C76 C71 111.0(2) . . ?
C75 C76 H76A 109.4 . . ?
C71 C76 H76A 109.4 . . ?
C75 C76 H76B 109.4 . . ?
C71 C76 H76B 109.4 . . ?
H76A C76 H76B 108.0 . . ?
C82 C81 C86 110.4(2) . . ?
C82 C81 P2 109.68(17) . . ?
C86 C81 P2 112.18(17) . . ?
C82 C81 H81 108.2 . . ?
C86 C81 H81 108.2 . . ?
P2 C81 H81 108.2 . . ?
C83 C82 C81 111.6(2) . . ?
C83 C82 H82A 109.3 . . ?
C81 C82 H82A 109.3 . . ?
C83 C82 H82B 109.3 . . ?
C81 C82 H82B 109.3 . . ?
H82A C82 H82B 108.0 . . ?
C84 C83 C82 110.5(3) . . ?
C84 C83 H83A 109.5 . . ?
C82 C83 H83A 109.5 . . ?
C84 C83 H83B 109.5 . . ?
C82 C83 H83B 109.5 . . ?
H83A C83 H83B 108.1 . . ?
C83 C84 C85 110.7(2) . . ?
C83 C84 H84A 109.5 . . ?
C85 C84 H84A 109.5 . . ?
C83 C84 H84B 109.5 . . ?
C85 C84 H84B 109.5 . . ?
H84A C84 H84B 108.1 . . ?
C86 C85 C84 111.8(2) . . ?
C86 C85 H85A 109.2 . . ?
C84 C85 H85A 109.2 . . ?
C86 C85 H85B 109.2 . . ?
C84 C85 H85B 109.2 . . ?
H85A C85 H85B 107.9 . . ?
C85 C86 C81 111.6(2) . . ?
C85 C86 H86A 109.3 . . ?
C81 C86 H86A 109.3 . . ?
C85 C86 H86B 109.3 . . ?
C81 C86 H86B 109.3 . . ?
H86A C86 H86B 108.0 . . ?
C96 C91 C92 109.5(2) . . ?
C96 C91 B2 111.5(2) . . ?
C92 C91 B2 112.4(2) . . ?
C96 C91 H91 107.7 . . ?
C92 C91 H91 107.7 . . ?
B2 C91 H91 107.7 . . ?
C93 C92 C91 113.0(2) . . ?
C93 C92 H92A 109.0 . . ?
C91 C92 H92A 109.0 . . ?
C93 C92 H92B 109.0 . . ?
C91 C92 H92B 109.0 . . ?
H92A C92 H92B 107.8 . . ?
C94 C93 C92 111.2(3) . . ?
C94 C93 H93A 109.4 . . ?
C92 C93 H93A 109.4 . . ?
C94 C93 H93B 109.4 . . ?
C92 C93 H93B 109.4 . . ?
H93A C93 H93B 108.0 . . ?
C95 C94 C93 111.2(2) . . ?
C95 C94 H94A 109.4 . . ?
C93 C94 H94A 109.4 . . ?
C95 C94 H94B 109.4 . . ?
C93 C94 H94B 109.4 . . ?
H94A C94 H94B 108.0 . . ?
C94 C95 C96 112.1(2) . . ?
C94 C95 H95A 109.2 . . ?
C96 C95 H95A 109.2 . . ?
C94 C95 H95B 109.2 . . ?
C96 C95 H95B 109.2 . . ?
H95A C95 H95B 107.9 . . ?
C91 C96 C95 111.7(2) . . ?
C91 C96 H96A 109.3 . . ?
C95 C96 H96A 109.3 . . ?
C91 C96 H96B 109.3 . . ?
C95 C96 H96B 109.3 . . ?
H96A C96 H96B 107.9 . . ?
C102 C101 C106 106.8(4) . . ?
C102 C101 B2 105.4(3) . . ?
C106 C101 B2 117.0(4) . . ?
C102 C101 H101 109.1 . . ?
C106 C101 H101 109.1 . . ?
B2 C101 H101 109.1 . . ?
C103 C102 C101 112.7(4) . . ?
C103 C102 H10A 109.1 . . ?
C101 C102 H10A 109.1 . . ?
C103 C102 H10B 109.1 . . ?
C101 C102 H10B 109.1 . . ?
H10A C102 H10B 107.8 . . ?
C104 C103 C102 112.3(4) . . ?
C104 C103 H10C 109.1 . . ?
C102 C103 H10C 109.1 . . ?
C104 C103 H10D 109.1 . . ?
C102 C103 H10D 109.1 . . ?
H10C C103 H10D 107.9 . . ?
C103 C104 C105 104.1(4) . . ?
C103 C104 H10E 110.9 . . ?
C105 C104 H10E 110.9 . . ?
C103 C104 H10F 110.9 . . ?
C105 C104 H10F 110.9 . . ?
H10E C104 H10F 108.9 . . ?
C104 C105 C106 111.5(5) . . ?
C104 C105 H10G 109.3 . . ?
C106 C105 H10G 109.3 . . ?
C104 C105 H10H 109.3 . . ?
C106 C105 H10H 109.3 . . ?
H10G C105 H10H 108.0 . . ?
C101 C106 C105 111.9(4) . . ?
C101 C106 H10I 109.2 . . ?
C105 C106 H10I 109.2 . . ?
C101 C106 H10J 109.2 . . ?
C105 C106 H10J 109.2 . . ?
H10I C106 H10J 107.9 . . ?
C202 C201 C206 113.5(6) . . ?
C202 C201 B2 119.1(5) . . ?
C206 C201 B2 103.8(5) . . ?
C202 C201 H201 106.5 . . ?
C206 C201 H201 106.5 . . ?
B2 C201 H201 106.5 . . ?
C201 C202 C203 110.6(6) . . ?
C201 C202 H20A 109.5 . . ?
C203 C202 H20A 109.5 . . ?
C201 C202 H20B 109.5 . . ?
C203 C202 H20B 109.5 . . ?
H20A C202 H20B 108.1 . . ?
C202 C203 C204 110.2(6) . . ?
C202 C203 H20C 109.6 . . ?
C204 C203 H20C 109.6 . . ?
C202 C203 H20D 109.6 . . ?
C204 C203 H20D 109.6 . . ?
H20C C203 H20D 108.1 . . ?
C205 C204 C203 120.5(7) . . ?
C205 C204 H20E 107.2 . . ?
C203 C204 H20E 107.2 . . ?
C205 C204 H20F 107.2 . . ?
C203 C204 H20F 107.2 . . ?
H20E C204 H20F 106.8 . . ?
C204 C205 C206 111.1(7) . . ?
C204 C205 H20G 109.4 . . ?
C206 C205 H20G 109.4 . . ?
C204 C205 H20H 109.4 . . ?
C206 C205 H20H 109.4 . . ?
H20G C205 H20H 108.0 . . ?
C205 C206 C201 114.0(6) . . ?
C205 C206 H20I 108.8 . . ?
C201 C206 H20I 108.8 . . ?
C205 C206 H20J 108.8 . . ?
C201 C206 H20J 108.8 . . ?
H20I C206 H20J 107.7 . . ?
B3 N3 P3 155.4(2) . . ?
N3 P3 C111 109.97(12) . . ?
N3 P3 C131 106.36(18) . . ?
C111 P3 C131 105.40(18) . . ?
N3 P3 C121 116.36(12) . . ?
C111 P3 C121 105.05(11) . . ?
C131 P3 C121 113.18(18) . . ?
N3 P3 C231 114.22(19) . . ?
C111 P3 C231 109.7(2) . . ?
C121 P3 C231 100.83(19) . . ?
C241 B3 N3 122.7(4) . . ?
C241 B3 C251 100.2(4) . . ?
N3 B3 C251 136.7(4) . . ?
C241 B3 C151 123.7(4) . . ?
N3 B3 C151 113.4(3) . . ?
N3 B3 C141 116.4(3) . . ?
C251 B3 C141 106.9(3) . . ?
C151 B3 C141 130.2(3) . . ?
C112 C111 C116 109.2(2) . . ?
C112 C111 P3 113.02(17) . . ?
C116 C111 P3 109.69(16) . . ?
C112 C111 H111 108.3 . . ?
C116 C111 H111 108.3 . . ?
P3 C111 H111 108.3 . . ?
C113 C112 C111 110.8(2) . . ?
C113 C112 H11C 109.5 . . ?
C111 C112 H11C 109.5 . . ?
C113 C112 H11D 109.5 . . ?
C111 C112 H11D 109.5 . . ?
H11C C112 H11D 108.1 . . ?
C114 C113 C112 111.5(2) . . ?
C114 C113 H11E 109.3 . . ?
C112 C113 H11E 109.3 . . ?
C114 C113 H11F 109.3 . . ?
C112 C113 H11F 109.3 . . ?
H11E C113 H11F 108.0 . . ?
C115 C114 C113 111.0(2) . . ?
C115 C114 H11G 109.4 . . ?
C113 C114 H11G 109.4 . . ?
C115 C114 H11H 109.4 . . ?
C113 C114 H11H 109.4 . . ?
H11G C114 H11H 108.0 . . ?
C114 C115 C116 111.7(2) . . ?
C114 C115 H11I 109.3 . . ?
C116 C115 H11I 109.3 . . ?
C114 C115 H11J 109.3 . . ?
C116 C115 H11J 109.3 . . ?
H11I C115 H11J 107.9 . . ?
C115 C116 C111 111.6(2) . . ?
C115 C116 H11K 109.3 . . ?
C111 C116 H11K 109.3 . . ?
C115 C116 H11L 109.3 . . ?
C111 C116 H11L 109.3 . . ?
H11K C116 H11L 108.0 . . ?
C126 C121 C122 110.2(2) . . ?
C126 C121 P3 111.48(17) . . ?
C122 C121 P3 117.26(17) . . ?
C126 C121 H121 105.6 . . ?
C122 C121 H121 105.6 . . ?
P3 C121 H121 105.6 . . ?
C123 C122 C121 110.8(2) . . ?
C123 C122 H12E 109.5 . . ?
C121 C122 H12E 109.5 . . ?
C123 C122 H12F 109.5 . . ?
C121 C122 H12F 109.5 . . ?
H12E C122 H12F 108.1 . . ?
C124 C123 C122 111.4(2) . . ?
C124 C123 H12G 109.4 . . ?
C122 C123 H12G 109.4 . . ?
C124 C123 H12H 109.4 . . ?
C122 C123 H12H 109.4 . . ?
H12G C123 H12H 108.0 . . ?
C125 C124 C123 110.3(2) . . ?
C125 C124 H12I 109.6 . . ?
C123 C124 H12I 109.6 . . ?
C125 C124 H12J 109.6 . . ?
C123 C124 H12J 109.6 . . ?
H12I C124 H12J 108.1 . . ?
C124 C125 C126 110.5(2) . . ?
C124 C125 H12K 109.6 . . ?
C126 C125 H12K 109.6 . . ?
C124 C125 H12L 109.6 . . ?
C126 C125 H12L 109.6 . . ?
H12K C125 H12L 108.1 . . ?
C125 C126 C121 111.3(2) . . ?
C125 C126 H12M 109.4 . . ?
C121 C126 H12M 109.4 . . ?
C125 C126 H12N 109.4 . . ?
C121 C126 H12N 109.4 . . ?
H12M C126 H12N 108.0 . . ?
C132 C131 C136 110.0(4) . . ?
C132 C131 P3 114.5(3) . . ?
C136 C131 P3 114.7(3) . . ?
C132 C131 H131 105.6 . . ?
C136 C131 H131 105.6 . . ?
P3 C131 H131 105.6 . . ?
C133 C132 C131 111.1(4) . . ?
C133 C132 H13E 109.4 . . ?
C131 C132 H13E 109.4 . . ?
C133 C132 H13F 109.4 . . ?
C131 C132 H13F 109.4 . . ?
H13E C132 H13F 108.0 . . ?
C134 C133 C132 112.2(4) . . ?
C134 C133 H13G 109.2 . . ?
C132 C133 H13G 109.2 . . ?
C134 C133 H13H 109.2 . . ?
C132 C133 H13H 109.2 . . ?
H13G C133 H13H 107.9 . . ?
C135 C134 C133 112.2(5) . . ?
C135 C134 H13I 109.2 . . ?
C133 C134 H13I 109.2 . . ?
C135 C134 H13J 109.2 . . ?
C133 C134 H13J 109.2 . . ?
H13I C134 H13J 107.9 . . ?
C134 C135 C136 110.3(5) . . ?
C134 C135 H13K 109.6 . . ?
C136 C135 H13K 109.6 . . ?
C134 C135 H13L 109.6 . . ?
C136 C135 H13L 109.6 . . ?
H13K C135 H13L 108.1 . . ?
C135 C136 C131 112.0(4) . . ?
C135 C136 H13M 109.2 . . ?
C131 C136 H13M 109.2 . . ?
C135 C136 H13N 109.2 . . ?
C131 C136 H13N 109.2 . . ?
H13M C136 H13N 107.9 . . ?
C236 C231 C232 110.8(5) . . ?
C236 C231 P3 117.1(4) . . ?
C232 C231 P3 108.2(4) . . ?
C236 C231 H231 106.7 . . ?
C232 C231 H231 106.7 . . ?
P3 C231 H231 106.7 . . ?
C231 C232 C233 110.3(4) . . ?
C231 C232 H23E 109.6 . . ?
C233 C232 H23E 109.6 . . ?
C231 C232 H23F 109.6 . . ?
C233 C232 H23F 109.6 . . ?
H23E C232 H23F 108.1 . . ?
C234 C233 C232 113.1(5) . . ?
C234 C233 H23G 109.0 . . ?
C232 C233 H23G 109.0 . . ?
C234 C233 H23H 109.0 . . ?
C232 C233 H23H 109.0 . . ?
H23G C233 H23H 107.8 . . ?
C233 C234 C235 111.5(5) . . ?
C233 C234 H23I 109.3 . . ?
C235 C234 H23I 109.3 . . ?
C233 C234 H23J 109.3 . . ?
C235 C234 H23J 109.3 . . ?
H23I C234 H23J 108.0 . . ?
C234 C235 C236 111.0(5) . . ?
C234 C235 H23K 109.4 . . ?
C236 C235 H23K 109.4 . . ?
C234 C235 H23L 109.4 . . ?
C236 C235 H23L 109.4 . . ?
H23K C235 H23L 108.0 . . ?
C231 C236 C235 110.8(5) . . ?
C231 C236 H23M 109.5 . . ?
C235 C236 H23M 109.5 . . ?
C231 C236 H23N 109.5 . . ?
C235 C236 H23N 109.5 . . ?
H23M C236 H23N 108.1 . . ?
C142 C141 C146 108.1(4) . . ?
C142 C141 B3 113.4(3) . . ?
C146 C141 B3 108.4(3) . . ?
C142 C141 H141 109.0 . . ?
C146 C141 H141 109.0 . . ?
B3 C141 H141 109.0 . . ?
C141 C142 C143 111.8(4) . . ?
C141 C142 H14E 109.2 . . ?
C143 C142 H14E 109.2 . . ?
C141 C142 H14F 109.2 . . ?
C143 C142 H14F 109.2 . . ?
H14E C142 H14F 107.9 . . ?
C144 C143 C142 111.5(4) . . ?
C144 C143 H14G 109.3 . . ?
C142 C143 H14G 109.3 . . ?
C144 C143 H14H 109.3 . . ?
C142 C143 H14H 109.3 . . ?
H14G C143 H14H 108.0 . . ?
C143 C144 C145 112.4(4) . . ?
C143 C144 H14I 109.1 . . ?
C145 C144 H14I 109.1 . . ?
C143 C144 H14J 109.1 . . ?
C145 C144 H14J 109.1 . . ?
H14I C144 H14J 107.9 . . ?
C144 C145 C146 110.9(4) . . ?
C144 C145 H14K 109.5 . . ?
C146 C145 H14K 109.5 . . ?
C144 C145 H14L 109.5 . . ?
C146 C145 H14L 109.5 . . ?
H14K C145 H14L 108.0 . . ?
C145 C146 C141 112.6(4) . . ?
C145 C146 H14M 109.1 . . ?
C141 C146 H14M 109.1 . . ?
C145 C146 H14N 109.1 . . ?
C141 C146 H14N 109.1 . . ?
H14M C146 H14N 107.8 . . ?
B3 C241 C242 117.2(5) . . ?
B3 C241 C246 105.6(5) . . ?
C242 C241 C246 107.1(5) . . ?
B3 C241 H241 108.9 . . ?
C242 C241 H241 108.9 . . ?
C246 C241 H241 108.9 . . ?
C241 C242 C243 114.1(6) . . ?
C241 C242 H24E 108.7 . . ?
C243 C242 H24E 108.7 . . ?
C241 C242 H24F 108.7 . . ?
C243 C242 H24F 108.7 . . ?
H24E C242 H24F 107.6 . . ?
C244 C243 C242 110.9(6) . . ?
C244 C243 H24G 109.5 . . ?
C242 C243 H24G 109.5 . . ?
C244 C243 H24H 109.5 . . ?
C242 C243 H24H 109.5 . . ?
H24G C243 H24H 108.0 . . ?
C243 C244 C245 111.2(6) . . ?
C243 C244 H24I 109.4 . . ?
C245 C244 H24I 109.4 . . ?
C243 C244 H24J 109.4 . . ?
C245 C244 H24J 109.4 . . ?
H24I C244 H24J 108.0 . . ?
C246 C245 C244 111.3(6) . . ?
C246 C245 H24K 109.4 . . ?
C244 C245 H24K 109.4 . . ?
C246 C245 H24L 109.4 . . ?
C244 C245 H24L 109.4 . . ?
H24K C245 H24L 108.0 . . ?
C245 C246 C241 114.0(6) . . ?
C245 C246 H24M 108.8 . . ?
C241 C246 H24M 108.8 . . ?
C245 C246 H24N 108.8 . . ?
C241 C246 H24N 108.8 . . ?
H24M C246 H24N 107.7 . . ?
C156 C151 C152 109.9(5) . . ?
C156 C151 B3 109.2(4) . . ?
C152 C151 B3 109.6(4) . . ?
C156 C151 H151 109.4 . . ?
C152 C151 H151 109.4 . . ?
B3 C151 H151 109.4 . . ?
C151 C152 C153 112.6(5) . . ?
C151 C152 H15E 109.1 . . ?
C153 C152 H15E 109.1 . . ?
C151 C152 H15F 109.1 . . ?
C153 C152 H15F 109.1 . . ?
H15E C152 H15F 107.8 . . ?
C154 C153 C152 110.8(5) . . ?
C154 C153 H15G 109.5 . . ?
C152 C153 H15G 109.5 . . ?
C154 C153 H15H 109.5 . . ?
C152 C153 H15H 109.5 . . ?
H15G C153 H15H 108.1 . . ?
C153 C154 C155 111.1(5) . . ?
C153 C154 H15I 109.4 . . ?
C155 C154 H15I 109.4 . . ?
C153 C154 H15J 109.4 . . ?
C155 C154 H15J 109.4 . . ?
H15I C154 H15J 108.0 . . ?
C156 C155 C154 109.8(5) . . ?
C156 C155 H15K 109.7 . . ?
C154 C155 H15K 109.7 . . ?
C156 C155 H15L 109.7 . . ?
C154 C155 H15L 109.7 . . ?
H15K C155 H15L 108.2 . . ?
C151 C156 C155 113.4(5) . . ?
C151 C156 H15M 108.9 . . ?
C155 C156 H15M 108.9 . . ?
C151 C156 H15N 108.9 . . ?
C155 C156 H15N 108.9 . . ?
H15M C156 H15N 107.7 . . ?
C252 C251 C256 112.6(5) . . ?
C252 C251 B3 113.3(5) . . ?
C256 C251 B3 115.0(4) . . ?
C252 C251 H251 104.9 . . ?
C256 C251 H251 104.9 . . ?
B3 C251 H251 104.9 . . ?
C251 C252 C253 115.1(5) . . ?
C251 C252 H25E 108.5 . . ?
C253 C252 H25E 108.5 . . ?
C251 C252 H25F 108.5 . . ?
C253 C252 H25F 108.5 . . ?
H25E C252 H25F 107.5 . . ?
C254 C253 C252 112.5(6) . . ?
C254 C253 H25G 109.1 . . ?
C252 C253 H25G 109.1 . . ?
C254 C253 H25H 109.1 . . ?
C252 C253 H25H 109.1 . . ?
H25G C253 H25H 107.8 . . ?
C255 C254 C253 115.7(6) . . ?
C255 C254 H25I 108.3 . . ?
C253 C254 H25I 108.3 . . ?
C255 C254 H25J 108.4 . . ?
C253 C254 H25J 108.3 . . ?
H25I C254 H25J 107.4 . . ?
C254 C255 C256 115.4(6) . . ?
C254 C255 H25K 108.4 . . ?
C256 C255 H25K 108.4 . . ?
C254 C255 H25L 108.4 . . ?
C256 C255 H25L 108.4 . . ?
H25K C255 H25L 107.5 . . ?
C255 C256 C251 113.1(5) . . ?
C255 C256 H25M 109.0 . . ?
C251 C256 H25M 109.0 . . ?
C255 C256 H25N 109.0 . . ?
C251 C256 H25N 109.0 . . ?
H25M C256 H25N 107.8 . . ?
_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.813
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.055


data_compound_1d
_database_code_depnum_ccdc_archive 'CCDC 929291'
#TrackingRef 'cif_revised.txt'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H37 B N P'
_chemical_formula_weight         453.39
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
_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                   14.7239(10)
_cell_length_b                   17.3602(12)
_cell_length_c                   10.2259(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.271(2)
_cell_angle_gamma                90.00
_cell_volume                     2533.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9981
_cell_measurement_theta_min      2.75
_cell_measurement_theta_max      33.06
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             976
_exptl_absorpt_coefficient_mu    0.127
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9629
_exptl_absorpt_correction_T_max  0.9962
_exptl_absorpt_process_details   sadabs
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            15658
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.43
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4455
_reflns_number_gt                3818
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0509P)^2^+0.6166P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4455
_refine_ls_number_parameters     298
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_ref         0.0949
_refine_ls_wR_factor_gt          0.0887
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.082
_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 0.26645(2) 0.61745(2) 0.02404(3) 0.01608(11) Uani 1 1 d . . .
N1 N 0.21575(8) 0.55194(7) 0.08358(11) 0.0198(3) Uani 1 1 d . . .
B1 B 0.19277(11) 0.47327(9) 0.06724(15) 0.0178(3) Uani 1 1 d . . .
C11 C 0.36339(9) 0.65383(8) 0.15660(13) 0.0185(3) Uani 1 1 d . . .
C12 C 0.39574(10) 0.60960(9) 0.27185(15) 0.0263(3) Uani 1 1 d . . .
H12 H 0.3670 0.5615 0.2805 0.032 Uiso 1 1 calc R . .
C13 C 0.47001(11) 0.63538(11) 0.37465(16) 0.0348(4) Uani 1 1 d . . .
H13 H 0.4923 0.6044 0.4526 0.042 Uiso 1 1 calc R . .
C14 C 0.51145(11) 0.70557(10) 0.36420(16) 0.0340(4) Uani 1 1 d . . .
H14 H 0.5619 0.7230 0.4349 0.041 Uiso 1 1 calc R . .
C15 C 0.47938(11) 0.75044(9) 0.25057(17) 0.0315(4) Uani 1 1 d . . .
H15 H 0.5077 0.7989 0.2433 0.038 Uiso 1 1 calc R . .
C16 C 0.40590(10) 0.72493(9) 0.14705(15) 0.0250(3) Uani 1 1 d . . .
H16 H 0.3843 0.7560 0.0691 0.030 Uiso 1 1 calc R . .
C21 C 0.18980(9) 0.69847(8) -0.03291(13) 0.0176(3) Uani 1 1 d . . .
C22 C 0.21464(10) 0.75749(8) -0.11078(14) 0.0205(3) Uani 1 1 d . . .
H22 H 0.2719 0.7544 -0.1376 0.025 Uiso 1 1 calc R . .
C23 C 0.15607(10) 0.82040(8) -0.14894(14) 0.0215(3) Uani 1 1 d . . .
H23 H 0.1733 0.8605 -0.2013 0.026 Uiso 1 1 calc R . .
C24 C 0.07226(10) 0.82459(9) -0.11035(14) 0.0243(3) Uani 1 1 d . . .
H24 H 0.0323 0.8678 -0.1360 0.029 Uiso 1 1 calc R . .
C25 C 0.04637(10) 0.76595(9) -0.03443(14) 0.0253(3) Uani 1 1 d . . .
H25 H -0.0114 0.7690 -0.0089 0.030 Uiso 1 1 calc R . .
C26 C 0.10482(10) 0.70308(8) 0.00404(14) 0.0204(3) Uani 1 1 d . . .
H26 H 0.0870 0.6630 0.0558 0.024 Uiso 1 1 calc R . .
C31 C 0.31671(10) 0.59648(8) -0.11821(13) 0.0176(3) Uani 1 1 d . . .
C32 C 0.25873(10) 0.59676(8) -0.24911(14) 0.0225(3) Uani 1 1 d . . .
H32 H 0.1959 0.6143 -0.2642 0.027 Uiso 1 1 calc R . .
C33 C 0.29232(11) 0.57164(9) -0.35658(15) 0.0268(3) Uani 1 1 d . . .
H33 H 0.2527 0.5725 -0.4453 0.032 Uiso 1 1 calc R . .
C34 C 0.38331(11) 0.54530(9) -0.33546(15) 0.0277(4) Uani 1 1 d . . .
H34 H 0.4055 0.5268 -0.4093 0.033 Uiso 1 1 calc R . .
C35 C 0.44213(11) 0.54574(9) -0.20724(15) 0.0267(3) Uani 1 1 d . . .
H35 H 0.5049 0.5283 -0.1932 0.032 Uiso 1 1 calc R . .
C36 C 0.40926(10) 0.57186(8) -0.09862(14) 0.0209(3) Uani 1 1 d . . .
H36 H 0.4501 0.5729 -0.0107 0.025 Uiso 1 1 calc R . .
C41 C 0.21342(9) 0.42262(8) -0.05261(13) 0.0171(3) Uani 1 1 d . . .
H41 H 0.2070 0.4573 -0.1325 0.021 Uiso 1 1 calc R . .
C42 C 0.31599(10) 0.39400(8) -0.01301(15) 0.0221(3) Uani 1 1 d . . .
H42A H 0.3583 0.4385 0.0149 0.027 Uiso 1 1 calc R . .
H42B H 0.3243 0.3587 0.0650 0.027 Uiso 1 1 calc R . .
C43 C 0.34299(11) 0.35228(9) -0.12923(16) 0.0287(4) Uani 1 1 d . . .
H43A H 0.3405 0.3889 -0.2043 0.034 Uiso 1 1 calc R . .
H43B H 0.4081 0.3331 -0.0987 0.034 Uiso 1 1 calc R . .
C44 C 0.27727(11) 0.28476(9) -0.17955(16) 0.0284(4) Uani 1 1 d . . .
H44A H 0.2929 0.2619 -0.2600 0.034 Uiso 1 1 calc R . .
H44B H 0.2866 0.2447 -0.1086 0.034 Uiso 1 1 calc R . .
C45 C 0.17493(10) 0.30993(9) -0.21589(14) 0.0242(3) Uani 1 1 d . . .
H45A H 0.1343 0.2641 -0.2396 0.029 Uiso 1 1 calc R . .
H45B H 0.1634 0.3441 -0.2959 0.029 Uiso 1 1 calc R . .
C46 C 0.14953(10) 0.35264(9) -0.09867(14) 0.0213(3) Uani 1 1 d . . .
H46A H 0.1550 0.3168 -0.0218 0.026 Uiso 1 1 calc R . .
H46B H 0.0836 0.3701 -0.1271 0.026 Uiso 1 1 calc R . .
C51 C 0.15009(10) 0.43432(8) 0.18156(14) 0.0221(3) Uani 1 1 d . . .
H51 H 0.1392 0.3785 0.1591 0.026 Uiso 1 1 calc R . .
C52 C 0.05581(10) 0.47053(9) 0.18746(14) 0.0253(3) Uani 1 1 d . . .
H52A H 0.0640 0.5269 0.1993 0.030 Uiso 1 1 calc R . .
H52B H 0.0096 0.4613 0.1005 0.030 Uiso 1 1 calc R . .
C53 C 0.01711(11) 0.43815(10) 0.30222(15) 0.0302(4) Uani 1 1 d . . .
H53A H -0.0407 0.4663 0.3057 0.036 Uiso 1 1 calc R . .
H53B H 0.0007 0.3832 0.2843 0.036 Uiso 1 1 calc R . .
C54 C 0.08856(11) 0.44559(9) 0.43768(14) 0.0261(3) Uani 1 1 d . . .
H54A H 0.0997 0.5008 0.4602 0.031 Uiso 1 1 calc R . .
H54B H 0.0632 0.4215 0.5089 0.031 Uiso 1 1 calc R . .
C55 C 0.18092(11) 0.40710(9) 0.43456(15) 0.0266(3) Uani 1 1 d . . .
H55A H 0.1710 0.3510 0.4210 0.032 Uiso 1 1 calc R . .
H55B H 0.2269 0.4152 0.5221 0.032 Uiso 1 1 calc R . .
C56 C 0.21972(10) 0.44030(9) 0.32076(14) 0.0244(3) Uani 1 1 d . . .
H56A H 0.2779 0.4125 0.3181 0.029 Uiso 1 1 calc R . .
H56B H 0.2361 0.4951 0.3404 0.029 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.01898(19) 0.0139(2) 0.01650(19) 0.00022(14) 0.00659(15) -0.00042(14)
N1 0.0250(6) 0.0180(6) 0.0186(6) 0.0001(5) 0.0095(5) -0.0011(5)
B1 0.0163(7) 0.0178(8) 0.0184(8) 0.0013(6) 0.0025(6) 0.0015(6)
C11 0.0197(7) 0.0186(7) 0.0191(7) -0.0037(6) 0.0081(6) 0.0023(6)
C12 0.0265(8) 0.0285(9) 0.0237(8) 0.0025(6) 0.0060(6) -0.0015(6)
C13 0.0318(9) 0.0469(11) 0.0232(8) 0.0041(7) 0.0023(7) -0.0012(8)
C14 0.0264(8) 0.0471(11) 0.0267(8) -0.0139(8) 0.0034(7) -0.0037(8)
C15 0.0284(9) 0.0249(9) 0.0411(9) -0.0102(7) 0.0081(7) -0.0050(7)
C16 0.0258(8) 0.0202(8) 0.0286(8) -0.0009(6) 0.0061(6) -0.0008(6)
C21 0.0196(7) 0.0160(7) 0.0168(7) -0.0017(6) 0.0038(6) -0.0009(5)
C22 0.0209(7) 0.0200(7) 0.0213(7) 0.0007(6) 0.0066(6) -0.0002(6)
C23 0.0270(8) 0.0177(7) 0.0187(7) 0.0013(6) 0.0033(6) -0.0006(6)
C24 0.0257(8) 0.0215(8) 0.0236(7) 0.0005(6) 0.0021(6) 0.0060(6)
C25 0.0196(7) 0.0306(9) 0.0262(8) 0.0005(7) 0.0068(6) 0.0035(6)
C26 0.0222(7) 0.0206(8) 0.0187(7) 0.0014(6) 0.0056(6) -0.0022(6)
C31 0.0224(7) 0.0127(7) 0.0191(7) 0.0000(5) 0.0079(6) -0.0021(5)
C32 0.0227(7) 0.0210(8) 0.0228(7) -0.0009(6) 0.0036(6) -0.0021(6)
C33 0.0347(9) 0.0270(8) 0.0172(7) -0.0004(6) 0.0037(6) -0.0034(7)
C34 0.0378(9) 0.0272(9) 0.0222(8) -0.0030(7) 0.0156(7) -0.0033(7)
C35 0.0243(8) 0.0284(9) 0.0298(8) -0.0004(7) 0.0114(7) 0.0020(6)
C36 0.0226(7) 0.0205(8) 0.0198(7) -0.0003(6) 0.0057(6) -0.0005(6)
C41 0.0197(7) 0.0155(7) 0.0166(7) 0.0028(6) 0.0054(6) 0.0006(5)
C42 0.0191(7) 0.0185(7) 0.0285(8) -0.0018(6) 0.0057(6) -0.0024(6)
C43 0.0246(8) 0.0252(8) 0.0396(9) -0.0051(7) 0.0143(7) 0.0007(6)
C44 0.0326(9) 0.0215(8) 0.0335(9) -0.0071(7) 0.0127(7) 0.0013(7)
C45 0.0298(8) 0.0212(8) 0.0208(7) -0.0027(6) 0.0046(6) -0.0019(6)
C46 0.0196(7) 0.0232(8) 0.0210(7) -0.0015(6) 0.0048(6) -0.0023(6)
C51 0.0333(8) 0.0145(7) 0.0207(7) -0.0018(6) 0.0111(6) -0.0032(6)
C52 0.0242(8) 0.0299(9) 0.0216(7) 0.0022(6) 0.0052(6) -0.0061(6)
C53 0.0274(8) 0.0379(10) 0.0285(8) 0.0015(7) 0.0127(7) -0.0070(7)
C54 0.0338(9) 0.0259(8) 0.0226(7) 0.0011(6) 0.0146(7) -0.0024(7)
C55 0.0354(9) 0.0251(8) 0.0210(7) 0.0052(6) 0.0104(7) 0.0028(7)
C56 0.0271(8) 0.0250(8) 0.0232(7) 0.0055(6) 0.0101(6) 0.0055(6)
_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 1.5638(12) . ?
P1 C21 1.8075(14) . ?
P1 C11 1.8219(14) . ?
P1 C31 1.8240(13) . ?
N1 B1 1.407(2) . ?
B1 C41 1.597(2) . ?
B1 C51 1.606(2) . ?
C11 C12 1.389(2) . ?
C11 C16 1.398(2) . ?
C12 C13 1.391(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.378(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.382(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.387(2) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C26 1.3957(19) . ?
C21 C22 1.4005(19) . ?
C22 C23 1.387(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.387(2) . ?
C23 H23 0.9500 . ?
C24 C25 1.389(2) . ?
C24 H24 0.9500 . ?
C25 C26 1.386(2) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C36 1.395(2) . ?
C31 C32 1.399(2) . ?
C32 C33 1.382(2) . ?
C32 H32 0.9500 . ?
C33 C34 1.381(2) . ?
C33 H33 0.9500 . ?
C34 C35 1.382(2) . ?
C34 H34 0.9500 . ?
C35 C36 1.392(2) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C46 1.5376(19) . ?
C41 C42 1.5460(19) . ?
C41 H41 1.0000 . ?
C42 C43 1.526(2) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.526(2) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.524(2) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C46 1.5321(19) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C51 C56 1.539(2) . ?
C51 C52 1.538(2) . ?
C51 H51 1.0000 . ?
C52 C53 1.5322(19) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C54 1.524(2) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.523(2) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 C56 1.5299(19) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9900 . ?
C56 H56B 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 C21 111.79(6) . . ?
N1 P1 C11 108.91(6) . . ?
C21 P1 C11 106.41(6) . . ?
N1 P1 C31 119.46(6) . . ?
C21 P1 C31 104.02(6) . . ?
C11 P1 C31 105.38(6) . . ?
B1 N1 P1 141.59(10) . . ?
N1 B1 C41 122.66(12) . . ?
N1 B1 C51 116.61(12) . . ?
C41 B1 C51 120.62(12) . . ?
C12 C11 C16 118.79(14) . . ?
C12 C11 P1 118.79(11) . . ?
C16 C11 P1 122.41(11) . . ?
C11 C12 C13 120.31(15) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C14 C13 C12 120.43(15) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C13 C14 C15 119.83(15) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C14 C15 C16 120.16(15) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C15 C16 C11 120.47(15) . . ?
C15 C16 H16 119.8 . . ?
C11 C16 H16 119.8 . . ?
C26 C21 C22 119.29(13) . . ?
C26 C21 P1 119.19(11) . . ?
C22 C21 P1 121.51(10) . . ?
C23 C22 C21 120.31(13) . . ?
C23 C22 H22 119.8 . . ?
C21 C22 H22 119.8 . . ?
C24 C23 C22 119.76(14) . . ?
C24 C23 H23 120.1 . . ?
C22 C23 H23 120.1 . . ?
C23 C24 C25 120.44(14) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
C26 C25 C24 119.94(14) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C25 C26 C21 120.26(13) . . ?
C25 C26 H26 119.9 . . ?
C21 C26 H26 119.9 . . ?
C36 C31 C32 118.86(13) . . ?
C36 C31 P1 121.38(10) . . ?
C32 C31 P1 119.38(11) . . ?
C33 C32 C31 120.40(14) . . ?
C33 C32 H32 119.8 . . ?
C31 C32 H32 119.8 . . ?
C34 C33 C32 120.23(14) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C33 C34 C35 120.23(14) . . ?
C33 C34 H34 119.9 . . ?
C35 C34 H34 119.9 . . ?
C34 C35 C36 119.93(14) . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C35 C36 C31 120.31(13) . . ?
C35 C36 H36 119.8 . . ?
C31 C36 H36 119.8 . . ?
C46 C41 C42 108.10(11) . . ?
C46 C41 B1 116.88(11) . . ?
C42 C41 B1 109.53(11) . . ?
C46 C41 H41 107.3 . . ?
C42 C41 H41 107.3 . . ?
B1 C41 H41 107.3 . . ?
C43 C42 C41 111.95(12) . . ?
C43 C42 H42A 109.2 . . ?
C41 C42 H42A 109.2 . . ?
C43 C42 H42B 109.2 . . ?
C41 C42 H42B 109.2 . . ?
H42A C42 H42B 107.9 . . ?
C44 C43 C42 111.21(12) . . ?
C44 C43 H43A 109.4 . . ?
C42 C43 H43A 109.4 . . ?
C44 C43 H43B 109.4 . . ?
C42 C43 H43B 109.4 . . ?
H43A C43 H43B 108.0 . . ?
C45 C44 C43 111.62(12) . . ?
C45 C44 H44A 109.3 . . ?
C43 C44 H44A 109.3 . . ?
C45 C44 H44B 109.3 . . ?
C43 C44 H44B 109.3 . . ?
H44A C44 H44B 108.0 . . ?
C44 C45 C46 111.42(12) . . ?
C44 C45 H45A 109.3 . . ?
C46 C45 H45A 109.3 . . ?
C44 C45 H45B 109.3 . . ?
C46 C45 H45B 109.3 . . ?
H45A C45 H45B 108.0 . . ?
C45 C46 C41 111.91(11) . . ?
C45 C46 H46A 109.2 . . ?
C41 C46 H46A 109.2 . . ?
C45 C46 H46B 109.2 . . ?
C41 C46 H46B 109.2 . . ?
H46A C46 H46B 107.9 . . ?
C56 C51 C52 109.75(11) . . ?
C56 C51 B1 110.72(12) . . ?
C52 C51 B1 112.03(12) . . ?
C56 C51 H51 108.1 . . ?
C52 C51 H51 108.1 . . ?
B1 C51 H51 108.1 . . ?
C53 C52 C51 112.93(12) . . ?
C53 C52 H52A 109.0 . . ?
C51 C52 H52A 109.0 . . ?
C53 C52 H52B 109.0 . . ?
C51 C52 H52B 109.0 . . ?
H52A C52 H52B 107.8 . . ?
C54 C53 C52 111.17(12) . . ?
C54 C53 H53A 109.4 . . ?
C52 C53 H53A 109.4 . . ?
C54 C53 H53B 109.4 . . ?
C52 C53 H53B 109.4 . . ?
H53A C53 H53B 108.0 . . ?
C55 C54 C53 111.32(12) . . ?
C55 C54 H54A 109.4 . . ?
C53 C54 H54A 109.4 . . ?
C55 C54 H54B 109.4 . . ?
C53 C54 H54B 109.4 . . ?
H54A C54 H54B 108.0 . . ?
C54 C55 C56 110.70(12) . . ?
C54 C55 H55A 109.5 . . ?
C56 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
C56 C55 H55B 109.5 . . ?
H55A C55 H55B 108.1 . . ?
C55 C56 C51 112.93(12) . . ?
C55 C56 H56A 109.0 . . ?
C51 C56 H56A 109.0 . . ?
C55 C56 H56B 109.0 . . ?
C51 C56 H56B 109.0 . . ?
H56A C56 H56B 107.8 . . ?
_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.037


data_compound_2a
_database_code_depnum_ccdc_archive 'CCDC 929292'
#TrackingRef 'cif_revised.txt'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H27 B F10 N P'
_chemical_formula_sum            'C24 H27 B F10 N P'
_chemical_formula_weight         561.25
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'
_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
'x-1/2, y, -z-1/2'
_cell_length_a                   17.7955(11)
_cell_length_b                   14.0784(8)
_cell_length_c                   20.1991(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5060.5(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6601
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      27.84
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2304
_exptl_absorpt_coefficient_mu    0.197
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9617
_exptl_absorpt_correction_T_max  0.9617
_exptl_absorpt_process_details   sadabs
_exptl_special_details           
;
APEX2, Bruker AXS, Madison, WI, USA.
;
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31559
_diffrn_reflns_av_R_equivalents  0.0791
_diffrn_reflns_av_unetI/netI     0.0756
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.02
_diffrn_reflns_theta_max         28.33
_reflns_number_total             6290
_reflns_number_gt                3742
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SHELXTL XPREP'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Mercury v3.0'
_computing_publication_material  'Bruker SHELXTL XCIF'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
Structure solved by direct methods to reveal all non-H atoms. H atoms added
at calculated positions and refined with a riding model. All non-H atoms
refined anisotropically.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1129P)^2^+2.4172P] where P=(Fo^2^+2Fc^2^)/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         6290
_refine_ls_number_parameters     343
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1233
_refine_ls_R_factor_gt           0.0672
_refine_ls_wR_factor_ref         0.2150
_refine_ls_wR_factor_gt          0.1770
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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 0.09252(5) 0.13710(6) 0.19030(4) 0.0180(2) Uani 1 1 d . . .
N1 N 0.09546(17) 0.1906(2) 0.12276(12) 0.0253(6) Uani 1 1 d . . .
B1 B 0.0940(2) 0.2236(3) 0.06030(16) 0.0199(7) Uani 1 1 d . . .
C11 C 0.02694(18) 0.2892(2) 0.03153(14) 0.0203(7) Uani 1 1 d . . .
F12 F 0.03717(13) 0.40198(15) 0.11803(9) 0.0359(5) Uani 1 1 d . . .
C12 C 0.00350(19) 0.3720(2) 0.06191(14) 0.0242(7) Uani 1 1 d . . .
F13 F -0.07550(13) 0.50705(16) 0.07029(10) 0.0406(6) Uani 1 1 d . . .
C13 C -0.0545(2) 0.4272(2) 0.03864(17) 0.0274(8) Uani 1 1 d . . .
F14 F -0.14791(13) 0.45467(17) -0.04274(11) 0.0442(6) Uani 1 1 d . . .
C14 C -0.09125(19) 0.4018(3) -0.01899(17) 0.0296(8) Uani 1 1 d . . .
F15 F -0.10642(13) 0.29334(17) -0.10645(10) 0.0437(6) Uani 1 1 d . . .
C15 C -0.0694(2) 0.3205(3) -0.05143(16) 0.0292(8) Uani 1 1 d . . .
F16 F 0.00786(12) 0.18823(15) -0.05997(9) 0.0352(5) Uani 1 1 d . . .
C16 C -0.01094(19) 0.2672(2) -0.02640(15) 0.0247(7) Uani 1 1 d . . .
C21 C 0.16108(18) 0.2048(2) 0.00814(14) 0.0205(7) Uani 1 1 d . . .
F22 F 0.21263(13) 0.35298(16) 0.03634(11) 0.0406(6) Uani 1 1 d . . .
C22 C 0.21619(19) 0.2728(3) 0.00018(16) 0.0268(7) Uani 1 1 d . . .
F23 F 0.32809(13) 0.3308(2) -0.04901(13) 0.0536(7) Uani 1 1 d . . .
C23 C 0.27603(19) 0.2628(3) -0.04376(17) 0.0315(8) Uani 1 1 d . . .
F24 F 0.33630(13) 0.17284(19) -0.12605(10) 0.0467(6) Uani 1 1 d . . .
C24 C 0.2803(2) 0.1828(3) -0.08132(16) 0.0312(8) Uani 1 1 d . . .
F25 F 0.23214(15) 0.03389(17) -0.11194(11) 0.0508(7) Uani 1 1 d . . .
C25 C 0.2272(2) 0.1129(3) -0.07474(15) 0.0313(8) Uani 1 1 d . . .
F26 F 0.11857(13) 0.05364(15) -0.02492(11) 0.0416(6) Uani 1 1 d . . .
C26 C 0.1694(2) 0.1242(2) -0.03030(15) 0.0253(7) Uani 1 1 d . . .
C31 C 0.1391(3) 0.0186(3) 0.18256(18) 0.0398(10) Uani 1 1 d . . .
C32 C 0.0834(3) -0.0469(3) 0.1418(2) 0.0665(16) Uani 1 1 d . . .
H32A H 0.0741 -0.0184 0.0983 0.100 Uiso 1 1 calc R . .
H32B H 0.0358 -0.0529 0.1658 0.100 Uiso 1 1 calc R . .
H32C H 0.1058 -0.1099 0.1360 0.100 Uiso 1 1 calc R . .
C33 C 0.2086(3) 0.0254(4) 0.1423(3) 0.0705(16) Uani 1 1 d . . .
H33A H 0.2478 0.0576 0.1680 0.106 Uiso 1 1 calc R . .
H33B H 0.1983 0.0617 0.1019 0.106 Uiso 1 1 calc R . .
H33C H 0.2257 -0.0385 0.1304 0.106 Uiso 1 1 calc R . .
C34 C 0.1530(3) -0.0336(3) 0.2474(2) 0.0445(10) Uani 1 1 d . . .
H34A H 0.1732 -0.0970 0.2380 0.067 Uiso 1 1 calc R . .
H34B H 0.1057 -0.0396 0.2717 0.067 Uiso 1 1 calc R . .
H34C H 0.1893 0.0021 0.2741 0.067 Uiso 1 1 calc R . .
C41 C 0.1438(2) 0.2121(3) 0.25301(17) 0.0322(8) Uani 1 1 d . . .
C42 C 0.1311(3) 0.3162(3) 0.2410(2) 0.0542(13) Uani 1 1 d . . .
H42A H 0.0776 0.3308 0.2465 0.081 Uiso 1 1 calc R . .
H42B H 0.1467 0.3323 0.1959 0.081 Uiso 1 1 calc R . .
H42C H 0.1605 0.3533 0.2728 0.081 Uiso 1 1 calc R . .
C43 C 0.2310(3) 0.1998(4) 0.2424(2) 0.0571(13) Uani 1 1 d . . .
H43A H 0.2437 0.2142 0.1963 0.086 Uiso 1 1 calc R . .
H43B H 0.2454 0.1342 0.2526 0.086 Uiso 1 1 calc R . .
H43C H 0.2581 0.2433 0.2718 0.086 Uiso 1 1 calc R . .
C44 C 0.1294(3) 0.1840(3) 0.32483(18) 0.0420(10) Uani 1 1 d . . .
H44A H 0.1605 0.2231 0.3541 0.063 Uiso 1 1 calc R . .
H44B H 0.1421 0.1169 0.3311 0.063 Uiso 1 1 calc R . .
H44C H 0.0762 0.1940 0.3354 0.063 Uiso 1 1 calc R . .
C51 C -0.0090(2) 0.1248(3) 0.21498(18) 0.0393(10) Uani 1 1 d . . .
C52 C -0.0553(3) 0.1007(4) 0.1555(2) 0.0657(16) Uani 1 1 d . . .
H52A H -0.0451 0.0351 0.1421 0.099 Uiso 1 1 calc R . .
H52B H -0.0425 0.1438 0.1191 0.099 Uiso 1 1 calc R . .
H52C H -0.1087 0.1075 0.1663 0.099 Uiso 1 1 calc R . .
C53 C -0.0247(2) 0.0564(3) 0.27240(17) 0.0383(9) Uani 1 1 d . . .
H53A H -0.0788 0.0547 0.2813 0.057 Uiso 1 1 calc R . .
H53B H 0.0019 0.0782 0.3121 0.057 Uiso 1 1 calc R . .
H53C H -0.0072 -0.0074 0.2606 0.057 Uiso 1 1 calc R . .
C54 C -0.0389(2) 0.2261(3) 0.2364(2) 0.0511(12) Uani 1 1 d . . .
H54A H -0.0287 0.2721 0.2011 0.077 Uiso 1 1 calc R . .
H54B H -0.0133 0.2463 0.2770 0.077 Uiso 1 1 calc R . .
H54C H -0.0931 0.2228 0.2444 0.077 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0196(4) 0.0194(4) 0.0151(4) 0.0018(3) -0.0017(3) -0.0005(3)
N1 0.0351(16) 0.0258(15) 0.0151(12) 0.0009(10) 0.0003(12) -0.0018(13)
B1 0.0247(18) 0.0162(17) 0.0187(16) -0.0018(12) 0.0008(15) -0.0016(15)
C11 0.0239(16) 0.0218(17) 0.0154(14) 0.0022(11) 0.0046(12) -0.0023(14)
F12 0.0521(14) 0.0311(12) 0.0244(10) -0.0093(8) -0.0057(9) 0.0065(11)
C12 0.0300(17) 0.0255(18) 0.0172(14) 0.0014(12) 0.0024(13) 0.0013(15)
F13 0.0511(14) 0.0321(12) 0.0386(12) -0.0041(9) 0.0061(10) 0.0178(11)
C13 0.0299(18) 0.0227(18) 0.0296(17) 0.0024(13) 0.0091(15) 0.0045(15)
F14 0.0362(12) 0.0492(15) 0.0471(13) 0.0145(11) -0.0036(10) 0.0140(12)
C14 0.0232(17) 0.035(2) 0.0309(18) 0.0112(15) 0.0011(15) 0.0050(16)
F15 0.0418(13) 0.0551(16) 0.0342(12) -0.0023(10) -0.0171(10) 0.0032(12)
C15 0.0265(17) 0.041(2) 0.0204(16) 0.0041(15) -0.0049(13) -0.0039(17)
F16 0.0374(12) 0.0397(13) 0.0286(10) -0.0140(9) -0.0086(9) 0.0045(10)
C16 0.0240(17) 0.0289(18) 0.0210(15) -0.0025(13) 0.0013(13) -0.0022(15)
C21 0.0217(15) 0.0249(17) 0.0150(14) 0.0002(12) -0.0032(12) 0.0039(14)
F22 0.0411(13) 0.0349(13) 0.0457(13) -0.0133(10) 0.0081(10) -0.0109(11)
C22 0.0308(18) 0.0270(19) 0.0226(16) -0.0016(13) -0.0018(14) 0.0025(16)
F23 0.0336(13) 0.0643(18) 0.0629(16) 0.0046(13) 0.0152(12) -0.0158(13)
C23 0.0230(17) 0.045(2) 0.0260(17) 0.0118(15) 0.0000(14) -0.0012(17)
F24 0.0332(12) 0.0776(18) 0.0291(11) 0.0086(11) 0.0140(10) 0.0161(12)
C24 0.0264(18) 0.050(2) 0.0174(15) 0.0085(15) 0.0051(14) 0.0126(17)
F25 0.0637(16) 0.0473(15) 0.0413(13) -0.0202(11) 0.0130(12) 0.0130(13)
C25 0.040(2) 0.037(2) 0.0168(15) -0.0009(13) 0.0018(14) 0.0144(18)
F26 0.0501(14) 0.0299(12) 0.0448(13) -0.0106(9) 0.0116(11) -0.0088(11)
C26 0.0278(17) 0.0259(18) 0.0221(16) -0.0008(13) 0.0006(13) 0.0000(15)
C31 0.066(3) 0.0240(19) 0.0296(18) -0.0012(14) -0.0034(19) 0.015(2)
C32 0.111(5) 0.034(3) 0.054(3) -0.012(2) -0.024(3) 0.006(3)
C33 0.082(4) 0.067(4) 0.063(3) 0.001(3) 0.025(3) 0.043(3)
C34 0.057(3) 0.033(2) 0.044(2) 0.0116(17) -0.007(2) 0.013(2)
C41 0.048(2) 0.0257(18) 0.0233(16) -0.0022(14) -0.0069(16) -0.0084(17)
C42 0.086(4) 0.035(2) 0.041(2) -0.0029(18) -0.011(2) -0.021(3)
C43 0.043(3) 0.076(4) 0.052(3) -0.008(2) -0.005(2) -0.018(3)
C44 0.056(3) 0.045(3) 0.0251(18) 0.0017(16) -0.0121(18) -0.010(2)
C51 0.0225(18) 0.063(3) 0.0323(19) 0.0174(18) -0.0038(15) -0.0083(19)
C52 0.038(2) 0.108(5) 0.051(3) 0.029(3) -0.015(2) -0.019(3)
C53 0.033(2) 0.047(2) 0.0344(19) 0.0136(17) 0.0047(17) -0.0135(19)
C54 0.038(2) 0.065(3) 0.051(3) 0.015(2) 0.010(2) 0.014(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
P1 N1 1.560(3) . ?
P1 C31 1.870(4) . ?
P1 C51 1.882(4) . ?
P1 C41 1.885(3) . ?
N1 B1 1.344(4) . ?
B1 C21 1.614(5) . ?
B1 C11 1.617(5) . ?
C11 C12 1.382(5) . ?
C11 C16 1.385(4) . ?
F12 C12 1.350(4) . ?
C12 C13 1.375(5) . ?
F13 C13 1.346(4) . ?
C13 C14 1.382(5) . ?
F14 C14 1.342(4) . ?
C14 C15 1.374(5) . ?
F15 C15 1.347(4) . ?
C15 C16 1.379(5) . ?
F16 C16 1.345(4) . ?
C21 C22 1.379(5) . ?
C21 C26 1.383(4) . ?
F22 C22 1.346(4) . ?
C22 C23 1.393(5) . ?
F23 C23 1.336(4) . ?
C23 C24 1.361(5) . ?
F24 C24 1.353(4) . ?
C24 C25 1.371(5) . ?
F25 C25 1.345(4) . ?
C25 C26 1.375(5) . ?
F26 C26 1.347(4) . ?
C31 C33 1.483(7) . ?
C31 C34 1.522(5) . ?
C31 C32 1.585(6) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C41 C42 1.503(5) . ?
C41 C44 1.526(5) . ?
C41 C43 1.575(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 . ?
C51 C52 1.497(6) . ?
C51 C53 1.533(5) . ?
C51 C54 1.583(6) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 P1 C31 110.07(16) . . ?
N1 P1 C51 107.96(16) . . ?
C31 P1 C51 111.5(2) . . ?
N1 P1 C41 107.52(15) . . ?
C31 P1 C41 109.94(18) . . ?
C51 P1 C41 109.79(18) . . ?
B1 N1 P1 170.8(3) . . ?
N1 B1 C21 122.8(3) . . ?
N1 B1 C11 123.3(3) . . ?
C21 B1 C11 113.9(3) . . ?
C12 C11 C16 114.6(3) . . ?
C12 C11 B1 123.0(3) . . ?
C16 C11 B1 122.4(3) . . ?
F12 C12 C13 116.3(3) . . ?
F12 C12 C11 120.2(3) . . ?
C13 C12 C11 123.5(3) . . ?
F13 C13 C12 121.2(3) . . ?
F13 C13 C14 119.0(3) . . ?
C12 C13 C14 119.8(3) . . ?
F14 C14 C15 120.2(3) . . ?
F14 C14 C13 120.9(3) . . ?
C15 C14 C13 118.9(3) . . ?
F15 C15 C14 119.5(3) . . ?
F15 C15 C16 121.1(3) . . ?
C14 C15 C16 119.4(3) . . ?
F16 C16 C15 116.9(3) . . ?
F16 C16 C11 119.3(3) . . ?
C15 C16 C11 123.7(3) . . ?
C22 C21 C26 115.3(3) . . ?
C22 C21 B1 119.2(3) . . ?
C26 C21 B1 125.4(3) . . ?
F22 C22 C21 119.0(3) . . ?
F22 C22 C23 117.8(3) . . ?
C21 C22 C23 123.2(3) . . ?
F23 C23 C24 120.7(3) . . ?
F23 C23 C22 120.6(3) . . ?
C24 C23 C22 118.7(3) . . ?
F24 C24 C23 119.9(4) . . ?
F24 C24 C25 119.9(3) . . ?
C23 C24 C25 120.1(3) . . ?
F25 C25 C24 119.6(3) . . ?
F25 C25 C26 120.6(4) . . ?
C24 C25 C26 119.7(3) . . ?
F26 C26 C25 118.0(3) . . ?
F26 C26 C21 119.2(3) . . ?
C25 C26 C21 122.8(3) . . ?
C33 C31 C34 111.5(4) . . ?
C33 C31 C32 105.9(4) . . ?
C34 C31 C32 105.5(4) . . ?
C33 C31 P1 111.0(3) . . ?
C34 C31 P1 115.6(3) . . ?
C32 C31 P1 106.5(3) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C42 C41 C44 112.4(3) . . ?
C42 C41 C43 103.5(4) . . ?
C44 C41 C43 105.5(3) . . ?
C42 C41 P1 111.4(3) . . ?
C44 C41 P1 114.3(3) . . ?
C43 C41 P1 108.9(3) . . ?
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 . . ?
C52 C51 C53 111.4(4) . . ?
C52 C51 C54 103.8(4) . . ?
C53 C51 C54 107.3(3) . . ?
C52 C51 P1 109.7(3) . . ?
C53 C51 P1 115.7(3) . . ?
C54 C51 P1 108.2(3) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C31 P1 N1 B1 48.1(19) . . . . ?
C51 P1 N1 B1 -73.8(18) . . . . ?
C41 P1 N1 B1 167.8(18) . . . . ?
P1 N1 B1 C21 -82.4(19) . . . . ?
P1 N1 B1 C11 100.4(18) . . . . ?
N1 B1 C11 C12 53.3(5) . . . . ?
C21 B1 C11 C12 -124.1(3) . . . . ?
N1 B1 C11 C16 -127.7(4) . . . . ?
C21 B1 C11 C16 54.9(4) . . . . ?
C16 C11 C12 F12 -178.7(3) . . . . ?
B1 C11 C12 F12 0.4(5) . . . . ?
C16 C11 C12 C13 2.4(5) . . . . ?
B1 C11 C12 C13 -178.6(3) . . . . ?
F12 C12 C13 F13 0.6(5) . . . . ?
C11 C12 C13 F13 179.6(3) . . . . ?
F12 C12 C13 C14 179.3(3) . . . . ?
C11 C12 C13 C14 -1.7(5) . . . . ?
F13 C13 C14 F14 -1.1(5) . . . . ?
C12 C13 C14 F14 -179.8(3) . . . . ?
F13 C13 C14 C15 179.6(3) . . . . ?
C12 C13 C14 C15 0.9(5) . . . . ?
F14 C14 C15 F15 -1.4(5) . . . . ?
C13 C14 C15 F15 177.8(3) . . . . ?
F14 C14 C15 C16 179.8(3) . . . . ?
C13 C14 C15 C16 -1.0(5) . . . . ?
F15 C15 C16 F16 1.0(5) . . . . ?
C14 C15 C16 F16 179.7(3) . . . . ?
F15 C15 C16 C11 -177.0(3) . . . . ?
C14 C15 C16 C11 1.8(5) . . . . ?
C12 C11 C16 F16 179.7(3) . . . . ?
B1 C11 C16 F16 0.6(5) . . . . ?
C12 C11 C16 C15 -2.4(5) . . . . ?
B1 C11 C16 C15 178.5(3) . . . . ?
N1 B1 C21 C22 -95.5(4) . . . . ?
C11 B1 C21 C22 82.0(4) . . . . ?
N1 B1 C21 C26 84.0(4) . . . . ?
C11 B1 C21 C26 -98.6(4) . . . . ?
C26 C21 C22 F22 -179.3(3) . . . . ?
B1 C21 C22 F22 0.2(4) . . . . ?
C26 C21 C22 C23 0.7(5) . . . . ?
B1 C21 C22 C23 -179.8(3) . . . . ?
F22 C22 C23 F23 0.5(5) . . . . ?
C21 C22 C23 F23 -179.5(3) . . . . ?
F22 C22 C23 C24 -179.3(3) . . . . ?
C21 C22 C23 C24 0.7(5) . . . . ?
F23 C23 C24 F24 -2.1(5) . . . . ?
C22 C23 C24 F24 177.7(3) . . . . ?
F23 C23 C24 C25 179.0(3) . . . . ?
C22 C23 C24 C25 -1.2(5) . . . . ?
F24 C24 C25 F25 1.4(5) . . . . ?
C23 C24 C25 F25 -179.7(3) . . . . ?
F24 C24 C25 C26 -178.5(3) . . . . ?
C23 C24 C25 C26 0.4(5) . . . . ?
F25 C25 C26 F26 0.5(5) . . . . ?
C24 C25 C26 F26 -179.5(3) . . . . ?
F25 C25 C26 C21 -178.8(3) . . . . ?
C24 C25 C26 C21 1.1(5) . . . . ?
C22 C21 C26 F26 179.1(3) . . . . ?
B1 C21 C26 F26 -0.4(5) . . . . ?
C22 C21 C26 C25 -1.6(5) . . . . ?
B1 C21 C26 C25 178.9(3) . . . . ?
N1 P1 C31 C33 41.0(4) . . . . ?
C51 P1 C31 C33 160.8(3) . . . . ?
C41 P1 C31 C33 -77.2(4) . . . . ?
N1 P1 C31 C34 169.3(3) . . . . ?
C51 P1 C31 C34 -71.0(4) . . . . ?
C41 P1 C31 C34 51.0(4) . . . . ?
N1 P1 C31 C32 -73.9(3) . . . . ?
C51 P1 C31 C32 45.9(3) . . . . ?
C41 P1 C31 C32 167.9(3) . . . . ?
N1 P1 C41 C42 36.1(3) . . . . ?
C31 P1 C41 C42 156.0(3) . . . . ?
C51 P1 C41 C42 -81.1(3) . . . . ?
N1 P1 C41 C44 164.9(3) . . . . ?
C31 P1 C41 C44 -75.3(3) . . . . ?
C51 P1 C41 C44 47.7(3) . . . . ?
N1 P1 C41 C43 -77.4(3) . . . . ?
C31 P1 C41 C43 42.4(3) . . . . ?
C51 P1 C41 C43 165.4(3) . . . . ?
N1 P1 C51 C52 40.7(4) . . . . ?
C31 P1 C51 C52 -80.3(4) . . . . ?
C41 P1 C51 C52 157.7(3) . . . . ?
N1 P1 C51 C53 167.7(3) . . . . ?
C31 P1 C51 C53 46.7(4) . . . . ?
C41 P1 C51 C53 -75.3(3) . . . . ?
N1 P1 C51 C54 -71.8(3) . . . . ?
C31 P1 C51 C54 167.2(2) . . . . ?
C41 P1 C51 C54 45.1(3) . . . . ?
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        28.33
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.040
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.088


data_compound_2b
_database_code_depnum_ccdc_archive 'CCDC 929293'
#TrackingRef 'cif_revised.txt'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H15 B F10 N P'
_chemical_formula_sum            'C30 H15 B F10 N P'
_chemical_formula_weight         621.21
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
_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                   8.1259(18)
_cell_length_b                   10.9061(15)
_cell_length_c                   15.541(2)
_cell_angle_alpha                74.213(8)
_cell_angle_beta                 86.100(9)
_cell_angle_gamma                89.851(8)
_cell_volume                     1322.0(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3103
_cell_measurement_theta_min      2.66
_cell_measurement_theta_max      29.87
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             624
_exptl_absorpt_coefficient_mu    0.198
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9616
_exptl_absorpt_correction_T_max  0.9805
_exptl_absorpt_process_details   multi-scan
_exptl_special_details           
;
APEX2, Bruker AXS, Wisconsin, USA
The crystal moved during the latter stages of data collection leading
to an abrupt drop in correlation coefficient and poor centring of
reflections in the final set of frames. Integration using all data
afforded a dataset with a large GOF in the cell refinement (GOF = 12.5)
and large R(int) = 0.135. Omission of the final series of frames led to
a much improved cell refinement (GOF = 5.70 and R(int) = 0.031. Taking
into account redundancy in the data this maintained 96% of the expected
data.
;
_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 APEX2 area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11563
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         27.50
_reflns_number_total             5846
_reflns_number_gt                4244
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The structure was solved by direct methods to reveal all non-H atoms.
All non-H atoms were refined anisotropically and H atoms at calculated
positions and refined with a riding model.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0567P)^2^+0.5187P] where P=(Fo^2^+2Fc^2^)/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         5846
_refine_ls_number_parameters     388
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0483
_refine_ls_wR_factor_ref         0.1302
_refine_ls_wR_factor_gt          0.1171
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_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 0.02212(7) 0.15077(6) 0.21270(4) 0.01957(15) Uani 1 1 d . . .
N1 N 0.1263(2) 0.27884(18) 0.17941(13) 0.0232(4) Uani 1 1 d . . .
B1 B 0.1483(3) 0.3883(3) 0.20373(18) 0.0216(5) Uani 1 1 d . . .
C11 C 0.2719(3) 0.4974(2) 0.14345(15) 0.0198(5) Uani 1 1 d . . .
F12 F 0.17689(18) 0.47878(14) 0.00624(9) 0.0320(3) Uani 1 1 d . . .
C12 C 0.2798(3) 0.5330(2) 0.05043(16) 0.0219(5) Uani 1 1 d . . .
F13 F 0.39142(19) 0.65494(14) -0.09203(9) 0.0333(4) Uani 1 1 d . . .
C13 C 0.3893(3) 0.6242(2) -0.00200(15) 0.0226(5) Uani 1 1 d . . .
F14 F 0.60241(18) 0.77429(14) -0.01246(10) 0.0341(4) Uani 1 1 d . . .
C14 C 0.4962(3) 0.6851(2) 0.03793(16) 0.0228(5) Uani 1 1 d . . .
F15 F 0.60069(19) 0.71118(14) 0.16966(10) 0.0352(4) Uani 1 1 d . . .
C15 C 0.4954(3) 0.6532(2) 0.13014(16) 0.0240(5) Uani 1 1 d . . .
F16 F 0.39170(18) 0.52956(13) 0.27085(9) 0.0290(3) Uani 1 1 d . . .
C16 C 0.3847(3) 0.5610(2) 0.18036(15) 0.0209(5) Uani 1 1 d . . .
C21 C 0.0548(3) 0.4157(2) 0.29112(15) 0.0221(5) Uani 1 1 d . . .
F22 F -0.0847(2) 0.59176(15) 0.20429(10) 0.0416(4) Uani 1 1 d . . .
C22 C -0.0605(3) 0.5111(2) 0.28538(16) 0.0265(5) Uani 1 1 d . . .
F23 F -0.2667(2) 0.62086(17) 0.34934(12) 0.0499(5) Uani 1 1 d . . .
C23 C -0.1559(3) 0.5276(2) 0.35838(18) 0.0312(6) Uani 1 1 d . . .
F24 F -0.2309(2) 0.45659(17) 0.51351(11) 0.0463(4) Uani 1 1 d . . .
C24 C -0.1369(3) 0.4447(3) 0.44168(17) 0.0316(6) Uani 1 1 d . . .
F25 F 0.0015(2) 0.27164(16) 0.53294(10) 0.0455(4) Uani 1 1 d . . .
C25 C -0.0213(3) 0.3506(2) 0.45101(16) 0.0298(6) Uani 1 1 d . . .
F26 F 0.18476(19) 0.24398(14) 0.38955(10) 0.0346(4) Uani 1 1 d . . .
C26 C 0.0717(3) 0.3376(2) 0.37669(16) 0.0249(5) Uani 1 1 d . . .
C31 C -0.1360(3) 0.1390(2) 0.30311(15) 0.0209(5) Uani 1 1 d . . .
C32 C -0.2624(3) 0.2282(2) 0.28833(16) 0.0240(5) Uani 1 1 d . . .
H32 H -0.2681 0.2866 0.2308 0.029 Uiso 1 1 calc R . .
C33 C -0.3798(3) 0.2321(2) 0.35691(17) 0.0282(5) Uani 1 1 d . . .
H33 H -0.4648 0.2933 0.3466 0.034 Uiso 1 1 calc R . .
C34 C -0.3712(3) 0.1457(2) 0.44058(17) 0.0304(6) Uani 1 1 d . . .
H34 H -0.4509 0.1482 0.4877 0.036 Uiso 1 1 calc R . .
C35 C -0.2482(3) 0.0560(2) 0.45618(17) 0.0314(6) Uani 1 1 d . . .
H35 H -0.2443 -0.0030 0.5136 0.038 Uiso 1 1 calc R . .
C36 C -0.1300(3) 0.0524(2) 0.38751(16) 0.0254(5) Uani 1 1 d . . .
H36 H -0.0453 -0.0090 0.3982 0.030 Uiso 1 1 calc R . .
C41 C 0.1598(3) 0.0193(2) 0.25045(15) 0.0223(5) Uani 1 1 d . . .
C46 C 0.3172(3) 0.0441(2) 0.27175(16) 0.0252(5) Uani 1 1 d . . .
H46 H 0.3529 0.1295 0.2641 0.030 Uiso 1 1 calc R . .
C42 C 0.1093(3) -0.1070(2) 0.26089(16) 0.0259(5) Uani 1 1 d . . .
H42 H 0.0016 -0.1251 0.2469 0.031 Uiso 1 1 calc R . .
C43 C 0.2172(3) -0.2055(2) 0.29172(17) 0.0290(6) Uani 1 1 d . . .
H43 H 0.1833 -0.2909 0.2977 0.035 Uiso 1 1 calc R . .
C44 C 0.3736(3) -0.1808(3) 0.31386(17) 0.0314(6) Uani 1 1 d . . .
H44 H 0.4464 -0.2489 0.3355 0.038 Uiso 1 1 calc R . .
C45 C 0.4230(3) -0.0560(3) 0.30423(17) 0.0318(6) Uani 1 1 d . . .
H45 H 0.5298 -0.0386 0.3199 0.038 Uiso 1 1 calc R . .
C51 C -0.0820(3) 0.1254(2) 0.12016(15) 0.0197(5) Uani 1 1 d . . .
C52 C -0.2190(3) 0.0425(2) 0.13431(16) 0.0247(5) Uani 1 1 d . . .
H52 H -0.2620 0.0020 0.1936 0.030 Uiso 1 1 calc R . .
C53 C -0.2916(3) 0.0197(2) 0.06218(17) 0.0267(5) Uani 1 1 d . . .
H53 H -0.3847 -0.0361 0.0718 0.032 Uiso 1 1 calc R . .
C54 C -0.2281(3) 0.0787(2) -0.02466(16) 0.0261(5) Uani 1 1 d . . .
H54 H -0.2770 0.0617 -0.0741 0.031 Uiso 1 1 calc R . .
C55 C -0.0944(3) 0.1616(2) -0.03943(16) 0.0251(5) Uani 1 1 d . . .
H55 H -0.0525 0.2022 -0.0989 0.030 Uiso 1 1 calc R . .
C56 C -0.0211(3) 0.1858(2) 0.03295(15) 0.0222(5) Uani 1 1 d . . .
H56 H 0.0703 0.2433 0.0228 0.027 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0201(3) 0.0190(3) 0.0199(3) -0.0062(2) 0.0010(2) -0.0021(2)
N1 0.0243(11) 0.0218(10) 0.0234(10) -0.0065(8) 0.0011(8) -0.0040(8)
B1 0.0187(13) 0.0237(14) 0.0222(13) -0.0060(11) -0.0016(10) 0.0003(10)
C11 0.0186(11) 0.0158(11) 0.0253(12) -0.0065(9) 0.0004(9) 0.0000(9)
F12 0.0333(8) 0.0366(8) 0.0278(8) -0.0107(6) -0.0070(6) -0.0069(6)
C12 0.0200(11) 0.0207(12) 0.0273(12) -0.0098(10) -0.0050(9) 0.0029(9)
F13 0.0373(9) 0.0389(9) 0.0203(7) -0.0028(6) 0.0006(6) 0.0028(7)
C13 0.0233(12) 0.0238(12) 0.0198(12) -0.0046(9) -0.0002(9) 0.0066(9)
F14 0.0295(8) 0.0308(8) 0.0382(9) -0.0053(7) 0.0085(7) -0.0086(6)
C14 0.0184(11) 0.0176(11) 0.0292(13) -0.0025(9) 0.0051(9) 0.0011(9)
F15 0.0316(8) 0.0361(9) 0.0400(9) -0.0134(7) -0.0043(7) -0.0118(7)
C15 0.0219(12) 0.0207(12) 0.0317(13) -0.0107(10) -0.0028(10) -0.0032(9)
F16 0.0348(8) 0.0298(8) 0.0228(7) -0.0072(6) -0.0040(6) -0.0046(6)
C16 0.0252(12) 0.0185(11) 0.0189(11) -0.0045(9) -0.0019(9) 0.0027(9)
C21 0.0236(12) 0.0202(12) 0.0231(12) -0.0073(9) 0.0004(9) -0.0034(9)
F22 0.0474(10) 0.0372(9) 0.0326(9) 0.0019(7) 0.0021(7) 0.0154(8)
C22 0.0275(13) 0.0252(13) 0.0266(13) -0.0069(10) -0.0002(10) -0.0007(10)
F23 0.0455(11) 0.0537(11) 0.0529(11) -0.0198(9) 0.0002(8) 0.0261(8)
C23 0.0275(14) 0.0312(14) 0.0377(15) -0.0147(12) -0.0001(11) 0.0056(11)
F24 0.0432(10) 0.0641(12) 0.0370(9) -0.0269(8) 0.0127(7) 0.0006(8)
C24 0.0306(14) 0.0415(16) 0.0277(13) -0.0194(12) 0.0041(11) -0.0056(12)
F25 0.0626(12) 0.0495(10) 0.0212(8) -0.0053(7) 0.0006(7) 0.0031(9)
C25 0.0356(15) 0.0332(14) 0.0206(12) -0.0073(11) -0.0007(10) -0.0062(11)
F26 0.0401(9) 0.0316(8) 0.0316(8) -0.0072(7) -0.0047(7) 0.0127(7)
C26 0.0278(13) 0.0214(12) 0.0275(13) -0.0101(10) -0.0016(10) 0.0007(10)
C31 0.0209(12) 0.0228(12) 0.0207(11) -0.0092(9) -0.0004(9) -0.0048(9)
C32 0.0252(12) 0.0249(13) 0.0216(12) -0.0052(10) -0.0041(9) -0.0015(10)
C33 0.0231(13) 0.0309(14) 0.0330(14) -0.0134(11) 0.0008(10) 0.0007(10)
C34 0.0285(14) 0.0359(15) 0.0267(13) -0.0108(11) 0.0081(10) -0.0051(11)
C35 0.0360(15) 0.0322(14) 0.0228(13) -0.0030(11) 0.0016(11) -0.0024(11)
C36 0.0267(13) 0.0227(12) 0.0245(12) -0.0034(10) 0.0008(10) -0.0012(10)
C41 0.0239(12) 0.0249(12) 0.0189(11) -0.0080(9) 0.0016(9) -0.0008(9)
C46 0.0218(12) 0.0270(13) 0.0275(13) -0.0090(10) -0.0001(10) 0.0008(10)
C42 0.0266(13) 0.0262(13) 0.0261(13) -0.0101(10) 0.0008(10) -0.0024(10)
C43 0.0349(14) 0.0230(13) 0.0293(13) -0.0082(10) 0.0008(11) 0.0026(11)
C44 0.0337(14) 0.0322(14) 0.0268(13) -0.0069(11) 0.0023(11) 0.0113(11)
C45 0.0252(13) 0.0419(16) 0.0292(14) -0.0117(12) 0.0001(10) 0.0041(11)
C51 0.0201(11) 0.0185(11) 0.0216(11) -0.0082(9) 0.0008(9) 0.0020(9)
C52 0.0247(12) 0.0259(13) 0.0234(12) -0.0072(10) 0.0009(9) -0.0039(10)
C53 0.0247(12) 0.0248(13) 0.0335(14) -0.0129(11) -0.0024(10) -0.0015(10)
C54 0.0296(13) 0.0261(13) 0.0258(13) -0.0113(10) -0.0068(10) 0.0054(10)
C55 0.0298(13) 0.0253(13) 0.0193(12) -0.0052(10) 0.0007(10) 0.0041(10)
C56 0.0220(12) 0.0192(11) 0.0248(12) -0.0058(9) 0.0016(9) 0.0002(9)
_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 1.578(2) . ?
P1 C51 1.801(2) . ?
P1 C41 1.809(2) . ?
P1 C31 1.816(2) . ?
N1 B1 1.362(3) . ?
B1 C11 1.604(3) . ?
B1 C21 1.609(3) . ?
C11 C12 1.388(3) . ?
C11 C16 1.394(3) . ?
F12 C12 1.350(3) . ?
C12 C13 1.382(3) . ?
F13 C13 1.346(3) . ?
C13 C14 1.372(3) . ?
F14 C14 1.343(3) . ?
C14 C15 1.379(3) . ?
F15 C15 1.339(3) . ?
C15 C16 1.383(3) . ?
F16 C16 1.359(3) . ?
C21 C26 1.386(3) . ?
C21 C22 1.387(3) . ?
F22 C22 1.353(3) . ?
C22 C23 1.383(3) . ?
F23 C23 1.341(3) . ?
C23 C24 1.381(4) . ?
F24 C24 1.345(3) . ?
C24 C25 1.375(4) . ?
F25 C25 1.354(3) . ?
C25 C26 1.377(3) . ?
F26 C26 1.355(3) . ?
C31 C36 1.396(3) . ?
C31 C32 1.400(3) . ?
C32 C33 1.390(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.389(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.383(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.395(3) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C46 1.389(3) . ?
C41 C42 1.402(3) . ?
C46 C45 1.393(3) . ?
C46 H46 0.9500 . ?
C42 C43 1.387(4) . ?
C42 H42 0.9500 . ?
C43 C44 1.385(4) . ?
C43 H43 0.9500 . ?
C44 C45 1.386(4) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C51 C56 1.393(3) . ?
C51 C52 1.404(3) . ?
C52 C53 1.381(3) . ?
C52 H52 0.9500 . ?
C53 C54 1.391(3) . ?
C53 H53 0.9500 . ?
C54 C55 1.382(3) . ?
C54 H54 0.9500 . ?
C55 C56 1.394(3) . ?
C55 H55 0.9500 . ?
C56 H56 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 C51 108.95(11) . . ?
N1 P1 C41 109.21(11) . . ?
C51 P1 C41 108.19(10) . . ?
N1 P1 C31 117.45(10) . . ?
C51 P1 C31 106.11(11) . . ?
C41 P1 C31 106.57(11) . . ?
B1 N1 P1 138.83(18) . . ?
N1 B1 C11 119.7(2) . . ?
N1 B1 C21 123.2(2) . . ?
C11 B1 C21 117.13(19) . . ?
C12 C11 C16 114.4(2) . . ?
C12 C11 B1 123.0(2) . . ?
C16 C11 B1 122.6(2) . . ?
F12 C12 C13 116.3(2) . . ?
F12 C12 C11 120.4(2) . . ?
C13 C12 C11 123.3(2) . . ?
F13 C13 C14 119.5(2) . . ?
F13 C13 C12 120.8(2) . . ?
C14 C13 C12 119.8(2) . . ?
F14 C14 C13 120.2(2) . . ?
F14 C14 C15 120.1(2) . . ?
C13 C14 C15 119.7(2) . . ?
F15 C15 C14 120.1(2) . . ?
F15 C15 C16 121.1(2) . . ?
C14 C15 C16 118.9(2) . . ?
F16 C16 C15 116.9(2) . . ?
F16 C16 C11 119.1(2) . . ?
C15 C16 C11 123.9(2) . . ?
C26 C21 C22 115.2(2) . . ?
C26 C21 B1 122.2(2) . . ?
C22 C21 B1 122.3(2) . . ?
F22 C22 C23 117.4(2) . . ?
F22 C22 C21 119.1(2) . . ?
C23 C22 C21 123.5(2) . . ?
F23 C23 C24 120.0(2) . . ?
F23 C23 C22 121.3(2) . . ?
C24 C23 C22 118.7(2) . . ?
F24 C24 C25 120.2(2) . . ?
F24 C24 C23 120.0(2) . . ?
C25 C24 C23 119.9(2) . . ?
F25 C25 C24 120.1(2) . . ?
F25 C25 C26 120.2(2) . . ?
C24 C25 C26 119.7(2) . . ?
F26 C26 C25 117.4(2) . . ?
F26 C26 C21 119.6(2) . . ?
C25 C26 C21 123.0(2) . . ?
C36 C31 C32 119.2(2) . . ?
C36 C31 P1 123.20(18) . . ?
C32 C31 P1 117.43(18) . . ?
C33 C32 C31 120.7(2) . . ?
C33 C32 H32 119.6 . . ?
C31 C32 H32 119.6 . . ?
C34 C33 C32 119.3(2) . . ?
C34 C33 H33 120.4 . . ?
C32 C33 H33 120.4 . . ?
C35 C34 C33 120.8(2) . . ?
C35 C34 H34 119.6 . . ?
C33 C34 H34 119.6 . . ?
C34 C35 C36 119.9(2) . . ?
C34 C35 H35 120.1 . . ?
C36 C35 H35 120.1 . . ?
C35 C36 C31 120.1(2) . . ?
C35 C36 H36 120.0 . . ?
C31 C36 H36 120.0 . . ?
C46 C41 C42 119.4(2) . . ?
C46 C41 P1 119.16(18) . . ?
C42 C41 P1 121.42(19) . . ?
C41 C46 C45 120.2(2) . . ?
C41 C46 H46 119.9 . . ?
C45 C46 H46 119.9 . . ?
C43 C42 C41 119.8(2) . . ?
C43 C42 H42 120.1 . . ?
C41 C42 H42 120.1 . . ?
C44 C43 C42 120.8(2) . . ?
C44 C43 H43 119.6 . . ?
C42 C43 H43 119.6 . . ?
C43 C44 C45 119.4(2) . . ?
C43 C44 H44 120.3 . . ?
C45 C44 H44 120.3 . . ?
C44 C45 C46 120.4(3) . . ?
C44 C45 H45 119.8 . . ?
C46 C45 H45 119.8 . . ?
C56 C51 C52 119.6(2) . . ?
C56 C51 P1 119.13(17) . . ?
C52 C51 P1 121.27(17) . . ?
C53 C52 C51 120.2(2) . . ?
C53 C52 H52 119.9 . . ?
C51 C52 H52 119.9 . . ?
C52 C53 C54 119.9(2) . . ?
C52 C53 H53 120.1 . . ?
C54 C53 H53 120.1 . . ?
C55 C54 C53 120.5(2) . . ?
C55 C54 H54 119.8 . . ?
C53 C54 H54 119.8 . . ?
C54 C55 C56 120.0(2) . . ?
C54 C55 H55 120.0 . . ?
C56 C55 H55 120.0 . . ?
C51 C56 C55 119.9(2) . . ?
C51 C56 H56 120.0 . . ?
C55 C56 H56 120.0 . . ?
_diffrn_measured_fraction_theta_max 0.961
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.961
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.063


data_compound_2c
_database_code_depnum_ccdc_archive 'CCDC 929294'
#TrackingRef 'cif_revised.txt'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H15 B F10 N P'
_chemical_formula_sum            'C32 H15 B F10 N P'
_chemical_formula_weight         645.23
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
_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                   10.4324(3)
_cell_length_b                   11.2938(3)
_cell_length_c                   13.4201(3)
_cell_angle_alpha                87.9772(14)
_cell_angle_beta                 69.0838(13)
_cell_angle_gamma                71.1715(12)
_cell_volume                     1392.22(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8640
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      27.46
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             648
_exptl_absorpt_coefficient_mu    0.191
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9628
_exptl_absorpt_correction_T_max  0.9812
_exptl_absorpt_process_details   sadabs
_exptl_special_details           
;
Saint Plus, Bruker AXS, Madison, WI, USA.
;
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17206
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.63
_diffrn_reflns_theta_max         27.51
_reflns_number_total             6298
_reflns_number_gt                4746
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT, v6.45a'
_computing_data_reduction        'Bruker SHELXTL XPREP'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Mercury v2.3'
_computing_publication_material  'Bruker SHELXTL XCIF'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
Structure solved by direct methods. All non-H atoms refined anisotropically
H atoms added at calculated positions and refined with a riding model.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+0.6645P] where P=(Fo^2^+2Fc^2^)/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         6298
_refine_ls_number_parameters     406
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0410
_refine_ls_wR_factor_ref         0.0961
_refine_ls_wR_factor_gt          0.0866
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_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 0.61461(5) 0.70053(4) 0.70870(3) 0.02056(11) Uani 1 1 d . . .
N1 N 0.75289(15) 0.59123(12) 0.71073(11) 0.0226(3) Uani 1 1 d . . .
C1 C 0.62510(19) 0.95210(16) 0.74245(14) 0.0249(4) Uani 1 1 d . . .
C2 C 0.60693(19) 0.85530(16) 0.72905(14) 0.0258(4) Uani 1 1 d . . .
B1 B 0.8767(2) 0.58423(17) 0.72842(14) 0.0201(4) Uani 1 1 d . . .
C11 C 0.59268(18) 0.69257(16) 0.58246(13) 0.0241(4) Uani 1 1 d . . .
C12 C 0.6543(2) 0.57967(18) 0.51880(14) 0.0287(4) Uani 1 1 d . . .
H12 H 0.7150 0.5079 0.5385 0.034 Uiso 1 1 calc R . .
C13 C 0.6262(2) 0.5728(2) 0.42593(15) 0.0362(5) Uani 1 1 d . . .
H13 H 0.6670 0.4956 0.3823 0.043 Uiso 1 1 calc R . .
C14 C 0.5392(2) 0.6776(2) 0.39674(16) 0.0422(5) Uani 1 1 d . . .
H14 H 0.5200 0.6722 0.3333 0.051 Uiso 1 1 calc R . .
C15 C 0.4800(2) 0.7904(2) 0.45955(17) 0.0469(6) Uani 1 1 d . . .
H15 H 0.4214 0.8626 0.4386 0.056 Uiso 1 1 calc R . .
C16 C 0.5057(2) 0.79838(19) 0.55255(15) 0.0360(5) Uani 1 1 d . . .
H16 H 0.4642 0.8757 0.5960 0.043 Uiso 1 1 calc R . .
C21 C 0.45095(18) 0.68845(16) 0.80793(13) 0.0230(4) Uani 1 1 d . . .
C22 C 0.4372(2) 0.57040(18) 0.82181(19) 0.0445(6) Uani 1 1 d . . .
H22 H 0.5163 0.4982 0.7836 0.053 Uiso 1 1 calc R . .
C23 C 0.3086(3) 0.5574(2) 0.8912(2) 0.0552(7) Uani 1 1 d . . .
H23 H 0.2994 0.4764 0.9004 0.066 Uiso 1 1 calc R . .
C24 C 0.1941(2) 0.6618(2) 0.94674(17) 0.0435(5) Uani 1 1 d . . .
H24 H 0.1058 0.6527 0.9941 0.052 Uiso 1 1 calc R . .
C25 C 0.2069(2) 0.7791(2) 0.93415(15) 0.0372(5) Uani 1 1 d . . .
H25 H 0.1278 0.8508 0.9734 0.045 Uiso 1 1 calc R . .
C26 C 0.3349(2) 0.79298(17) 0.86428(14) 0.0295(4) Uani 1 1 d . . .
H26 H 0.3430 0.8744 0.8550 0.035 Uiso 1 1 calc R . .
C31 C 0.65443(19) 1.06476(15) 0.75644(15) 0.0260(4) Uani 1 1 d . . .
C32 C 0.7604(2) 1.09585(18) 0.67309(16) 0.0330(4) Uani 1 1 d . . .
H32 H 0.8103 1.0441 0.6074 0.040 Uiso 1 1 calc R . .
C33 C 0.7928(2) 1.2021(2) 0.6863(2) 0.0450(5) Uani 1 1 d . . .
H33 H 0.8634 1.2246 0.6290 0.054 Uiso 1 1 calc R . .
C34 C 0.7231(3) 1.27538(19) 0.7820(2) 0.0497(6) Uani 1 1 d . . .
H34 H 0.7473 1.3475 0.7910 0.060 Uiso 1 1 calc R . .
C35 C 0.6182(3) 1.24514(19) 0.8654(2) 0.0458(6) Uani 1 1 d . . .
H35 H 0.5705 1.2963 0.9314 0.055 Uiso 1 1 calc R . .
C36 C 0.5821(2) 1.13985(17) 0.85273(16) 0.0352(5) Uani 1 1 d . . .
H36 H 0.5088 1.1195 0.9094 0.042 Uiso 1 1 calc R . .
C41 C 0.99458(17) 0.44942(15) 0.72019(13) 0.0203(3) Uani 1 1 d . . .
F42 F 1.01372(12) 0.49596(10) 0.88382(8) 0.0346(3) Uani 1 1 d . . .
C42 C 1.05309(19) 0.41358(16) 0.79892(14) 0.0252(4) Uani 1 1 d . . .
F43 F 1.20016(14) 0.26684(12) 0.87726(10) 0.0517(3) Uani 1 1 d . . .
C43 C 1.1478(2) 0.29530(18) 0.79811(16) 0.0329(4) Uani 1 1 d . . .
F44 F 1.28117(13) 0.09133(10) 0.71320(11) 0.0532(4) Uani 1 1 d . . .
C44 C 1.1891(2) 0.20657(17) 0.71518(17) 0.0343(5) Uani 1 1 d . . .
F45 F 1.17716(13) 0.15164(10) 0.55176(10) 0.0447(3) Uani 1 1 d . . .
C45 C 1.1368(2) 0.23745(16) 0.63368(15) 0.0305(4) Uani 1 1 d . . .
C46 C 1.04217(18) 0.35685(16) 0.63737(13) 0.0234(4) Uani 1 1 d . . .
F46 F 0.99585(12) 0.38179(9) 0.55518(8) 0.0319(3) Uani 1 1 d . . .
C51 C 0.91063(18) 0.70304(15) 0.76132(13) 0.0211(3) Uani 1 1 d . . .
F52 F 0.72389(12) 0.73786(10) 0.93117(8) 0.0378(3) Uani 1 1 d . . .
C52 C 0.83234(19) 0.77147(16) 0.85988(13) 0.0244(4) Uani 1 1 d . . .
F53 F 0.77768(14) 0.93918(10) 0.98603(9) 0.0451(3) Uani 1 1 d . . .
C53 C 0.8579(2) 0.87486(16) 0.88933(14) 0.0287(4) Uani 1 1 d . . .
F54 F 0.99019(14) 1.01575(10) 0.84449(10) 0.0464(3) Uani 1 1 d . . .
C54 C 0.9649(2) 0.91391(16) 0.81801(15) 0.0301(4) Uani 1 1 d . . .
C55 C 1.0455(2) 0.84949(17) 0.71889(15) 0.0316(4) Uani 1 1 d . . .
F55 F 1.14815(14) 0.88911(12) 0.64818(10) 0.0551(4) Uani 1 1 d . . .
F56 F 1.09997(12) 0.68479(10) 0.59476(8) 0.0399(3) Uani 1 1 d . . .
C56 C 1.01788(19) 0.74562(16) 0.69314(14) 0.0259(4) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0180(2) 0.0183(2) 0.0260(2) 0.00011(17) -0.00827(17) -0.00624(17)
N1 0.0210(7) 0.0188(7) 0.0285(8) -0.0006(6) -0.0095(6) -0.0063(6)
C1 0.0226(9) 0.0219(9) 0.0305(9) 0.0047(7) -0.0118(7) -0.0057(7)
C2 0.0219(9) 0.0239(9) 0.0317(10) 0.0042(7) -0.0109(7) -0.0068(7)
B1 0.0218(10) 0.0215(9) 0.0166(9) 0.0016(7) -0.0051(7) -0.0086(8)
C11 0.0166(8) 0.0315(10) 0.0248(9) 0.0013(7) -0.0064(7) -0.0099(7)
C12 0.0250(9) 0.0326(10) 0.0294(9) -0.0001(8) -0.0071(8) -0.0134(8)
C13 0.0321(11) 0.0477(12) 0.0303(10) -0.0056(9) -0.0057(8) -0.0207(10)
C14 0.0330(11) 0.0708(15) 0.0284(10) 0.0010(10) -0.0151(9) -0.0199(11)
C15 0.0340(12) 0.0624(15) 0.0399(12) 0.0053(11) -0.0204(10) -0.0027(11)
C16 0.0278(10) 0.0399(11) 0.0335(10) -0.0011(9) -0.0134(8) 0.0004(9)
C21 0.0204(9) 0.0245(9) 0.0250(9) 0.0020(7) -0.0096(7) -0.0074(7)
C22 0.0281(11) 0.0240(10) 0.0667(15) 0.0022(10) -0.0010(10) -0.0077(9)
C23 0.0408(13) 0.0384(12) 0.0790(18) 0.0145(12) -0.0065(12) -0.0222(11)
C24 0.0283(11) 0.0586(14) 0.0397(12) 0.0069(10) -0.0031(9) -0.0200(11)
C25 0.0259(10) 0.0442(12) 0.0332(10) -0.0085(9) -0.0022(8) -0.0092(9)
C26 0.0267(10) 0.0258(9) 0.0325(10) -0.0049(8) -0.0074(8) -0.0074(8)
C31 0.0256(9) 0.0184(8) 0.0396(10) 0.0094(7) -0.0184(8) -0.0080(7)
C32 0.0285(10) 0.0342(11) 0.0439(11) 0.0121(9) -0.0190(9) -0.0144(9)
C33 0.0395(12) 0.0426(12) 0.0688(16) 0.0226(12) -0.0278(11) -0.0271(11)
C34 0.0513(14) 0.0275(11) 0.0902(19) 0.0132(12) -0.0412(14) -0.0223(11)
C35 0.0521(14) 0.0261(10) 0.0639(15) -0.0045(10) -0.0295(12) -0.0088(10)
C36 0.0389(11) 0.0241(10) 0.0435(12) 0.0037(8) -0.0159(9) -0.0109(9)
C41 0.0164(8) 0.0202(8) 0.0234(8) 0.0032(7) -0.0049(7) -0.0078(7)
F42 0.0413(7) 0.0356(6) 0.0286(6) 0.0007(5) -0.0183(5) -0.0083(5)
C42 0.0227(9) 0.0249(9) 0.0265(9) 0.0022(7) -0.0076(7) -0.0075(7)
F43 0.0535(8) 0.0499(8) 0.0553(8) 0.0184(6) -0.0359(7) -0.0051(6)
C43 0.0283(10) 0.0341(10) 0.0379(11) 0.0133(9) -0.0161(8) -0.0088(8)
F44 0.0397(7) 0.0267(6) 0.0772(9) 0.0082(6) -0.0180(7) 0.0054(5)
C44 0.0239(10) 0.0204(9) 0.0498(12) 0.0079(8) -0.0090(9) -0.0017(8)
F45 0.0416(7) 0.0269(6) 0.0523(7) -0.0149(5) -0.0046(6) -0.0067(5)
C45 0.0237(9) 0.0213(9) 0.0388(11) -0.0052(8) -0.0012(8) -0.0081(8)
C46 0.0207(9) 0.0239(9) 0.0264(9) 0.0030(7) -0.0062(7) -0.0112(7)
F46 0.0383(6) 0.0311(6) 0.0290(5) -0.0022(4) -0.0146(5) -0.0118(5)
C51 0.0198(8) 0.0198(8) 0.0255(9) 0.0014(7) -0.0118(7) -0.0047(7)
F52 0.0409(7) 0.0384(6) 0.0273(6) -0.0024(5) 0.0002(5) -0.0180(5)
C52 0.0245(9) 0.0234(9) 0.0257(9) 0.0035(7) -0.0105(7) -0.0072(7)
F53 0.0643(8) 0.0321(6) 0.0303(6) -0.0102(5) -0.0105(6) -0.0114(6)
C53 0.0354(11) 0.0219(9) 0.0268(9) -0.0043(7) -0.0154(8) -0.0019(8)
F54 0.0582(8) 0.0313(6) 0.0591(8) -0.0070(5) -0.0241(6) -0.0227(6)
C54 0.0368(11) 0.0194(9) 0.0418(11) -0.0023(8) -0.0220(9) -0.0102(8)
C55 0.0269(10) 0.0312(10) 0.0392(11) 0.0015(8) -0.0097(8) -0.0152(8)
F55 0.0479(8) 0.0543(8) 0.0612(8) -0.0075(6) 0.0021(6) -0.0380(7)
F56 0.0365(7) 0.0424(7) 0.0331(6) -0.0121(5) 0.0031(5) -0.0193(5)
C56 0.0225(9) 0.0255(9) 0.0279(9) -0.0046(7) -0.0076(7) -0.0066(7)
_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 1.5754(15) . ?
P1 C2 1.7504(18) . ?
P1 C21 1.7948(17) . ?
P1 C11 1.7976(18) . ?
N1 B1 1.372(2) . ?
C1 C2 1.198(2) . ?
C1 C31 1.434(2) . ?
B1 C41 1.597(2) . ?
B1 C51 1.607(2) . ?
C11 C12 1.387(2) . ?
C11 C16 1.393(3) . ?
C12 C13 1.388(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.380(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.383(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.379(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C26 1.385(2) . ?
C21 C22 1.386(3) . ?
C22 C23 1.383(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.374(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.372(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.385(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C36 1.388(3) . ?
C31 C32 1.392(3) . ?
C32 C33 1.380(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.372(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.381(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.390(3) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C42 1.387(2) . ?
C41 C46 1.388(2) . ?
F42 C42 1.352(2) . ?
C42 C43 1.379(3) . ?
F43 C43 1.344(2) . ?
C43 C44 1.373(3) . ?
F44 C44 1.340(2) . ?
C44 C45 1.375(3) . ?
F45 C45 1.344(2) . ?
C45 C46 1.381(3) . ?
C46 F46 1.342(2) . ?
C51 C56 1.380(2) . ?
C51 C52 1.381(2) . ?
F52 C52 1.348(2) . ?
C52 C53 1.378(2) . ?
F53 C53 1.346(2) . ?
C53 C54 1.372(3) . ?
F54 C54 1.3456(19) . ?
C54 C55 1.371(3) . ?
C55 F55 1.342(2) . ?
C55 C56 1.377(2) . ?
F56 C56 1.3511(19) . ?
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 C2 117.90(8) . . ?
N1 P1 C21 111.37(8) . . ?
C2 P1 C21 105.15(8) . . ?
N1 P1 C11 111.04(8) . . ?
C2 P1 C11 104.87(8) . . ?
C21 P1 C11 105.57(8) . . ?
B1 N1 P1 135.45(12) . . ?
C2 C1 C31 177.17(19) . . ?
C1 C2 P1 168.98(16) . . ?
N1 B1 C41 118.88(15) . . ?
N1 B1 C51 124.56(15) . . ?
C41 B1 C51 116.53(14) . . ?
C12 C11 C16 120.35(17) . . ?
C12 C11 P1 120.10(14) . . ?
C16 C11 P1 119.42(13) . . ?
C11 C12 C13 119.28(18) . . ?
C11 C12 H12 120.4 . . ?
C13 C12 H12 120.4 . . ?
C14 C13 C12 120.28(18) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C13 C14 C15 120.23(18) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C16 C15 C14 120.1(2) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C15 C16 C11 119.72(19) . . ?
C15 C16 H16 120.1 . . ?
C11 C16 H16 120.1 . . ?
C26 C21 C22 119.32(17) . . ?
C26 C21 P1 122.40(13) . . ?
C22 C21 P1 118.09(14) . . ?
C23 C22 C21 120.18(19) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C24 C23 C22 120.0(2) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C25 C24 C23 120.31(19) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C24 C25 C26 120.05(18) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C25 C26 C21 120.12(17) . . ?
C25 C26 H26 119.9 . . ?
C21 C26 H26 119.9 . . ?
C36 C31 C32 120.16(17) . . ?
C36 C31 C1 120.80(16) . . ?
C32 C31 C1 119.01(17) . . ?
C33 C32 C31 119.7(2) . . ?
C33 C32 H32 120.1 . . ?
C31 C32 H32 120.1 . . ?
C34 C33 C32 120.2(2) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C33 C34 C35 120.53(19) . . ?
C33 C34 H34 119.7 . . ?
C35 C34 H34 119.7 . . ?
C34 C35 C36 120.0(2) . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C31 C36 C35 119.31(19) . . ?
C31 C36 H36 120.3 . . ?
C35 C36 H36 120.3 . . ?
C42 C41 C46 114.45(15) . . ?
C42 C41 B1 122.04(15) . . ?
C46 C41 B1 123.46(15) . . ?
F42 C42 C43 116.71(16) . . ?
F42 C42 C41 119.57(15) . . ?
C43 C42 C41 123.68(17) . . ?
F43 C43 C44 120.07(17) . . ?
F43 C43 C42 120.54(18) . . ?
C44 C43 C42 119.39(18) . . ?
F44 C44 C43 120.08(19) . . ?
F44 C44 C45 120.37(18) . . ?
C43 C44 C45 119.55(16) . . ?
F45 C45 C44 120.08(16) . . ?
F45 C45 C46 120.58(18) . . ?
C44 C45 C46 119.34(17) . . ?
F46 C46 C45 116.63(15) . . ?
F46 C46 C41 119.80(15) . . ?
C45 C46 C41 123.57(17) . . ?
C56 C51 C52 115.06(15) . . ?
C56 C51 B1 122.82(14) . . ?
C52 C51 B1 122.11(15) . . ?
F52 C52 C53 117.57(15) . . ?
F52 C52 C51 119.23(15) . . ?
C53 C52 C51 123.20(16) . . ?
F53 C53 C54 119.69(15) . . ?
F53 C53 C52 120.98(17) . . ?
C54 C53 C52 119.32(16) . . ?
F54 C54 C55 119.88(17) . . ?
F54 C54 C53 120.32(16) . . ?
C55 C54 C53 119.79(15) . . ?
F55 C55 C54 119.88(16) . . ?
F55 C55 C56 121.05(17) . . ?
C54 C55 C56 119.06(17) . . ?
F56 C56 C55 117.12(15) . . ?
F56 C56 C51 119.32(14) . . ?
C55 C56 C51 123.54(16) . . ?
_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.048


data_compound_3
_database_code_depnum_ccdc_archive 'CCDC 929295'
#TrackingRef 'cif_revised.txt'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H18 B F10 N4 P'
_chemical_formula_sum            'C33 H18 B F10 N4 P'
_chemical_formula_weight         702.29
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'
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'
F F 0.0171 0.0103 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   Cc
_symmetry_space_group_name_Hall  'C -2yc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
_cell_length_a                   17.9949(12)
_cell_length_b                   14.7759(10)
_cell_length_c                   14.0239(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 122.870(2)
_cell_angle_gamma                90.00
_cell_volume                     3131.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9041
_cell_measurement_theta_min      2.76
_cell_measurement_theta_max      28.23
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1416
_exptl_absorpt_coefficient_mu    0.179
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9651
_exptl_absorpt_correction_T_max  0.9651
_exptl_absorpt_process_details   multi-scan
_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 CCd area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12649
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.93
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4755
_reflns_number_gt                4489
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
Structure solved using Superflip in Crystals. and refined in SHELXTL.
All non-H atoms located in the solution and non-H atoms added at calc
positions.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+2.0383P] where P=(Fo^2^+2Fc^2^)/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   -0.11(8)
_refine_ls_number_reflns         4755
_refine_ls_number_parameters     443
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0763
_refine_ls_wR_factor_gt          0.0743
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_restrained_S_all      0.946
_refine_ls_shift/su_max          0.003
_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 0.41569(4) 0.42088(3) 0.34240(4) 0.01716(13) Uani 1 1 d . . .
N4 N 0.35261(14) 0.50513(12) 0.27275(16) 0.0203(4) Uani 1 1 d . . .
H4 H 0.3446 0.5219 0.2076 0.024 Uiso 1 1 calc R . .
B1 B 0.30664(18) 0.55565(17) 0.3231(2) 0.0185(6) Uani 1 1 d . . .
C1 C 0.43666(16) 0.40526(15) 0.57168(17) 0.0185(5) Uani 1 1 d . . .
N1 N 0.38896(13) 0.45334(12) 0.60333(15) 0.0205(4) Uani 1 1 d . . .
C2 C 0.41237(15) 0.43753(14) 0.46582(18) 0.0167(5) Uani 1 1 d . . .
N2 N 0.33731(13) 0.51254(13) 0.52302(15) 0.0209(4) Uani 1 1 d . . .
N3 N 0.35143(12) 0.50385(12) 0.44048(15) 0.0171(4) Uani 1 1 d . . .
C11 C 0.33441(17) 0.66279(16) 0.3415(2) 0.0228(5) Uani 1 1 d . . .
C12 C 0.40982(18) 0.69716(17) 0.4375(2) 0.0314(6) Uani 1 1 d . . .
F12 F 0.46613(11) 0.64199(10) 0.52417(13) 0.0446(4) Uani 1 1 d . . .
C13 C 0.4344(2) 0.78757(19) 0.4525(3) 0.0455(8) Uani 1 1 d . . .
F13 F 0.50877(14) 0.81473(12) 0.54746(19) 0.0751(7) Uani 1 1 d . . .
C14 C 0.3830(3) 0.84777(19) 0.3682(3) 0.0537(9) Uani 1 1 d . . .
F14 F 0.40664(18) 0.93571(11) 0.3811(2) 0.0890(8) Uani 1 1 d . . .
C15 C 0.3088(2) 0.81854(19) 0.2713(3) 0.0459(8) Uani 1 1 d . . .
F15 F 0.25821(15) 0.87739(12) 0.1874(2) 0.0746(7) Uani 1 1 d . . .
C16 C 0.28679(19) 0.72748(17) 0.2595(2) 0.0328(6) Uani 1 1 d . . .
F16 F 0.21258(12) 0.70256(11) 0.16001(14) 0.0496(5) Uani 1 1 d . . .
C21 C 0.19991(16) 0.54128(16) 0.26133(18) 0.0226(5) Uani 1 1 d . . .
C22 C 0.15478(17) 0.58455(17) 0.3031(2) 0.0275(6) Uani 1 1 d . . .
F22 F 0.19726(10) 0.64730(10) 0.38691(12) 0.0347(4) Uani 1 1 d . . .
C23 C 0.0676(2) 0.5695(2) 0.2650(3) 0.0408(7) Uani 1 1 d . . .
F23 F 0.02934(12) 0.61480(16) 0.31017(18) 0.0681(6) Uani 1 1 d . . .
C24 C 0.02023(18) 0.5078(2) 0.1794(3) 0.0463(8) Uani 1 1 d . . .
F24 F -0.06531(12) 0.49235(16) 0.1396(2) 0.0780(7) Uani 1 1 d . . .
C25 C 0.0601(2) 0.46440(19) 0.1326(2) 0.0412(8) Uani 1 1 d . . .
F25 F 0.01368(12) 0.40557(12) 0.04721(16) 0.0626(6) Uani 1 1 d . . .
C26 C 0.14761(18) 0.48184(17) 0.1728(2) 0.0303(6) Uani 1 1 d . . .
F26 F 0.18136(11) 0.43634(11) 0.12165(13) 0.0485(5) Uani 1 1 d . . .
C31 C 0.52244(17) 0.43232(15) 0.36244(18) 0.0223(5) Uani 1 1 d . . .
C32 C 0.55188(19) 0.3694(2) 0.3166(2) 0.0355(7) Uani 1 1 d . . .
H32 H 0.5188 0.3159 0.2820 0.043 Uiso 1 1 calc R . .
C33 C 0.6298(2) 0.3852(2) 0.3217(3) 0.0478(8) Uani 1 1 d . . .
H33 H 0.6496 0.3431 0.2890 0.057 Uiso 1 1 calc R . .
C34 C 0.6786(2) 0.4619(2) 0.3741(3) 0.0434(7) Uani 1 1 d . . .
H34 H 0.7321 0.4723 0.3777 0.052 Uiso 1 1 calc R . .
C35 C 0.6504(2) 0.5236(2) 0.4215(3) 0.0458(8) Uani 1 1 d . . .
H35 H 0.6847 0.5762 0.4581 0.055 Uiso 1 1 calc R . .
C36 C 0.57245(18) 0.50907(18) 0.4157(2) 0.0339(6) Uani 1 1 d . . .
H36 H 0.5529 0.5517 0.4482 0.041 Uiso 1 1 calc R . .
C41 C 0.37350(15) 0.31095(15) 0.28331(19) 0.0190(5) Uani 1 1 d . . .
C42 C 0.32488(18) 0.30130(16) 0.16539(19) 0.0270(6) Uani 1 1 d . . .
H42 H 0.3136 0.3523 0.1181 0.032 Uiso 1 1 calc R . .
C43 C 0.29325(18) 0.21655(17) 0.1181(2) 0.0330(6) Uani 1 1 d . . .
H43 H 0.2602 0.2094 0.0379 0.040 Uiso 1 1 calc R . .
C44 C 0.30939(18) 0.14257(17) 0.1866(2) 0.0332(6) Uani 1 1 d . . .
H44 H 0.2879 0.0847 0.1534 0.040 Uiso 1 1 calc R . .
C45 C 0.35678(17) 0.15219(17) 0.3034(2) 0.0312(6) Uani 1 1 d . . .
H45 H 0.3667 0.1012 0.3501 0.037 Uiso 1 1 calc R . .
C46 C 0.38982(17) 0.23627(15) 0.3522(2) 0.0242(5) Uani 1 1 d . . .
H46 H 0.4235 0.2427 0.4324 0.029 Uiso 1 1 calc R . .
C51 C 0.50198(16) 0.33848(15) 0.64958(18) 0.0198(5) Uani 1 1 d . . .
C52 C 0.49158(19) 0.29788(18) 0.7311(2) 0.0320(6) Uani 1 1 d . . .
H52 H 0.4393 0.3084 0.7305 0.038 Uiso 1 1 calc R . .
C53 C 0.5573(2) 0.2420(2) 0.8133(2) 0.0387(7) Uani 1 1 d . . .
H53 H 0.5498 0.2157 0.8693 0.046 Uiso 1 1 calc R . .
C54 C 0.63327(17) 0.22403(17) 0.8154(2) 0.0278(6) Uani 1 1 d . . .
C55 C 0.64097(17) 0.26151(18) 0.7311(2) 0.0294(6) Uani 1 1 d . . .
H55 H 0.6917 0.2479 0.7291 0.035 Uiso 1 1 calc R . .
C56 C 0.57705(17) 0.31815(17) 0.6497(2) 0.0278(6) Uani 1 1 d . . .
H56 H 0.5847 0.3434 0.5933 0.033 Uiso 1 1 calc R . .
C57 C 0.7054(2) 0.1666(2) 0.9083(2) 0.0427(7) Uani 1 1 d . . .
H57A H 0.6790 0.1154 0.9240 0.064 Uiso 1 1 calc R . .
H57B H 0.7404 0.2032 0.9772 0.064 Uiso 1 1 calc R . .
H57C H 0.7439 0.1440 0.8842 0.064 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0230(3) 0.0169(3) 0.0163(2) -0.0004(2) 0.0137(2) 0.0007(3)
N4 0.0308(12) 0.0180(9) 0.0177(9) 0.0018(7) 0.0168(9) 0.0037(8)
B1 0.0249(16) 0.0172(12) 0.0159(12) 0.0003(10) 0.0127(12) 0.0018(11)
C1 0.0208(13) 0.0205(11) 0.0163(10) -0.0030(9) 0.0113(10) -0.0007(10)
N1 0.0237(11) 0.0245(10) 0.0151(9) -0.0007(8) 0.0117(9) 0.0016(9)
C2 0.0172(13) 0.0176(11) 0.0181(11) -0.0002(8) 0.0114(10) 0.0010(9)
N2 0.0261(12) 0.0227(10) 0.0174(9) -0.0017(8) 0.0142(9) 0.0018(8)
N3 0.0199(11) 0.0195(9) 0.0143(8) -0.0012(7) 0.0109(8) 0.0014(8)
C11 0.0282(14) 0.0191(11) 0.0308(12) -0.0008(10) 0.0224(12) 0.0036(10)
C12 0.0344(17) 0.0237(13) 0.0400(14) -0.0062(11) 0.0226(14) -0.0028(11)
F12 0.0408(10) 0.0368(9) 0.0339(8) -0.0025(7) 0.0058(8) -0.0091(7)
C13 0.049(2) 0.0278(15) 0.0637(19) -0.0135(14) 0.0329(17) -0.0083(14)
F13 0.0707(15) 0.0455(11) 0.0821(14) -0.0294(10) 0.0240(12) -0.0303(10)
C14 0.067(2) 0.0153(13) 0.091(3) -0.0038(15) 0.052(2) -0.0029(14)
F14 0.1060(19) 0.0186(8) 0.148(2) -0.0023(11) 0.0729(18) -0.0098(10)
C15 0.055(2) 0.0271(14) 0.072(2) 0.0196(14) 0.045(2) 0.0138(14)
F15 0.0797(15) 0.0408(11) 0.1031(16) 0.0393(11) 0.0496(13) 0.0199(10)
C16 0.0373(17) 0.0291(13) 0.0394(15) 0.0083(11) 0.0255(14) 0.0056(12)
F16 0.0489(11) 0.0481(10) 0.0393(9) 0.0231(8) 0.0157(9) 0.0066(8)
C21 0.0238(14) 0.0222(12) 0.0176(11) 0.0051(9) 0.0086(10) 0.0036(10)
C22 0.0260(15) 0.0297(13) 0.0239(12) -0.0002(10) 0.0115(11) 0.0024(11)
F22 0.0326(9) 0.0404(8) 0.0334(8) -0.0107(6) 0.0194(7) 0.0032(7)
C23 0.0309(18) 0.0461(17) 0.0482(17) 0.0020(14) 0.0233(15) 0.0074(14)
F23 0.0377(11) 0.0928(16) 0.0844(15) -0.0192(12) 0.0401(11) 0.0051(10)
C24 0.0165(17) 0.0501(18) 0.0568(19) 0.0020(15) 0.0098(15) -0.0022(13)
F24 0.0247(11) 0.0869(15) 0.1013(17) -0.0143(13) 0.0205(11) -0.0099(10)
C25 0.0289(18) 0.0314(15) 0.0378(15) -0.0004(12) 0.0015(13) -0.0026(13)
F25 0.0378(11) 0.0480(10) 0.0562(11) -0.0191(9) -0.0043(9) -0.0052(8)
C26 0.0298(17) 0.0275(13) 0.0248(12) -0.0009(10) 0.0091(12) 0.0067(11)
F26 0.0399(10) 0.0524(10) 0.0388(9) -0.0255(8) 0.0120(8) 0.0028(8)
C31 0.0266(15) 0.0239(12) 0.0190(11) 0.0045(9) 0.0141(11) 0.0026(11)
C32 0.0347(17) 0.0405(16) 0.0414(15) -0.0075(12) 0.0273(14) -0.0008(13)
C33 0.040(2) 0.059(2) 0.064(2) -0.0091(16) 0.0407(17) 0.0011(16)
C34 0.0275(17) 0.0598(19) 0.0515(17) 0.0116(15) 0.0270(15) 0.0023(15)
C35 0.0341(19) 0.0442(17) 0.0558(18) -0.0038(15) 0.0223(16) -0.0113(14)
C36 0.0301(16) 0.0329(14) 0.0427(15) -0.0073(12) 0.0224(14) -0.0037(12)
C41 0.0175(13) 0.0191(11) 0.0237(11) -0.0024(9) 0.0133(11) 0.0019(9)
C42 0.0383(16) 0.0244(12) 0.0231(12) -0.0010(10) 0.0197(12) -0.0006(11)
C43 0.0396(17) 0.0322(14) 0.0240(12) -0.0098(11) 0.0151(12) -0.0046(12)
C44 0.0331(16) 0.0223(12) 0.0386(14) -0.0105(11) 0.0158(13) -0.0024(11)
C45 0.0338(16) 0.0201(12) 0.0333(14) 0.0034(10) 0.0140(13) 0.0001(11)
C46 0.0253(14) 0.0220(12) 0.0223(11) 0.0012(9) 0.0109(10) 0.0024(10)
C51 0.0216(13) 0.0214(11) 0.0169(10) -0.0004(9) 0.0107(10) 0.0030(10)
C52 0.0331(16) 0.0390(15) 0.0338(13) 0.0161(12) 0.0244(12) 0.0148(12)
C53 0.0497(19) 0.0451(17) 0.0318(14) 0.0185(12) 0.0288(14) 0.0166(14)
C54 0.0248(15) 0.0289(13) 0.0251(12) 0.0014(10) 0.0104(11) 0.0066(11)
C55 0.0199(14) 0.0384(14) 0.0312(13) 0.0037(11) 0.0147(11) 0.0046(12)
C56 0.0281(15) 0.0337(14) 0.0268(13) 0.0044(10) 0.0183(12) 0.0028(11)
C57 0.0462(19) 0.0464(17) 0.0320(15) 0.0106(13) 0.0189(14) 0.0183(15)
_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 N4 1.6090(19) . ?
P1 C2 1.781(2) . ?
P1 C31 1.792(3) . ?
P1 C41 1.794(2) . ?
N4 B1 1.540(3) . ?
N4 H4 0.8800 . ?
B1 N3 1.583(3) . ?
B1 C21 1.637(4) . ?
B1 C11 1.638(3) . ?
C1 N1 1.361(3) . ?
C1 C2 1.385(3) . ?
C1 C51 1.468(3) . ?
N1 N2 1.327(3) . ?
C2 N3 1.366(3) . ?
N2 N3 1.319(3) . ?
C11 C16 1.378(3) . ?
C11 C12 1.389(4) . ?
C12 F12 1.354(3) . ?
C12 C13 1.387(4) . ?
C13 F13 1.338(4) . ?
C13 C14 1.364(5) . ?
C14 F14 1.349(3) . ?
C14 C15 1.358(5) . ?
C15 F15 1.345(3) . ?
C15 C16 1.387(4) . ?
C16 F16 1.358(3) . ?
C21 C22 1.389(4) . ?
C21 C26 1.389(3) . ?
C22 F22 1.360(3) . ?
C22 C23 1.373(4) . ?
C23 F23 1.341(4) . ?
C23 C24 1.375(4) . ?
C24 F24 1.342(3) . ?
C24 C25 1.365(5) . ?
C25 F25 1.343(3) . ?
C25 C26 1.379(4) . ?
C26 F26 1.345(3) . ?
C31 C32 1.388(4) . ?
C31 C36 1.387(3) . ?
C32 C33 1.385(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.377(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.376(5) . ?
C34 H34 0.9500 . ?
C35 C36 1.378(4) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C46 1.389(3) . ?
C41 C42 1.396(3) . ?
C42 C43 1.386(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.378(4) . ?
C43 H43 0.9500 . ?
C44 C45 1.384(4) . ?
C44 H44 0.9500 . ?
C45 C46 1.387(3) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C51 C56 1.383(4) . ?
C51 C52 1.390(3) . ?
C52 C53 1.389(4) . ?
C52 H52 0.9500 . ?
C53 C54 1.376(4) . ?
C53 H53 0.9500 . ?
C54 C55 1.379(4) . ?
C54 C57 1.506(4) . ?
C55 C56 1.379(3) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 P1 C2 95.65(10) . . ?
N4 P1 C31 111.41(11) . . ?
C2 P1 C31 115.66(11) . . ?
N4 P1 C41 115.97(10) . . ?
C2 P1 C41 110.18(10) . . ?
C31 P1 C41 107.86(11) . . ?
B1 N4 P1 118.30(15) . . ?
B1 N4 H4 120.8 . . ?
P1 N4 H4 120.8 . . ?
N4 B1 N3 98.36(17) . . ?
N4 B1 C21 117.56(19) . . ?
N3 B1 C21 106.04(18) . . ?
N4 B1 C11 110.3(2) . . ?
N3 B1 C11 111.34(18) . . ?
C21 B1 C11 112.26(19) . . ?
N1 C1 C2 106.38(19) . . ?
N1 C1 C51 120.01(18) . . ?
C2 C1 C51 133.5(2) . . ?
N2 N1 C1 110.02(17) . . ?
N3 C2 C1 105.52(19) . . ?
N3 C2 P1 106.98(15) . . ?
C1 C2 P1 146.79(18) . . ?
N3 N2 N1 107.50(17) . . ?
N2 N3 C2 110.57(17) . . ?
N2 N3 B1 129.33(18) . . ?
C2 N3 B1 120.06(18) . . ?
C16 C11 C12 113.1(2) . . ?
C16 C11 B1 122.7(2) . . ?
C12 C11 B1 124.1(2) . . ?
F12 C12 C11 120.8(2) . . ?
F12 C12 C13 114.9(2) . . ?
C11 C12 C13 124.3(3) . . ?
F13 C13 C14 120.6(3) . . ?
F13 C13 C12 120.3(3) . . ?
C14 C13 C12 119.0(3) . . ?
F14 C14 C15 120.5(3) . . ?
F14 C14 C13 119.7(3) . . ?
C15 C14 C13 119.8(3) . . ?
F15 C15 C14 120.1(3) . . ?
F15 C15 C16 120.6(3) . . ?
C14 C15 C16 119.3(3) . . ?
F16 C16 C11 119.2(2) . . ?
F16 C16 C15 116.4(2) . . ?
C11 C16 C15 124.4(3) . . ?
C22 C21 C26 113.6(2) . . ?
C22 C21 B1 120.3(2) . . ?
C26 C21 B1 125.9(2) . . ?
F22 C22 C23 115.7(2) . . ?
F22 C22 C21 119.7(2) . . ?
C23 C22 C21 124.6(2) . . ?
F23 C23 C22 120.4(3) . . ?
F23 C23 C24 120.6(3) . . ?
C22 C23 C24 118.9(3) . . ?
F24 C24 C25 120.2(3) . . ?
F24 C24 C23 120.2(3) . . ?
C25 C24 C23 119.5(3) . . ?
F25 C25 C24 119.9(3) . . ?
F25 C25 C26 120.3(3) . . ?
C24 C25 C26 119.8(3) . . ?
F26 C26 C25 115.8(2) . . ?
F26 C26 C21 120.6(2) . . ?
C25 C26 C21 123.6(2) . . ?
C32 C31 C36 119.8(2) . . ?
C32 C31 P1 120.67(19) . . ?
C36 C31 P1 119.25(19) . . ?
C33 C32 C31 119.6(3) . . ?
C33 C32 H32 120.2 . . ?
C31 C32 H32 120.2 . . ?
C34 C33 C32 120.0(3) . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C33 C34 C35 120.6(3) . . ?
C33 C34 H34 119.7 . . ?
C35 C34 H34 119.7 . . ?
C34 C35 C36 119.9(3) . . ?
C34 C35 H35 120.1 . . ?
C36 C35 H35 120.1 . . ?
C35 C36 C31 120.1(3) . . ?
C35 C36 H36 119.9 . . ?
C31 C36 H36 119.9 . . ?
C46 C41 C42 120.1(2) . . ?
C46 C41 P1 121.44(17) . . ?
C42 C41 P1 118.40(18) . . ?
C43 C42 C41 119.3(2) . . ?
C43 C42 H42 120.3 . . ?
C41 C42 H42 120.3 . . ?
C44 C43 C42 120.4(2) . . ?
C44 C43 H43 119.8 . . ?
C42 C43 H43 119.8 . . ?
C43 C44 C45 120.3(2) . . ?
C43 C44 H44 119.8 . . ?
C45 C44 H44 119.8 . . ?
C44 C45 C46 120.0(2) . . ?
C44 C45 H45 120.0 . . ?
C46 C45 H45 120.0 . . ?
C45 C46 C41 119.8(2) . . ?
C45 C46 H46 120.1 . . ?
C41 C46 H46 120.1 . . ?
C56 C51 C52 118.2(2) . . ?
C56 C51 C1 122.3(2) . . ?
C52 C51 C1 119.4(2) . . ?
C53 C52 C51 120.3(2) . . ?
C53 C52 H52 119.9 . . ?
C51 C52 H52 119.9 . . ?
C54 C53 C52 121.4(2) . . ?
C54 C53 H53 119.3 . . ?
C52 C53 H53 119.3 . . ?
C53 C54 C55 117.7(2) . . ?
C53 C54 C57 120.5(2) . . ?
C55 C54 C57 121.8(3) . . ?
C56 C55 C54 121.8(2) . . ?
C56 C55 H55 119.1 . . ?
C54 C55 H55 119.1 . . ?
C51 C56 C55 120.6(2) . . ?
C51 C56 H56 119.7 . . ?
C55 C56 H56 119.7 . . ?
C54 C57 H57A 109.5 . . ?
C54 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C54 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max         0.202
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.038


data_d12277
_database_code_depnum_ccdc_archive 'CCDC 929332'
#TrackingRef 'd12277.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H20 B F10 N P2'
_chemical_formula_sum            'C38 H20 B F10 N P2'
_chemical_formula_weight         753.30
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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                   13.6525(11)
_cell_length_b                   9.9457(8)
_cell_length_c                   13.7064(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.177(5)
_cell_angle_gamma                90.00
_cell_volume                     1710.9(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    147(2)
_cell_measurement_reflns_used    7394
_cell_measurement_theta_min      3.51
_cell_measurement_theta_max      66.06
_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             760
_exptl_absorpt_coefficient_mu    1.915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4645
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      147(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Bruker ImuS'
_diffrn_radiation_monochromator  'multi-layer optics'
_diffrn_measurement_device_type  'Bruker Kappa APEX-DUO CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9612
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0660
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.51
_diffrn_reflns_theta_max         66.47
_reflns_number_total             3883
_reflns_number_gt                3478
_reflns_threshold_expression     I>2\s(I)
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       APEX2
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0787P)^2^] where P=(Fo^2^+2Fc^2^)/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   0.02(3)
_refine_ls_number_reflns         3883
_refine_ls_number_parameters     469
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0482
_refine_ls_wR_factor_ref         0.1246
_refine_ls_wR_factor_gt          0.1209
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_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
N1 N 0.2992(3) 0.1044(4) 0.3950(2) 0.0350(7) Uani 1 1 d . . .
P1 P -0.08696(8) -0.03537(10) 0.06152(8) 0.0358(3) Uani 1 1 d . . .
P2 P 0.27370(7) 0.03550(10) 0.28449(8) 0.0333(2) Uani 1 1 d . . .
F1 F 0.2977(2) -0.0020(3) 0.6586(2) 0.0580(7) Uani 1 1 d . . .
F2 F 0.4114(2) 0.1041(3) 0.85083(19) 0.0670(8) Uani 1 1 d . . .
F3 F 0.4765(2) 0.3654(3) 0.8676(2) 0.0621(8) Uani 1 1 d . . .
F4 F 0.4338(2) 0.5138(3) 0.6908(2) 0.0618(7) Uani 1 1 d . . .
F5 F 0.3286(2) 0.4061(3) 0.4986(2) 0.0594(7) Uani 1 1 d . . .
F6 F 0.08850(18) 0.3310(3) 0.45103(18) 0.0452(6) Uani 1 1 d . . .
F7 F -0.11905(19) 0.2880(4) 0.3984(2) 0.0639(8) Uani 1 1 d . . .
F8 F -0.20125(19) 0.0364(4) 0.3448(2) 0.0736(9) Uani 1 1 d . . .
F9 F -0.0720(2) -0.1720(3) 0.3436(2) 0.0655(8) Uani 1 1 d . . .
F10 F 0.1364(2) -0.1285(3) 0.3982(2) 0.0515(6) Uani 1 1 d . . .
C1 C 0.0469(3) 0.0050(4) 0.1416(3) 0.0350(9) Uani 1 1 d . . .
C2 C 0.1391(3) 0.0162(4) 0.1977(3) 0.0373(9) Uani 1 1 d . . .
C3 C -0.1553(3) 0.1094(5) 0.0891(3) 0.0393(9) Uani 1 1 d . . .
C4 C -0.2601(4) 0.0845(6) 0.0778(4) 0.0579(13) Uani 1 1 d . . .
H4A H -0.2899 -0.0029 0.0594 0.069 Uiso 1 1 calc R . .
C5 C -0.3201(4) 0.1878(8) 0.0936(5) 0.0811(19) Uani 1 1 d . . .
H5A H -0.3913 0.1710 0.0855 0.097 Uiso 1 1 calc R . .
C6 C -0.2780(4) 0.3137(7) 0.1206(5) 0.0745(17) Uani 1 1 d . . .
H6A H -0.3201 0.3842 0.1307 0.089 Uiso 1 1 calc R . .
C7 C -0.1743(4) 0.3382(6) 0.1330(4) 0.0632(14) Uani 1 1 d . . .
H7A H -0.1443 0.4252 0.1530 0.076 Uiso 1 1 calc R . .
C8 C -0.1142(4) 0.2365(5) 0.1163(4) 0.0491(11) Uani 1 1 d . . .
H8A H -0.0432 0.2544 0.1238 0.059 Uiso 1 1 calc R . .
C9 C -0.0876(3) 0.0035(4) -0.0692(3) 0.0345(9) Uani 1 1 d . . .
C10 C -0.0360(4) 0.1111(5) -0.0914(3) 0.0461(10) Uani 1 1 d . . .
H10A H 0.0053 0.1697 -0.0357 0.055 Uiso 1 1 calc R . .
C11 C -0.0437(4) 0.1350(5) -0.1940(4) 0.0545(12) Uani 1 1 d . . .
H11A H -0.0087 0.2102 -0.2087 0.065 Uiso 1 1 calc R . .
C12 C -0.1024(4) 0.0487(5) -0.2742(4) 0.0560(12) Uani 1 1 d . . .
H12A H -0.1077 0.0640 -0.3446 0.067 Uiso 1 1 calc R . .
C13 C -0.1532(4) -0.0589(6) -0.2532(4) 0.0533(12) Uani 1 1 d . . .
H13A H -0.1938 -0.1177 -0.3091 0.064 Uiso 1 1 calc R . .
C14 C -0.1463(3) -0.0832(5) -0.1515(3) 0.0431(10) Uani 1 1 d . . .
H14A H -0.1814 -0.1588 -0.1376 0.052 Uiso 1 1 calc R . .
C15 C 0.3286(3) 0.1340(4) 0.2085(3) 0.0365(9) Uani 1 1 d . . .
C16 C 0.4068(3) 0.2290(4) 0.2585(3) 0.0415(10) Uani 1 1 d . . .
H16A H 0.4301 0.2432 0.3328 0.050 Uiso 1 1 calc R . .
C17 C 0.4507(4) 0.3032(5) 0.2004(4) 0.0500(11) Uani 1 1 d . . .
H17A H 0.5051 0.3669 0.2352 0.060 Uiso 1 1 calc R . .
C18 C 0.4158(4) 0.2851(5) 0.0924(4) 0.0554(13) Uani 1 1 d . . .
H18A H 0.4461 0.3365 0.0529 0.066 Uiso 1 1 calc R . .
C19 C 0.3377(4) 0.1932(6) 0.0420(4) 0.0592(14) Uani 1 1 d . . .
H19A H 0.3136 0.1821 -0.0326 0.071 Uiso 1 1 calc R . .
C20 C 0.2932(3) 0.1160(5) 0.0983(3) 0.0451(10) Uani 1 1 d . . .
H20A H 0.2394 0.0518 0.0627 0.054 Uiso 1 1 calc R . .
C21 C 0.3273(3) -0.1334(4) 0.3024(3) 0.0338(8) Uani 1 1 d . . .
C22 C 0.3798(3) -0.1819(5) 0.4044(3) 0.0451(10) Uani 1 1 d . . .
H22A H 0.3893 -0.1262 0.4637 0.054 Uiso 1 1 calc R . .
C23 C 0.4183(4) -0.3115(5) 0.4192(4) 0.0525(11) Uani 1 1 d . . .
H23A H 0.4538 -0.3453 0.4892 0.063 Uiso 1 1 calc R . .
C24 C 0.4058(3) -0.3925(5) 0.3339(4) 0.0471(10) Uani 1 1 d . . .
H24A H 0.4327 -0.4817 0.3450 0.056 Uiso 1 1 calc R . .
C25 C 0.3542(4) -0.3440(5) 0.2322(4) 0.0467(11) Uani 1 1 d . . .
H25A H 0.3454 -0.4001 0.1733 0.056 Uiso 1 1 calc R . .
C26 C 0.3155(3) -0.2152(4) 0.2158(3) 0.0385(9) Uani 1 1 d . . .
H26A H 0.2808 -0.1816 0.1456 0.046 Uiso 1 1 calc R . .
C27 C 0.3076(3) 0.1994(4) 0.5710(3) 0.0349(9) Uani 1 1 d . . .
C28 C 0.3298(3) 0.1265(4) 0.6646(3) 0.0397(10) Uani 1 1 d . . .
C29 C 0.3873(4) 0.1815(5) 0.7635(3) 0.0431(10) Uani 1 1 d . . .
C30 C 0.4210(3) 0.3102(5) 0.7718(3) 0.0436(10) Uani 1 1 d . . .
C31 C 0.4004(3) 0.3871(5) 0.6812(3) 0.0432(10) Uani 1 1 d . . .
C32 C 0.3452(3) 0.3289(4) 0.5849(3) 0.0390(9) Uani 1 1 d . . .
C33 C 0.1203(3) 0.1035(4) 0.4261(3) 0.0370(9) Uani 1 1 d . . .
C34 C 0.0506(3) 0.2043(4) 0.4251(3) 0.0392(10) Uani 1 1 d . . .
C35 C -0.0568(3) 0.1857(5) 0.3979(3) 0.0479(12) Uani 1 1 d . . .
C36 C -0.0971(4) 0.0567(6) 0.3711(3) 0.0535(13) Uani 1 1 d . . .
C37 C -0.0316(4) -0.0462(6) 0.3709(3) 0.0508(12) Uani 1 1 d . . .
C38 C 0.0751(3) -0.0241(5) 0.3986(3) 0.0417(10) Uani 1 1 d . . .
B1 B 0.2435(4) 0.1314(4) 0.4571(4) 0.0343(9) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0330(18) 0.0493(17) 0.0218(16) -0.0066(14) 0.0099(14) -0.0031(15)
P1 0.0293(5) 0.0456(5) 0.0327(6) 0.0004(4) 0.0124(5) -0.0003(4)
P2 0.0284(5) 0.0471(5) 0.0260(5) -0.0017(4) 0.0125(4) 0.0017(4)
F1 0.0747(18) 0.0555(15) 0.0444(16) 0.0036(12) 0.0241(14) -0.0127(13)
F2 0.084(2) 0.0870(19) 0.0275(13) 0.0068(13) 0.0192(14) -0.0094(18)
F3 0.0561(17) 0.090(2) 0.0332(14) -0.0244(14) 0.0102(13) -0.0133(15)
F4 0.0536(16) 0.0561(15) 0.0629(18) -0.0068(14) 0.0092(14) -0.0155(13)
F5 0.0660(18) 0.0611(15) 0.0399(15) 0.0093(13) 0.0087(13) -0.0137(14)
F6 0.0426(14) 0.0545(14) 0.0436(14) -0.0002(11) 0.0224(12) 0.0009(11)
F7 0.0405(15) 0.096(2) 0.0599(18) -0.0009(16) 0.0249(14) 0.0134(15)
F8 0.0349(15) 0.128(3) 0.0608(18) -0.0083(19) 0.0220(13) -0.0194(18)
F9 0.0682(18) 0.0801(19) 0.0620(18) -0.0254(16) 0.0403(16) -0.0379(16)
F10 0.0610(17) 0.0505(13) 0.0534(16) -0.0074(12) 0.0335(14) -0.0062(12)
C1 0.034(2) 0.044(2) 0.030(2) -0.0002(16) 0.0149(19) -0.0005(16)
C2 0.036(2) 0.048(2) 0.032(2) -0.0019(17) 0.017(2) 0.0021(17)
C3 0.027(2) 0.064(2) 0.027(2) -0.0002(19) 0.0107(18) 0.0045(19)
C4 0.039(3) 0.076(3) 0.063(3) -0.018(3) 0.025(2) -0.006(2)
C5 0.046(3) 0.104(5) 0.100(5) -0.037(4) 0.035(3) 0.004(3)
C6 0.065(4) 0.091(4) 0.073(4) -0.013(3) 0.033(3) 0.030(3)
C7 0.075(4) 0.057(3) 0.063(3) -0.007(3) 0.033(3) 0.005(3)
C8 0.047(3) 0.052(2) 0.055(3) -0.002(2) 0.027(2) 0.000(2)
C9 0.027(2) 0.047(2) 0.026(2) -0.0032(16) 0.0067(17) 0.0057(16)
C10 0.056(3) 0.051(2) 0.031(2) -0.007(2) 0.017(2) -0.008(2)
C11 0.079(4) 0.052(2) 0.040(3) -0.005(2) 0.032(3) -0.007(2)
C12 0.072(3) 0.063(3) 0.034(2) 0.000(2) 0.023(2) 0.007(3)
C13 0.050(3) 0.071(3) 0.036(3) -0.013(2) 0.012(2) -0.001(2)
C14 0.033(2) 0.054(2) 0.040(2) -0.010(2) 0.012(2) -0.0017(19)
C15 0.026(2) 0.052(2) 0.030(2) 0.0059(18) 0.0097(18) 0.0128(17)
C16 0.038(2) 0.049(2) 0.040(2) 0.006(2) 0.018(2) 0.0059(19)
C17 0.041(3) 0.050(2) 0.066(3) 0.015(2) 0.029(3) 0.008(2)
C18 0.057(3) 0.065(3) 0.062(3) 0.013(3) 0.042(3) 0.014(2)
C19 0.066(3) 0.083(3) 0.045(3) 0.011(3) 0.038(3) 0.018(3)
C20 0.046(3) 0.063(3) 0.030(2) 0.004(2) 0.020(2) 0.008(2)
C21 0.023(2) 0.051(2) 0.027(2) 0.0025(17) 0.0097(17) -0.0002(16)
C22 0.043(3) 0.053(2) 0.034(2) -0.005(2) 0.010(2) -0.001(2)
C23 0.051(3) 0.058(3) 0.041(3) 0.004(2) 0.010(2) 0.002(2)
C24 0.040(3) 0.043(2) 0.057(3) 0.004(2) 0.017(2) 0.0040(19)
C25 0.043(3) 0.051(2) 0.050(3) -0.005(2) 0.023(2) -0.002(2)
C26 0.036(2) 0.050(2) 0.031(2) -0.0041(18) 0.0140(19) -0.0013(18)
C27 0.032(2) 0.050(2) 0.028(2) -0.0016(17) 0.0161(19) -0.0008(18)
C28 0.038(2) 0.054(2) 0.032(2) -0.0007(19) 0.019(2) -0.0033(19)
C29 0.044(3) 0.063(3) 0.026(2) 0.0020(19) 0.019(2) -0.001(2)
C30 0.032(2) 0.071(3) 0.026(2) -0.008(2) 0.0100(19) -0.002(2)
C31 0.031(2) 0.052(2) 0.045(3) -0.007(2) 0.012(2) -0.0043(19)
C32 0.033(2) 0.051(2) 0.032(2) 0.0059(19) 0.0121(19) -0.0020(19)
C33 0.038(2) 0.055(2) 0.0221(19) -0.0013(17) 0.0168(19) -0.0044(19)
C34 0.038(2) 0.058(2) 0.026(2) -0.0017(18) 0.0167(19) -0.004(2)
C35 0.035(3) 0.082(3) 0.034(3) -0.002(2) 0.021(2) 0.000(2)
C36 0.033(2) 0.094(4) 0.038(2) -0.005(3) 0.018(2) -0.016(3)
C37 0.050(3) 0.074(3) 0.034(2) -0.012(2) 0.024(2) -0.024(3)
C38 0.044(3) 0.059(2) 0.030(2) -0.005(2) 0.023(2) -0.006(2)
B1 0.036(3) 0.041(2) 0.028(2) -0.0012(19) 0.015(2) -0.0039(19)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 B1 1.373(5) . ?
N1 P2 1.571(3) . ?
P1 C1 1.768(4) . ?
P1 C9 1.830(4) . ?
P1 C3 1.835(4) . ?
P2 C2 1.763(4) . ?
P2 C15 1.794(4) . ?
P2 C21 1.810(4) . ?
F1 C28 1.343(5) . ?
F2 C29 1.350(5) . ?
F3 C30 1.347(5) . ?
F4 C31 1.329(5) . ?
F5 C32 1.353(5) . ?
F6 C34 1.356(5) . ?
F7 C35 1.327(6) . ?
F8 C36 1.337(5) . ?
F9 C37 1.359(6) . ?
F10 C38 1.335(5) . ?
C1 C2 1.194(5) . ?
C3 C8 1.373(7) . ?
C3 C4 1.399(6) . ?
C4 C5 1.383(8) . ?
C4 H4A 0.9500 . ?
C5 C6 1.367(10) . ?
C5 H5A 0.9500 . ?
C6 C7 1.381(8) . ?
C6 H6A 0.9500 . ?
C7 C8 1.377(7) . ?
C7 H7A 0.9500 . ?
C8 H8A 0.9500 . ?
C9 C10 1.380(6) . ?
C9 C14 1.395(5) . ?
C10 C11 1.389(6) . ?
C10 H10A 0.9500 . ?
C11 C12 1.376(7) . ?
C11 H11A 0.9500 . ?
C12 C13 1.367(7) . ?
C12 H12A 0.9500 . ?
C13 C14 1.380(6) . ?
C13 H13A 0.9500 . ?
C14 H14A 0.9500 . ?
C15 C16 1.388(6) . ?
C15 C20 1.405(5) . ?
C16 C17 1.383(6) . ?
C16 H16A 0.9500 . ?
C17 C18 1.377(7) . ?
C17 H17A 0.9500 . ?
C18 C19 1.368(7) . ?
C18 H18A 0.9500 . ?
C19 C20 1.386(6) . ?
C19 H19A 0.9500 . ?
C20 H20A 0.9500 . ?
C21 C22 1.382(6) . ?
C21 C26 1.395(5) . ?
C22 C23 1.376(7) . ?
C22 H22A 0.9500 . ?
C23 C24 1.374(6) . ?
C23 H23A 0.9500 . ?
C24 C25 1.377(6) . ?
C24 H24A 0.9500 . ?
C25 C26 1.371(7) . ?
C25 H25A 0.9500 . ?
C26 H26A 0.9500 . ?
C27 C32 1.372(6) . ?
C27 C28 1.399(6) . ?
C27 B1 1.608(6) . ?
C28 C29 1.384(6) . ?
C29 C30 1.350(7) . ?
C30 C31 1.390(6) . ?
C31 C32 1.365(6) . ?
C33 C34 1.379(6) . ?
C33 C38 1.397(6) . ?
C33 B1 1.590(6) . ?
C34 C35 1.375(6) . ?
C35 C36 1.388(8) . ?
C36 C37 1.361(8) . ?
C37 C38 1.370(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
B1 N1 P2 135.7(3) . . ?
C1 P1 C9 99.53(16) . . ?
C1 P1 C3 100.33(19) . . ?
C9 P1 C3 103.25(17) . . ?
N1 P2 C2 118.33(17) . . ?
N1 P2 C15 109.65(19) . . ?
C2 P2 C15 103.32(19) . . ?
N1 P2 C21 110.47(18) . . ?
C2 P2 C21 104.42(19) . . ?
C15 P2 C21 110.26(16) . . ?
C2 C1 P1 172.2(3) . . ?
C1 C2 P2 177.7(3) . . ?
C8 C3 C4 119.0(4) . . ?
C8 C3 P1 126.2(3) . . ?
C4 C3 P1 114.8(4) . . ?
C5 C4 C3 119.5(5) . . ?
C5 C4 H4A 120.2 . . ?
C3 C4 H4A 120.2 . . ?
C6 C5 C4 120.8(5) . . ?
C6 C5 H5A 119.6 . . ?
C4 C5 H5A 119.6 . . ?
C5 C6 C7 119.7(5) . . ?
C5 C6 H6A 120.1 . . ?
C7 C6 H6A 120.1 . . ?
C8 C7 C6 120.0(5) . . ?
C8 C7 H7A 120.0 . . ?
C6 C7 H7A 120.0 . . ?
C3 C8 C7 121.0(4) . . ?
C3 C8 H8A 119.5 . . ?
C7 C8 H8A 119.5 . . ?
C10 C9 C14 118.8(4) . . ?
C10 C9 P1 125.0(3) . . ?
C14 C9 P1 116.2(3) . . ?
C9 C10 C11 121.0(4) . . ?
C9 C10 H10A 119.5 . . ?
C11 C10 H10A 119.5 . . ?
C12 C11 C10 119.3(4) . . ?
C12 C11 H11A 120.3 . . ?
C10 C11 H11A 120.3 . . ?
C13 C12 C11 120.3(4) . . ?
C13 C12 H12A 119.9 . . ?
C11 C12 H12A 119.9 . . ?
C12 C13 C14 120.8(5) . . ?
C12 C13 H13A 119.6 . . ?
C14 C13 H13A 119.6 . . ?
C13 C14 C9 119.8(4) . . ?
C13 C14 H14A 120.1 . . ?
C9 C14 H14A 120.1 . . ?
C16 C15 C20 119.3(4) . . ?
C16 C15 P2 120.1(3) . . ?
C20 C15 P2 120.6(3) . . ?
C17 C16 C15 120.2(4) . . ?
C17 C16 H16A 119.9 . . ?
C15 C16 H16A 119.9 . . ?
C18 C17 C16 120.3(5) . . ?
C18 C17 H17A 119.9 . . ?
C16 C17 H17A 119.9 . . ?
C19 C18 C17 120.1(4) . . ?
C19 C18 H18A 120.0 . . ?
C17 C18 H18A 120.0 . . ?
C18 C19 C20 121.0(5) . . ?
C18 C19 H19A 119.5 . . ?
C20 C19 H19A 119.5 . . ?
C19 C20 C15 119.2(5) . . ?
C19 C20 H20A 120.4 . . ?
C15 C20 H20A 120.4 . . ?
C22 C21 C26 119.8(4) . . ?
C22 C21 P2 118.8(3) . . ?
C26 C21 P2 121.4(3) . . ?
C23 C22 C21 119.5(4) . . ?
C23 C22 H22A 120.3 . . ?
C21 C22 H22A 120.3 . . ?
C24 C23 C22 120.7(5) . . ?
C24 C23 H23A 119.7 . . ?
C22 C23 H23A 119.7 . . ?
C23 C24 C25 119.9(4) . . ?
C23 C24 H24A 120.0 . . ?
C25 C24 H24A 120.0 . . ?
C26 C25 C24 120.3(4) . . ?
C26 C25 H25A 119.9 . . ?
C24 C25 H25A 119.9 . . ?
C25 C26 C21 119.8(4) . . ?
C25 C26 H26A 120.1 . . ?
C21 C26 H26A 120.1 . . ?
C32 C27 C28 115.2(4) . . ?
C32 C27 B1 124.1(4) . . ?
C28 C27 B1 120.8(4) . . ?
F1 C28 C29 118.8(4) . . ?
F1 C28 C27 119.3(4) . . ?
C29 C28 C27 121.9(4) . . ?
C30 C29 F2 120.6(4) . . ?
C30 C29 C28 120.0(4) . . ?
F2 C29 C28 119.3(4) . . ?
F3 C30 C29 120.7(4) . . ?
F3 C30 C31 119.0(4) . . ?
C29 C30 C31 120.3(4) . . ?
F4 C31 C32 122.3(4) . . ?
F4 C31 C30 119.5(4) . . ?
C32 C31 C30 118.1(4) . . ?
F5 C32 C31 116.3(4) . . ?
F5 C32 C27 119.1(4) . . ?
C31 C32 C27 124.5(4) . . ?
C34 C33 C38 115.4(4) . . ?
C34 C33 B1 122.0(4) . . ?
C38 C33 B1 122.6(4) . . ?
F6 C34 C35 116.9(4) . . ?
F6 C34 C33 118.9(4) . . ?
C35 C34 C33 124.2(4) . . ?
F7 C35 C34 120.8(5) . . ?
F7 C35 C36 121.4(4) . . ?
C34 C35 C36 117.8(5) . . ?
F8 C36 C37 121.1(5) . . ?
F8 C36 C35 118.7(5) . . ?
C37 C36 C35 120.2(4) . . ?
F9 C37 C36 119.8(4) . . ?
F9 C37 C38 119.7(5) . . ?
C36 C37 C38 120.5(5) . . ?
F10 C38 C37 118.3(4) . . ?
F10 C38 C33 119.8(4) . . ?
C37 C38 C33 121.9(4) . . ?
N1 B1 C33 126.0(4) . . ?
N1 B1 C27 117.5(4) . . ?
C33 B1 C27 116.5(3) . . ?
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
B1 N1 P2 C2 17.8(5) . . . . ?
B1 N1 P2 C15 135.9(4) . . . . ?
B1 N1 P2 C21 -102.4(5) . . . . ?
C1 P1 C3 C8 28.7(4) . . . . ?
C9 P1 C3 C8 -73.7(4) . . . . ?
C1 P1 C3 C4 -153.0(3) . . . . ?
C9 P1 C3 C4 104.5(3) . . . . ?
C8 C3 C4 C5 0.4(8) . . . . ?
P1 C3 C4 C5 -178.1(5) . . . . ?
C3 C4 C5 C6 -0.3(10) . . . . ?
C4 C5 C6 C7 -0.4(11) . . . . ?
C5 C6 C7 C8 1.2(9) . . . . ?
C4 C3 C8 C7 0.4(7) . . . . ?
P1 C3 C8 C7 178.6(4) . . . . ?
C6 C7 C8 C3 -1.1(8) . . . . ?
C1 P1 C9 C10 -39.1(4) . . . . ?
C3 P1 C9 C10 64.0(4) . . . . ?
C1 P1 C9 C14 141.6(3) . . . . ?
C3 P1 C9 C14 -115.3(3) . . . . ?
C14 C9 C10 C11 1.3(6) . . . . ?
P1 C9 C10 C11 -178.0(4) . . . . ?
C9 C10 C11 C12 -0.9(7) . . . . ?
C10 C11 C12 C13 0.4(7) . . . . ?
C11 C12 C13 C14 -0.2(7) . . . . ?
C12 C13 C14 C9 0.6(7) . . . . ?
C10 C9 C14 C13 -1.1(6) . . . . ?
P1 C9 C14 C13 178.3(3) . . . . ?
N1 P2 C15 C16 17.5(4) . . . . ?
C2 P2 C15 C16 144.6(3) . . . . ?
C21 P2 C15 C16 -104.3(3) . . . . ?
N1 P2 C15 C20 -162.4(3) . . . . ?
C2 P2 C15 C20 -35.4(4) . . . . ?
C21 P2 C15 C20 75.7(4) . . . . ?
C20 C15 C16 C17 -1.3(6) . . . . ?
P2 C15 C16 C17 178.7(3) . . . . ?
C15 C16 C17 C18 1.2(6) . . . . ?
C16 C17 C18 C19 -0.2(7) . . . . ?
C17 C18 C19 C20 -0.7(7) . . . . ?
C18 C19 C20 C15 0.6(7) . . . . ?
C16 C15 C20 C19 0.4(6) . . . . ?
P2 C15 C20 C19 -179.6(4) . . . . ?
N1 P2 C21 C22 1.1(4) . . . . ?
C2 P2 C21 C22 -127.1(3) . . . . ?
C15 P2 C21 C22 122.5(3) . . . . ?
N1 P2 C21 C26 -179.6(3) . . . . ?
C2 P2 C21 C26 52.1(3) . . . . ?
C15 P2 C21 C26 -58.3(4) . . . . ?
C26 C21 C22 C23 -1.2(6) . . . . ?
P2 C21 C22 C23 178.1(3) . . . . ?
C21 C22 C23 C24 0.6(7) . . . . ?
C22 C23 C24 C25 -0.1(7) . . . . ?
C23 C24 C25 C26 0.2(6) . . . . ?
C24 C25 C26 C21 -0.8(6) . . . . ?
C22 C21 C26 C25 1.3(6) . . . . ?
P2 C21 C26 C25 -178.0(3) . . . . ?
C32 C27 C28 F1 -178.8(4) . . . . ?
B1 C27 C28 F1 0.5(6) . . . . ?
C32 C27 C28 C29 -1.1(6) . . . . ?
B1 C27 C28 C29 178.3(4) . . . . ?
F1 C28 C29 C30 179.7(4) . . . . ?
C27 C28 C29 C30 1.9(6) . . . . ?
F1 C28 C29 F2 1.4(6) . . . . ?
C27 C28 C29 F2 -176.3(4) . . . . ?
F2 C29 C30 F3 -2.1(6) . . . . ?
C28 C29 C30 F3 179.6(3) . . . . ?
F2 C29 C30 C31 176.7(3) . . . . ?
C28 C29 C30 C31 -1.5(6) . . . . ?
F3 C30 C31 F4 -1.4(6) . . . . ?
C29 C30 C31 F4 179.7(4) . . . . ?
F3 C30 C31 C32 179.3(3) . . . . ?
C29 C30 C31 C32 0.4(6) . . . . ?
F4 C31 C32 F5 1.9(6) . . . . ?
C30 C31 C32 F5 -178.8(3) . . . . ?
F4 C31 C32 C27 -178.9(4) . . . . ?
C30 C31 C32 C27 0.4(6) . . . . ?
C28 C27 C32 F5 179.1(3) . . . . ?
B1 C27 C32 F5 -0.2(6) . . . . ?
C28 C27 C32 C31 0.0(6) . . . . ?
B1 C27 C32 C31 -179.4(4) . . . . ?
C38 C33 C34 F6 180.0(3) . . . . ?
B1 C33 C34 F6 0.2(5) . . . . ?
C38 C33 C34 C35 -1.0(6) . . . . ?
B1 C33 C34 C35 179.2(4) . . . . ?
F6 C34 C35 F7 -0.7(6) . . . . ?
C33 C34 C35 F7 -179.7(4) . . . . ?
F6 C34 C35 C36 180.0(4) . . . . ?
C33 C34 C35 C36 0.9(6) . . . . ?
F7 C35 C36 F8 0.4(7) . . . . ?
C34 C35 C36 F8 179.7(3) . . . . ?
F7 C35 C36 C37 179.8(4) . . . . ?
C34 C35 C36 C37 -0.9(6) . . . . ?
F8 C36 C37 F9 0.0(6) . . . . ?
C35 C36 C37 F9 -179.4(4) . . . . ?
F8 C36 C37 C38 -179.7(4) . . . . ?
C35 C36 C37 C38 0.9(6) . . . . ?
F9 C37 C38 F10 -0.3(6) . . . . ?
C36 C37 C38 F10 179.3(4) . . . . ?
F9 C37 C38 C33 179.3(4) . . . . ?
C36 C37 C38 C33 -1.0(6) . . . . ?
C34 C33 C38 F10 -179.4(3) . . . . ?
B1 C33 C38 F10 0.4(6) . . . . ?
C34 C33 C38 C37 1.0(6) . . . . ?
B1 C33 C38 C37 -179.2(4) . . . . ?
P2 N1 B1 C33 -4.2(7) . . . . ?
P2 N1 B1 C27 176.7(3) . . . . ?
C34 C33 B1 N1 -123.0(5) . . . . ?
C38 C33 B1 N1 57.2(6) . . . . ?
C34 C33 B1 C27 56.1(5) . . . . ?
C38 C33 B1 C27 -123.6(4) . . . . ?
C32 C27 B1 N1 69.5(6) . . . . ?
C28 C27 B1 N1 -109.8(4) . . . . ?
C32 C27 B1 C33 -109.7(4) . . . . ?
C28 C27 B1 C33 71.0(5) . . . . ?
_diffrn_measured_fraction_theta_max 0.953
_diffrn_reflns_theta_full        66.47
_diffrn_measured_fraction_theta_full 0.953
_refine_diff_density_max         0.600
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.061
_vrf_PLAT029_d12277              
;
PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.953
RESPONSE: Data were collected using CuKalpha
radiation using a Bruker Microsource system eqipped with
multi layer optics. We feel that the precision of the structure
is good enough to support any claims made regadring the
geometry of the molecule and the intermolecular distances.
;
# end Validation Reply Form
_iucr_refine_instructions_details 
;
TITL cu_d12277_0m in P2(1)
CELL 1.54178 13.6525 9.9457 13.7064 90.000 113.177 90.000
ZERR 2.00 0.0011 0.0008 0.0011 0.000 0.005 0.000
LATT -1
SYMM -x, y+1/2, -z
SFAC C H N B F P
UNIT 76 40 2 2 20 4
TEMP -126.150
SIZE 0.060 0.140 0.270
OMIT 7 5 6
ACTA
L.S. 4
FMAP 2
PLAN 20
HTAB
BOND $H
CONF
WGHT 0.0787 0.0000
FVAR 0.24580
N1 3 0.299240 0.104408 0.394971 11.00000 0.03301 0.04927 =
0.02181 -0.00656 0.00989 -0.00307
P1 6 -0.086958 -0.035372 0.061519 11.00000 0.02934 0.04563 =
0.03268 0.00041 0.01242 -0.00030
P2 6 0.273697 0.035497 0.284492 11.00000 0.02838 0.04706 =
0.02601 -0.00174 0.01253 0.00173
F1 5 0.297731 -0.002000 0.658601 11.00000 0.07467 0.05545 =
0.04437 0.00362 0.02407 -0.01265
F2 5 0.411418 0.104127 0.850836 11.00000 0.08398 0.08696 =
0.02747 0.00678 0.01922 -0.00939
F3 5 0.476452 0.365435 0.867560 11.00000 0.05606 0.09017 =
0.03317 -0.02441 0.01024 -0.01325
F4 5 0.433818 0.513821 0.690804 11.00000 0.05358 0.05607 =
0.06291 -0.00683 0.00921 -0.01551
F5 5 0.328594 0.406145 0.498611 11.00000 0.06597 0.06112 =
0.03991 0.00932 0.00870 -0.01373
F6 5 0.088498 0.331029 0.451030 11.00000 0.04260 0.05448 =
0.04357 -0.00022 0.02244 0.00086
F7 5 -0.119049 0.287989 0.398403 11.00000 0.04045 0.09630 =
0.05992 -0.00085 0.02493 0.01343
F8 5 -0.201248 0.036448 0.344752 11.00000 0.03493 0.12795 =
0.06080 -0.00828 0.02197 -0.01937
F9 5 -0.071989 -0.172036 0.343614 11.00000 0.06815 0.08012 =
0.06196 -0.02536 0.04029 -0.03795
F10 5 0.136432 -0.128494 0.398226 11.00000 0.06099 0.05049 =
0.05339 -0.00738 0.03347 -0.00619
C1 1 0.046891 0.005011 0.141597 11.00000 0.03359 0.04381 =
0.02980 -0.00023 0.01491 -0.00049
C2 1 0.139075 0.016234 0.197711 11.00000 0.03551 0.04800 =
0.03208 -0.00195 0.01723 0.00207
C3 1 -0.155345 0.109412 0.089101 11.00000 0.02737 0.06361 =
0.02699 -0.00018 0.01072 0.00453
C4 1 -0.260120 0.084453 0.077782 11.00000 0.03895 0.07606 =
0.06304 -0.01758 0.02469 -0.00584
AFIX 43
H4A 2 -0.289882 -0.002880 0.059378 11.00000 -1.20000
AFIX 0
C5 1 -0.320052 0.187779 0.093567 11.00000 0.04603 0.10359 =
0.09992 -0.03656 0.03535 0.00405
AFIX 43
H5A 2 -0.391324 0.171012 0.085546 11.00000 -1.20000
AFIX 0
C6 1 -0.278048 0.313749 0.120566 11.00000 0.06527 0.09056 =
0.07314 -0.01253 0.03326 0.02989
AFIX 43
H6A 2 -0.320093 0.384172 0.130739 11.00000 -1.20000
AFIX 0
C7 1 -0.174260 0.338196 0.132990 11.00000 0.07531 0.05745 =
0.06274 -0.00748 0.03344 0.00516
AFIX 43
H7A 2 -0.144302 0.425168 0.153019 11.00000 -1.20000
AFIX 0
C8 1 -0.114189 0.236455 0.116335 11.00000 0.04675 0.05240 =
0.05505 -0.00182 0.02736 0.00010
AFIX 43
H8A 2 -0.043245 0.254393 0.123789 11.00000 -1.20000
AFIX 0
C9 1 -0.087641 0.003489 -0.069232 11.00000 0.02727 0.04656 =
0.02604 -0.00320 0.00668 0.00571
C10 1 -0.036044 0.111107 -0.091446 11.00000 0.05616 0.05098 =
0.03141 -0.00652 0.01750 -0.00837
AFIX 43
H10A 2 0.005321 0.169737 -0.035741 11.00000 -1.20000
AFIX 0
C11 1 -0.043671 0.135025 -0.194044 11.00000 0.07928 0.05209 =
0.03972 -0.00514 0.03169 -0.00749
AFIX 43
H11A 2 -0.008689 0.210164 -0.208705 11.00000 -1.20000
AFIX 0
C12 1 -0.102440 0.048718 -0.274238 11.00000 0.07210 0.06339 =
0.03418 0.00008 0.02267 0.00671
AFIX 43
H12A 2 -0.107712 0.064022 -0.344550 11.00000 -1.20000
AFIX 0
C13 1 -0.153242 -0.058899 -0.253157 11.00000 0.04962 0.07066 =
0.03569 -0.01278 0.01244 -0.00110
AFIX 43
H13A 2 -0.193804 -0.117670 -0.309131 11.00000 -1.20000
AFIX 0
C14 1 -0.146306 -0.083194 -0.151497 11.00000 0.03332 0.05387 =
0.03972 -0.00970 0.01181 -0.00175
AFIX 43
H14A 2 -0.181398 -0.158758 -0.137597 11.00000 -1.20000
AFIX 0
C15 1 0.328604 0.133958 0.208526 11.00000 0.02636 0.05150 =
0.03020 0.00588 0.00973 0.01280
C16 1 0.406756 0.229039 0.258479 11.00000 0.03828 0.04861 =
0.03998 0.00638 0.01802 0.00587
AFIX 43
H16A 2 0.430143 0.243197 0.332761 11.00000 -1.20000
AFIX 0
C17 1 0.450676 0.303218 0.200444 11.00000 0.04127 0.05034 =
0.06587 0.01456 0.02903 0.00753
AFIX 43
H17A 2 0.505109 0.366950 0.235238 11.00000 -1.20000
AFIX 0
C18 1 0.415850 0.285103 0.092427 11.00000 0.05676 0.06483 =
0.06221 0.01344 0.04230 0.01363
AFIX 43
H18A 2 0.446124 0.336501 0.052870 11.00000 -1.20000
AFIX 0
C19 1 0.337713 0.193181 0.042036 11.00000 0.06565 0.08317 =
0.04455 0.01111 0.03847 0.01816
AFIX 43
H19A 2 0.313594 0.182061 -0.032620 11.00000 -1.20000
AFIX 0
C20 1 0.293200 0.116017 0.098266 11.00000 0.04611 0.06335 =
0.03016 0.00390 0.01958 0.00779
AFIX 43
H20A 2 0.239434 0.051810 0.062712 11.00000 -1.20000
AFIX 0
C21 1 0.327290 -0.133424 0.302382 11.00000 0.02331 0.05057 =
0.02731 0.00247 0.00975 -0.00021
C22 1 0.379805 -0.181906 0.404352 11.00000 0.04309 0.05338 =
0.03448 -0.00514 0.01047 -0.00142
AFIX 43
H22A 2 0.389261 -0.126208 0.463697 11.00000 -1.20000
AFIX 0
C23 1 0.418280 -0.311484 0.419226 11.00000 0.05126 0.05832 =
0.04056 0.00375 0.01013 0.00197
AFIX 43
H23A 2 0.453847 -0.345304 0.489215 11.00000 -1.20000
AFIX 0
C24 1 0.405788 -0.392477 0.333889 11.00000 0.03955 0.04265 =
0.05705 0.00384 0.01698 0.00399
AFIX 43
H24A 2 0.432698 -0.481752 0.344997 11.00000 -1.20000
AFIX 0
C25 1 0.354192 -0.344009 0.232238 11.00000 0.04262 0.05132 =
0.05025 -0.00500 0.02276 -0.00165
AFIX 43
H25A 2 0.345384 -0.400131 0.173282 11.00000 -1.20000
AFIX 0
C26 1 0.315509 -0.215156 0.215791 11.00000 0.03583 0.04975 =
0.03072 -0.00414 0.01401 -0.00130
AFIX 43
H26A 2 0.280769 -0.181610 0.145608 11.00000 -1.20000
AFIX 0
C27 1 0.307638 0.199411 0.570998 11.00000 0.03176 0.04955 =
0.02761 -0.00160 0.01614 -0.00083
C28 1 0.329833 0.126505 0.664603 11.00000 0.03754 0.05446 =
0.03208 -0.00069 0.01909 -0.00328
C29 1 0.387304 0.181486 0.763542 11.00000 0.04448 0.06340 =
0.02585 0.00201 0.01864 -0.00127
C30 1 0.420997 0.310166 0.771835 11.00000 0.03240 0.07146 =
0.02562 -0.00812 0.00998 -0.00172
C31 1 0.400447 0.387061 0.681211 11.00000 0.03074 0.05192 =
0.04450 -0.00722 0.01207 -0.00427
C32 1 0.345184 0.328915 0.584902 11.00000 0.03337 0.05098 =
0.03183 0.00585 0.01205 -0.00205
C33 1 0.120252 0.103487 0.426125 11.00000 0.03810 0.05543 =
0.02208 -0.00129 0.01681 -0.00437
C34 1 0.050570 0.204320 0.425135 11.00000 0.03780 0.05763 =
0.02603 -0.00168 0.01672 -0.00391
C35 1 -0.056789 0.185750 0.397878 11.00000 0.03454 0.08163 =
0.03417 -0.00166 0.02068 0.00044
C36 1 -0.097147 0.056696 0.371071 11.00000 0.03252 0.09422 =
0.03778 -0.00463 0.01800 -0.01564
C37 1 -0.031552 -0.046226 0.370899 11.00000 0.05043 0.07374 =
0.03451 -0.01166 0.02353 -0.02361
C38 1 0.075107 -0.024148 0.398567 11.00000 0.04382 0.05927 =
0.02971 -0.00532 0.02263 -0.00605
B1 4 0.243529 0.131443 0.457050 11.00000 0.03645 0.04080 =
0.02772 -0.00119 0.01498 -0.00388
HKLF 4 1 1 0 0 0 1 0 0 0 1
REM cu_d12277_0m in P2(1)
REM R1 = 0.0482 for 3478 Fo > 4sig(Fo) and 0.0542 for all 3883 data
REM 469 parameters refined using 1 restraints
END
REM Highest difference peak 0.600, deepest hole -0.446, 1-sigma level 0.061
Q1 1 0.1980 0.0348 0.2317 11.00000 0.05 0.60
Q2 1 -0.0112 -0.0292 0.1139 11.00000 0.05 0.46
Q3 1 -0.0921 0.0534 0.0670 11.00000 0.05 0.35
Q4 1 0.2805 -0.0552 0.2872 11.00000 0.05 0.29
Q5 1 0.3383 0.1194 0.8225 11.00000 0.05 0.27
Q6 1 -0.0963 -0.1289 0.0688 11.00000 0.05 0.27
Q7 1 -0.0052 0.0174 0.0639 11.00000 0.05 0.26
Q8 1 0.2754 0.1363 0.2847 11.00000 0.05 0.24
Q9 1 0.2318 0.0969 0.3412 11.00000 0.05 0.23
Q10 1 0.2185 0.0156 0.6207 11.00000 0.05 0.23
Q11 1 0.3489 0.0346 0.3306 11.00000 0.05 0.22
Q12 1 -0.2199 0.2662 0.3407 11.00000 0.05 0.22
Q13 1 -0.1557 -0.0375 0.0026 11.00000 0.05 0.21
Q14 1 0.3945 0.1523 0.7240 11.00000 0.05 0.20
Q15 1 -0.2052 -0.2183 0.2820 11.00000 0.05 0.20
Q16 1 0.4980 0.5432 0.6261 11.00000 0.05 0.20
Q17 1 0.3970 -0.1590 0.1817 11.00000 0.05 0.20
Q18 1 -0.0778 -0.0619 -0.0870 11.00000 0.05 0.20
Q19 1 0.0018 -0.0144 0.2391 11.00000 0.05 0.19
Q20 1 0.0401 0.4025 0.4821 11.00000 0.05 0.19
;


data_d12293a
_database_code_depnum_ccdc_archive 'CCDC 929333'
#TrackingRef 'd12293a.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C64 H30 B4 F40 N6 O12 P4'
_chemical_formula_sum            'C64 H30 B4 F40 N6 O12 P4'
_chemical_formula_weight         2002.06
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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   'C c'
_symmetry_space_group_name_Hall  'C -2yc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
_cell_length_a                   16.250(2)
_cell_length_b                   20.594(3)
_cell_length_c                   24.262(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.673(3)
_cell_angle_gamma                90.00
_cell_volume                     7736(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    147(2)
_cell_measurement_reflns_used    9930
_cell_measurement_theta_min      2.63
_cell_measurement_theta_max      27.43
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3968
_exptl_absorpt_coefficient_mu    0.258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9454
_exptl_absorpt_correction_T_max  0.9672
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      147(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'Bruker Triumph'
_diffrn_measurement_device_type  'Bruker Kappa APEX-DUO CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34318
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.65
_diffrn_reflns_theta_max         27.49
_reflns_number_total             15431
_reflns_number_gt                12817
_reflns_threshold_expression     I>2\s(I)
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       APEX2
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0541P)^2^+18.4778P] where P=(Fo^2^+2Fc^2^)/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   0.27(8)
_refine_ls_number_reflns         15431
_refine_ls_number_parameters     1171
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0528
_refine_ls_wR_factor_ref         0.1327
_refine_ls_wR_factor_gt          0.1233
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0.003
_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 0.32826(7) 0.90374(5) 0.72701(5) 0.0311(2) Uani 1 1 d . . .
P2 P 0.16186(6) 0.74510(5) 0.87767(4) 0.0240(2) Uani 1 1 d . . .
P3 P 0.20533(6) 0.57212(5) 0.88124(5) 0.0279(2) Uani 1 1 d . . .
P4 P 0.35867(6) 0.73109(5) 0.72462(4) 0.0241(2) Uani 1 1 d . . .
F1 F 0.2643(2) 0.78124(19) 0.57493(17) 0.0825(12) Uani 1 1 d . . .
F2 F 0.1964(3) 0.8423(2) 0.4752(2) 0.1084(17) Uani 1 1 d . . .
F3 F 0.2688(2) 0.95265(17) 0.44973(14) 0.0641(9) Uani 1 1 d . . .
F4 F 0.4082(3) 1.00397(19) 0.52832(17) 0.0802(12) Uani 1 1 d . . .
F5 F 0.4772(3) 0.9449(2) 0.63023(17) 0.0940(15) Uani 1 1 d . . .
F6 F 0.57214(17) 0.90051(17) 0.75286(16) 0.0640(9) Uani 1 1 d . . .
F7 F 0.73723(19) 0.8763(2) 0.76919(19) 0.0923(14) Uani 1 1 d . . .
F8 F 0.7861(2) 0.7779(3) 0.7115(3) 0.133(2) Uani 1 1 d . . .
F9 F 0.6635(3) 0.7079(4) 0.6318(3) 0.153(3) Uani 1 1 d . . .
F10 F 0.4962(3) 0.7347(2) 0.61247(18) 0.0874(13) Uani 1 1 d . . .
F11 F 0.2450(3) 0.69515(18) 1.0278(2) 0.1039(18) Uani 1 1 d . . .
F12 F 0.3041(4) 0.6416(2) 1.1314(2) 0.120(2) Uani 1 1 d . . .
F13 F 0.2331(3) 0.5331(2) 1.15783(15) 0.0932(15) Uani 1 1 d . . .
F14 F 0.1034(3) 0.4718(3) 1.0748(2) 0.1077(17) Uani 1 1 d . . .
F15 F 0.0447(3) 0.5245(2) 0.96888(18) 0.0938(15) Uani 1 1 d . . .
F16 F -0.04234(16) 0.56607(15) 0.84067(14) 0.0524(7) Uani 1 1 d . . .
F17 F -0.21106(17) 0.58398(17) 0.81763(15) 0.0636(9) Uani 1 1 d . . .
F18 F -0.27236(19) 0.6802(2) 0.8688(2) 0.0931(14) Uani 1 1 d . . .
F19 F -0.1601(2) 0.7542(2) 0.9524(2) 0.1050(17) Uani 1 1 d . . .
F20 F 0.0101(2) 0.73325(18) 0.97965(17) 0.0684(10) Uani 1 1 d . . .
F21 F -0.07322(16) 0.70887(14) 0.78358(11) 0.0453(7) Uani 1 1 d . . .
F22 F -0.1806(2) 0.6241(2) 0.71415(17) 0.0828(12) Uani 1 1 d . . .
F23 F -0.1689(3) 0.5998(3) 0.6070(2) 0.1115(18) Uani 1 1 d . . .
F24 F -0.0527(3) 0.6665(3) 0.56865(17) 0.1076(18) Uani 1 1 d . . .
F25 F 0.05988(18) 0.74733(17) 0.63841(12) 0.0560(8) Uani 1 1 d . . .
F26 F -0.00380(17) 0.82554(15) 0.85951(12) 0.0465(7) Uani 1 1 d . . .
F27 F -0.0953(2) 0.93267(18) 0.85602(16) 0.0711(10) Uani 1 1 d . . .
F28 F -0.1333(2) 1.01266(15) 0.7618(2) 0.0841(13) Uani 1 1 d . . .
F29 F -0.0765(2) 0.98129(17) 0.67071(19) 0.0767(11) Uani 1 1 d . . .
F30 F 0.01234(18) 0.87272(15) 0.67224(13) 0.0505(7) Uani 1 1 d . . .
F31 F 0.51306(17) 0.61138(14) 0.93394(12) 0.0478(7) Uani 1 1 d . . .
F32 F 0.6001(2) 0.50139(16) 0.9384(2) 0.0883(14) Uani 1 1 d . . .
F33 F 0.6529(2) 0.46456(16) 0.8470(2) 0.0980(16) Uani 1 1 d . . .
F34 F 0.6117(2) 0.53842(19) 0.75032(19) 0.0868(14) Uani 1 1 d . . .
F35 F 0.52291(17) 0.64706(16) 0.74354(13) 0.0543(8) Uani 1 1 d . . .
F36 F 0.59613(15) 0.76649(14) 0.81374(11) 0.0417(6) Uani 1 1 d . . .
F37 F 0.7070(2) 0.85227(19) 0.87751(17) 0.0806(11) Uani 1 1 d . . .
F38 F 0.7015(3) 0.8821(3) 0.9856(2) 0.1142(19) Uani 1 1 d . . .
F39 F 0.5847(3) 0.8236(3) 1.02752(17) 0.0997(16) Uani 1 1 d . . .
F40 F 0.46844(17) 0.74053(16) 0.96331(12) 0.0510(7) Uani 1 1 d . . .
O1 O 0.40574(17) 0.87084(15) 0.71705(13) 0.0335(6) Uani 1 1 d . . .
O2 O 0.38482(18) 0.76229(15) 0.67606(12) 0.0338(6) Uani 1 1 d . . .
O3 O 0.2850(2) 0.94871(14) 0.67613(14) 0.0391(7) Uani 1 1 d . . .
O4 O 0.3570(2) 0.94546(16) 0.78192(15) 0.0505(9) Uani 1 1 d . . .
O5 O 0.33155(17) 0.66009(14) 0.71014(12) 0.0303(6) Uani 1 1 d . . .
O6 O 0.42940(16) 0.73467(14) 0.78175(12) 0.0279(6) Uani 1 1 d . . .
O7 O 0.12135(17) 0.60032(14) 0.88577(12) 0.0305(6) Uani 1 1 d . . .
O8 O 0.13397(17) 0.71033(14) 0.92392(12) 0.0302(6) Uani 1 1 d . . .
O9 O 0.24960(19) 0.53461(14) 0.93664(13) 0.0364(7) Uani 1 1 d . . .
O10 O 0.1909(2) 0.52329(15) 0.83112(14) 0.0431(8) Uani 1 1 d . . .
O11 O 0.18492(18) 0.81639(13) 0.89470(13) 0.0306(6) Uani 1 1 d . . .
O12 O 0.09314(16) 0.74231(13) 0.81975(11) 0.0256(6) Uani 1 1 d . . .
N1 N 0.1813(2) 0.85305(16) 0.74567(14) 0.0275(7) Uani 1 1 d . . .
N2 N 0.14964(19) 0.79360(16) 0.74802(14) 0.0243(6) Uani 1 1 d . . .
N3 N 0.19924(19) 0.74500(15) 0.73985(14) 0.0228(6) Uani 1 1 d . . .
N4 N 0.32325(19) 0.73534(15) 0.86268(14) 0.0237(6) Uani 1 1 d . . .
N5 N 0.37472(19) 0.68720(15) 0.85630(14) 0.0226(6) Uani 1 1 d . . .
N6 N 0.34490(19) 0.62783(15) 0.86002(14) 0.0253(7) Uani 1 1 d . . .
C1 C 0.2571(2) 0.84195(18) 0.73447(17) 0.0244(8) Uani 1 1 d . . .
C2 C 0.2680(2) 0.77470(19) 0.73145(15) 0.0236(8) Uani 1 1 d . . .
C3 C 0.2556(2) 0.70503(18) 0.87180(16) 0.0224(7) Uani 1 1 d . . .
C4 C 0.2696(2) 0.63736(18) 0.87064(16) 0.0240(7) Uani 1 1 d . . .
C5 C 0.2043(3) 0.9840(2) 0.6700(3) 0.0499(13) Uani 1 1 d . . .
H5A H 0.1697 0.9611 0.6913 0.060 Uiso 1 1 calc R . .
H5B H 0.2171 1.0283 0.6861 0.060 Uiso 1 1 calc R . .
C6 C 0.1564(6) 0.9875(6) 0.6091(4) 0.132(4) Uani 1 1 d . . .
H6A H 0.1020 1.0108 0.6042 0.198 Uiso 1 1 calc R . .
H6B H 0.1439 0.9434 0.5934 0.198 Uiso 1 1 calc R . .
H6C H 0.1908 1.0105 0.5884 0.198 Uiso 1 1 calc R . .
C7 C 0.4160(5) 0.9117(3) 0.8409(3) 0.0693(17) Uani 1 1 d . . .
H7A H 0.4205 0.8643 0.8359 0.083 Uiso 1 1 calc R . .
H7B H 0.4747 0.9307 0.8536 0.083 Uiso 1 1 calc R . .
C8 C 0.3702(5) 0.9259(4) 0.8813(4) 0.090(2) Uani 1 1 d . . .
H8A H 0.4009 0.9070 0.9189 0.135 Uiso 1 1 calc R . .
H8B H 0.3119 0.9075 0.8673 0.135 Uiso 1 1 calc R . .
H8C H 0.3663 0.9731 0.8852 0.135 Uiso 1 1 calc R . .
C9 C 0.2720(4) 0.6395(3) 0.6541(2) 0.0604(15) Uani 1 1 d . . .
H9A H 0.2337 0.6048 0.6604 0.073 Uiso 1 1 calc R . .
H9B H 0.2353 0.6767 0.6356 0.073 Uiso 1 1 calc R . .
C10 C 0.3186(6) 0.6159(3) 0.6162(3) 0.091(3) Uani 1 1 d . . .
H10A H 0.2775 0.6022 0.5794 0.137 Uiso 1 1 calc R . .
H10B H 0.3545 0.5789 0.6344 0.137 Uiso 1 1 calc R . .
H10C H 0.3554 0.6506 0.6092 0.137 Uiso 1 1 calc R . .
C11 C 0.3338(3) 0.5008(3) 0.9464(2) 0.0496(12) Uani 1 1 d . . .
H11A H 0.3246 0.4536 0.9396 0.060 Uiso 1 1 calc R . .
H11B H 0.3641 0.5177 0.9196 0.060 Uiso 1 1 calc R . .
C12 C 0.3852(5) 0.5134(6) 1.0071(4) 0.121(4) Uani 1 1 d . . .
H12A H 0.4414 0.4918 1.0154 0.182 Uiso 1 1 calc R . .
H12B H 0.3543 0.4965 1.0331 0.182 Uiso 1 1 calc R . .
H12C H 0.3939 0.5603 1.0131 0.182 Uiso 1 1 calc R . .
C13 C 0.1727(3) 0.5389(3) 0.7703(2) 0.0525(13) Uani 1 1 d . . .
H13A H 0.1848 0.5006 0.7494 0.063 Uiso 1 1 calc R . .
H13B H 0.2107 0.5748 0.7659 0.063 Uiso 1 1 calc R . .
C14 C 0.0815(4) 0.5584(3) 0.7450(3) 0.0729(18) Uani 1 1 d . . .
H14A H 0.0705 0.5690 0.7040 0.109 Uiso 1 1 calc R . .
H14B H 0.0696 0.5965 0.7656 0.109 Uiso 1 1 calc R . .
H14C H 0.0439 0.5225 0.7486 0.109 Uiso 1 1 calc R . .
C15 C 0.2323(4) 0.8373(3) 0.9547(2) 0.0590(14) Uani 1 1 d . . .
H15A H 0.2667 0.8768 0.9536 0.071 Uiso 1 1 calc R . .
H15B H 0.2724 0.8026 0.9748 0.071 Uiso 1 1 calc R . .
C16 C 0.1680(5) 0.8514(3) 0.9868(3) 0.076(2) Uani 1 1 d . . .
H16A H 0.1988 0.8650 1.0264 0.115 Uiso 1 1 calc R . .
H16B H 0.1343 0.8122 0.9878 0.115 Uiso 1 1 calc R . .
H16C H 0.1291 0.8863 0.9670 0.115 Uiso 1 1 calc R . .
C17 C 0.3763(3) 0.8595(2) 0.60671(19) 0.0359(10) Uani 1 1 d . . .
C18 C 0.3035(3) 0.8360(3) 0.5661(2) 0.0461(12) Uani 1 1 d . . .
C19 C 0.2678(3) 0.8671(3) 0.5136(2) 0.0572(14) Uani 1 1 d . . .
C20 C 0.3033(3) 0.9232(3) 0.5010(2) 0.0479(12) Uani 1 1 d . . .
C21 C 0.3744(4) 0.9484(3) 0.5403(2) 0.0489(12) Uani 1 1 d . . .
C22 C 0.4085(3) 0.9164(3) 0.5921(2) 0.0478(12) Uani 1 1 d . . .
C23 C 0.5254(3) 0.8181(3) 0.6828(2) 0.0449(12) Uani 1 1 d . . .
C24 C 0.5899(3) 0.8522(3) 0.7211(3) 0.0530(14) Uani 1 1 d . . .
C25 C 0.6776(3) 0.8396(3) 0.7307(3) 0.0666(19) Uani 1 1 d . . .
C26 C 0.7007(4) 0.7894(5) 0.7004(4) 0.091(3) Uani 1 1 d . . .
C27 C 0.6411(5) 0.7564(5) 0.6621(4) 0.091(3) Uani 1 1 d . . .
C28 C 0.5533(4) 0.7691(4) 0.6528(3) 0.0707(19) Uani 1 1 d . . .
C29 C 0.1393(3) 0.6154(2) 0.99348(19) 0.0351(10) Uani 1 1 d . . .
C30 C 0.2066(3) 0.6412(2) 1.0364(2) 0.0472(12) Uani 1 1 d . . .
C31 C 0.2394(4) 0.6143(3) 1.0915(3) 0.0679(19) Uani 1 1 d . . .
C32 C 0.2042(4) 0.5594(3) 1.1047(2) 0.0635(17) Uani 1 1 d . . .
C33 C 0.1368(4) 0.5290(3) 1.0627(3) 0.0663(18) Uani 1 1 d . . .
C34 C 0.1073(3) 0.5575(3) 1.0094(2) 0.0573(15) Uani 1 1 d . . .
C35 C -0.0073(3) 0.6498(2) 0.91107(19) 0.0342(9) Uani 1 1 d . . .
C36 C -0.0666(3) 0.6125(2) 0.8705(2) 0.0383(10) Uani 1 1 d . . .
C37 C -0.1556(3) 0.6222(3) 0.8563(2) 0.0460(12) Uani 1 1 d . . .
C38 C -0.1863(3) 0.6697(3) 0.8828(3) 0.0584(15) Uani 1 1 d . . .
C39 C -0.1306(4) 0.7074(3) 0.9244(3) 0.0653(17) Uani 1 1 d . . .
C40 C -0.0426(3) 0.6962(3) 0.9375(2) 0.0477(12) Uani 1 1 d . . .
C41 C 0.0015(2) 0.7296(2) 0.71609(18) 0.0300(9) Uani 1 1 d . . .
C42 C -0.0637(3) 0.6975(2) 0.73113(19) 0.0367(10) Uani 1 1 d . . .
C43 C -0.1198(3) 0.6547(3) 0.6955(3) 0.0573(14) Uani 1 1 d . . .
C44 C -0.1148(4) 0.6424(3) 0.6418(3) 0.0692(18) Uani 1 1 d . . .
C45 C -0.0549(4) 0.6752(4) 0.6228(3) 0.0661(18) Uani 1 1 d . . .
C46 C 0.0021(3) 0.7177(2) 0.6599(2) 0.0416(11) Uani 1 1 d . . .
C47 C 0.0124(2) 0.8448(2) 0.76696(19) 0.0308(9) Uani 1 1 d . . .
C48 C -0.0187(3) 0.8625(2) 0.8124(2) 0.0377(10) Uani 1 1 d . . .
C49 C -0.0676(3) 0.9182(3) 0.8101(3) 0.0491(13) Uani 1 1 d . . .
C50 C -0.0868(3) 0.9584(2) 0.7635(3) 0.0567(16) Uani 1 1 d . . .
C51 C -0.0584(3) 0.9424(2) 0.7174(3) 0.0511(13) Uani 1 1 d . . .
C52 C -0.0107(3) 0.8869(2) 0.7203(2) 0.0393(10) Uani 1 1 d . . .
C53 C 0.5102(2) 0.63456(19) 0.83801(19) 0.0301(9) Uani 1 1 d . . .
C54 C 0.5340(3) 0.5943(2) 0.8872(2) 0.0383(10) Uani 1 1 d . . .
C55 C 0.5804(3) 0.5375(2) 0.8901(3) 0.0563(16) Uani 1 1 d . . .
C56 C 0.6074(3) 0.5190(3) 0.8443(3) 0.0619(18) Uani 1 1 d . . .
C57 C 0.5871(3) 0.5560(3) 0.7958(3) 0.0560(17) Uani 1 1 d . . .
C58 C 0.5391(3) 0.6125(2) 0.7932(2) 0.0374(10) Uani 1 1 d . . .
C59 C 0.5236(2) 0.75231(19) 0.88380(17) 0.0252(8) Uani 1 1 d . . .
C60 C 0.5881(3) 0.7815(2) 0.86545(19) 0.0328(9) Uani 1 1 d . . .
C61 C 0.6473(3) 0.8249(3) 0.8988(3) 0.0523(13) Uani 1 1 d . . .
C62 C 0.6445(4) 0.8402(3) 0.9524(3) 0.0670(18) Uani 1 1 d . . .
C63 C 0.5844(4) 0.8100(3) 0.9734(2) 0.0580(15) Uani 1 1 d . . .
C64 C 0.5259(3) 0.7678(2) 0.93941(19) 0.0366(10) Uani 1 1 d . . .
B1 B 0.4225(3) 0.8271(3) 0.6702(2) 0.0337(10) Uani 1 1 d . . .
B2 B 0.4605(3) 0.7014(2) 0.83944(19) 0.0244(9) Uani 1 1 d . . .
B3 B 0.0974(3) 0.6435(3) 0.9288(2) 0.0330(10) Uani 1 1 d . . .
B4 B 0.0639(3) 0.7787(2) 0.76282(19) 0.0244(9) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0260(5) 0.0354(6) 0.0341(6) -0.0036(4) 0.0122(4) -0.0089(4)
P2 0.0164(4) 0.0310(5) 0.0263(5) -0.0025(4) 0.0091(4) -0.0008(4)
P3 0.0229(5) 0.0310(5) 0.0326(5) -0.0035(4) 0.0126(4) -0.0054(4)
P4 0.0161(4) 0.0353(6) 0.0220(5) -0.0006(4) 0.0076(4) 0.0019(4)
F1 0.053(2) 0.089(3) 0.079(3) 0.043(2) -0.0204(18) -0.0235(19)
F2 0.080(3) 0.112(3) 0.087(3) 0.047(2) -0.045(2) -0.026(2)
F3 0.0567(18) 0.083(2) 0.0475(18) 0.0327(16) 0.0087(15) 0.0204(16)
F4 0.084(3) 0.082(3) 0.065(2) 0.0390(19) 0.0083(19) -0.019(2)
F5 0.093(3) 0.098(3) 0.063(2) 0.042(2) -0.019(2) -0.047(2)
F6 0.0265(14) 0.063(2) 0.091(3) 0.0147(18) 0.0022(15) -0.0151(13)
F7 0.0219(15) 0.127(3) 0.117(3) 0.053(3) 0.0038(18) -0.0115(18)
F8 0.0331(19) 0.201(6) 0.180(5) 0.049(4) 0.057(3) 0.035(3)
F9 0.090(3) 0.221(7) 0.179(6) -0.028(5) 0.088(4) 0.053(4)
F10 0.062(2) 0.138(4) 0.077(3) -0.029(2) 0.043(2) 0.010(2)
F11 0.086(3) 0.059(2) 0.110(3) 0.025(2) -0.055(2) -0.026(2)
F12 0.139(4) 0.074(3) 0.083(3) -0.003(2) -0.063(3) 0.016(3)
F13 0.103(3) 0.135(4) 0.0395(19) 0.034(2) 0.0184(19) 0.069(3)
F14 0.071(3) 0.142(4) 0.102(3) 0.080(3) 0.015(2) -0.014(3)
F15 0.068(2) 0.103(3) 0.085(3) 0.045(2) -0.013(2) -0.043(2)
F16 0.0256(13) 0.0657(19) 0.0670(19) -0.0173(15) 0.0158(13) -0.0086(12)
F17 0.0231(13) 0.085(2) 0.077(2) 0.0019(17) 0.0062(14) -0.0173(14)
F18 0.0210(15) 0.105(3) 0.153(4) -0.010(3) 0.026(2) 0.0084(16)
F19 0.048(2) 0.105(3) 0.179(5) -0.059(3) 0.060(3) 0.000(2)
F20 0.0445(17) 0.087(2) 0.085(2) -0.0343(19) 0.0367(18) -0.0063(16)
F21 0.0272(13) 0.0707(19) 0.0394(15) 0.0038(13) 0.0122(11) -0.0142(12)
F22 0.052(2) 0.109(3) 0.083(3) -0.007(2) 0.0148(19) -0.051(2)
F23 0.078(3) 0.151(4) 0.100(3) -0.072(3) 0.018(2) -0.067(3)
F24 0.079(3) 0.197(5) 0.052(2) -0.067(3) 0.027(2) -0.059(3)
F25 0.0335(15) 0.104(2) 0.0345(16) -0.0156(15) 0.0163(13) -0.0156(15)
F26 0.0326(13) 0.0684(19) 0.0454(16) -0.0123(13) 0.0221(12) 0.0063(12)
F27 0.0441(17) 0.085(2) 0.088(3) -0.048(2) 0.0257(17) 0.0064(16)
F28 0.0398(17) 0.0426(18) 0.155(4) -0.032(2) 0.007(2) 0.0185(14)
F29 0.0481(19) 0.059(2) 0.115(3) 0.038(2) 0.012(2) 0.0173(15)
F30 0.0365(15) 0.0646(18) 0.0490(17) 0.0170(14) 0.0111(13) 0.0070(13)
F31 0.0331(14) 0.0571(17) 0.0511(18) 0.0203(13) 0.0094(13) 0.0059(12)
F32 0.0482(19) 0.0508(19) 0.150(4) 0.047(2) 0.006(2) 0.0119(15)
F33 0.0410(18) 0.0404(18) 0.197(5) -0.035(2) 0.013(2) 0.0131(14)
F34 0.0391(17) 0.101(3) 0.124(3) -0.076(3) 0.0316(19) 0.0011(17)
F35 0.0319(14) 0.090(2) 0.0454(17) -0.0214(15) 0.0179(13) 0.0037(14)
F36 0.0266(12) 0.0671(18) 0.0350(14) 0.0019(12) 0.0147(11) -0.0099(12)
F37 0.0523(19) 0.106(3) 0.087(3) -0.010(2) 0.0271(18) -0.053(2)
F38 0.083(3) 0.149(4) 0.113(4) -0.083(3) 0.033(3) -0.078(3)
F39 0.071(2) 0.171(4) 0.063(2) -0.073(3) 0.029(2) -0.053(3)
F40 0.0325(14) 0.089(2) 0.0353(16) -0.0144(13) 0.0164(12) -0.0141(13)
O1 0.0191(13) 0.0476(18) 0.0340(16) 0.0001(13) 0.0085(12) -0.0070(12)
O2 0.0275(14) 0.0471(18) 0.0301(15) 0.0059(12) 0.0136(12) 0.0055(12)
O3 0.0391(17) 0.0329(16) 0.0520(19) 0.0041(13) 0.0238(15) 0.0011(12)
O4 0.058(2) 0.050(2) 0.046(2) -0.0183(16) 0.0205(17) -0.0248(17)
O5 0.0236(13) 0.0368(16) 0.0288(15) -0.0058(11) 0.0055(11) 0.0042(11)
O6 0.0154(12) 0.0448(18) 0.0240(14) 0.0012(11) 0.0065(11) -0.0009(11)
O7 0.0203(13) 0.0406(17) 0.0323(16) 0.0033(12) 0.0104(12) -0.0057(11)
O8 0.0212(13) 0.0437(17) 0.0289(15) -0.0029(11) 0.0125(11) -0.0029(11)
O9 0.0344(16) 0.0380(17) 0.0422(18) 0.0083(13) 0.0197(14) 0.0038(12)
O10 0.0449(18) 0.0444(18) 0.0454(19) -0.0134(14) 0.0220(15) -0.0158(14)
O11 0.0272(14) 0.0295(15) 0.0347(16) -0.0071(11) 0.0087(12) -0.0021(11)
O12 0.0191(13) 0.0303(15) 0.0275(15) 0.0011(10) 0.0072(11) -0.0003(10)
N1 0.0184(15) 0.0339(19) 0.0313(18) -0.0033(13) 0.0092(14) -0.0060(13)
N2 0.0165(14) 0.0271(17) 0.0284(17) -0.0032(12) 0.0055(13) 0.0016(12)
N3 0.0153(14) 0.0285(17) 0.0256(17) -0.0030(12) 0.0080(13) -0.0007(11)
N4 0.0154(14) 0.0293(17) 0.0261(17) -0.0022(12) 0.0058(13) 0.0035(12)
N5 0.0155(14) 0.0269(17) 0.0257(16) -0.0018(12) 0.0070(12) 0.0000(12)
N6 0.0184(15) 0.0261(17) 0.0318(17) 0.0012(13) 0.0080(13) -0.0001(12)
C1 0.0165(17) 0.028(2) 0.029(2) -0.0018(15) 0.0068(15) -0.0011(14)
C2 0.0140(16) 0.039(2) 0.0188(17) -0.0031(15) 0.0060(14) -0.0009(14)
C3 0.0180(17) 0.025(2) 0.0240(18) -0.0003(14) 0.0058(15) 0.0010(14)
C4 0.0202(17) 0.028(2) 0.0238(18) -0.0024(14) 0.0070(15) -0.0047(14)
C5 0.041(3) 0.033(2) 0.082(4) 0.007(2) 0.028(3) 0.006(2)
C6 0.058(5) 0.246(13) 0.089(7) 0.028(7) 0.018(4) 0.058(6)
C7 0.082(4) 0.060(4) 0.073(4) -0.002(3) 0.034(4) 0.018(3)
C8 0.080(5) 0.083(5) 0.115(6) 0.004(4) 0.043(5) -0.002(4)
C9 0.074(4) 0.055(3) 0.037(3) -0.014(2) -0.006(3) 0.001(3)
C10 0.158(8) 0.067(4) 0.042(3) -0.003(3) 0.021(4) 0.039(5)
C11 0.041(3) 0.055(3) 0.060(3) 0.016(2) 0.025(2) 0.017(2)
C12 0.053(4) 0.231(12) 0.070(5) 0.015(6) 0.004(4) 0.044(6)
C13 0.042(3) 0.079(4) 0.040(3) -0.022(2) 0.018(2) -0.014(3)
C14 0.081(5) 0.063(4) 0.071(4) -0.007(3) 0.017(4) 0.018(3)
C15 0.058(3) 0.068(4) 0.043(3) -0.024(3) 0.005(3) -0.016(3)
C16 0.124(6) 0.063(4) 0.052(4) -0.017(3) 0.041(4) -0.005(4)
C17 0.027(2) 0.049(3) 0.036(2) 0.0112(18) 0.0163(18) 0.0057(18)
C18 0.031(2) 0.065(3) 0.038(3) 0.012(2) 0.005(2) 0.010(2)
C19 0.040(3) 0.070(4) 0.052(3) 0.016(3) -0.001(2) 0.008(2)
C20 0.038(3) 0.068(3) 0.035(3) 0.015(2) 0.007(2) 0.019(2)
C21 0.051(3) 0.050(3) 0.050(3) 0.015(2) 0.023(2) 0.002(2)
C22 0.041(3) 0.061(3) 0.038(3) 0.015(2) 0.006(2) -0.002(2)
C23 0.025(2) 0.068(3) 0.046(3) 0.020(2) 0.017(2) 0.003(2)
C24 0.031(2) 0.060(3) 0.071(4) 0.034(3) 0.019(2) 0.005(2)
C25 0.022(2) 0.098(5) 0.079(4) 0.048(4) 0.015(3) -0.002(3)
C26 0.039(3) 0.131(7) 0.117(7) 0.052(5) 0.045(4) 0.031(4)
C27 0.049(4) 0.140(7) 0.101(6) 0.011(5) 0.049(4) 0.028(4)
C28 0.042(3) 0.114(5) 0.071(4) 0.015(4) 0.040(3) 0.020(3)
C29 0.023(2) 0.056(3) 0.029(2) 0.0052(18) 0.0127(17) 0.0081(18)
C30 0.049(3) 0.037(3) 0.050(3) 0.002(2) 0.006(2) 0.012(2)
C31 0.074(4) 0.058(4) 0.045(3) -0.010(3) -0.022(3) 0.036(3)
C32 0.067(4) 0.089(5) 0.036(3) 0.022(3) 0.019(3) 0.045(3)
C33 0.048(3) 0.102(5) 0.054(4) 0.040(3) 0.023(3) 0.013(3)
C34 0.036(3) 0.086(4) 0.050(3) 0.018(3) 0.013(2) -0.007(3)
C35 0.0228(19) 0.047(3) 0.035(2) 0.0070(18) 0.0122(17) 0.0002(17)
C36 0.022(2) 0.050(3) 0.044(3) 0.008(2) 0.0108(19) -0.0087(18)
C37 0.027(2) 0.060(3) 0.054(3) 0.010(2) 0.016(2) -0.005(2)
C38 0.018(2) 0.072(4) 0.089(4) 0.010(3) 0.022(3) -0.001(2)
C39 0.042(3) 0.059(3) 0.109(5) -0.006(3) 0.045(3) 0.008(3)
C40 0.030(2) 0.057(3) 0.063(3) -0.012(2) 0.023(2) -0.007(2)
C41 0.0165(18) 0.039(2) 0.035(2) -0.0041(17) 0.0084(16) -0.0022(15)
C42 0.023(2) 0.051(3) 0.034(2) -0.0024(19) 0.0068(18) -0.0041(18)
C43 0.033(2) 0.074(4) 0.065(4) -0.012(3) 0.015(2) -0.023(2)
C44 0.044(3) 0.097(5) 0.062(4) -0.040(3) 0.009(3) -0.032(3)
C45 0.044(3) 0.111(5) 0.043(3) -0.035(3) 0.012(2) -0.019(3)
C46 0.027(2) 0.062(3) 0.036(2) -0.010(2) 0.0098(19) -0.009(2)
C47 0.0152(17) 0.036(2) 0.040(2) -0.0061(17) 0.0066(17) 0.0023(15)
C48 0.0155(18) 0.048(3) 0.048(3) -0.015(2) 0.0077(18) 0.0011(17)
C49 0.023(2) 0.057(3) 0.068(4) -0.033(3) 0.016(2) -0.004(2)
C50 0.018(2) 0.034(3) 0.104(5) -0.019(3) -0.001(3) 0.0075(18)
C51 0.021(2) 0.040(3) 0.083(4) 0.011(3) 0.003(2) 0.0063(18)
C52 0.0169(18) 0.046(3) 0.052(3) 0.002(2) 0.0052(19) -0.0010(17)
C53 0.0115(16) 0.029(2) 0.048(3) -0.0078(17) 0.0066(17) -0.0033(14)
C54 0.0179(18) 0.029(2) 0.062(3) 0.0048(19) 0.004(2) 0.0002(15)
C55 0.024(2) 0.030(3) 0.104(5) 0.008(3) 0.004(3) 0.0011(18)
C56 0.024(2) 0.034(3) 0.118(6) -0.021(3) 0.007(3) 0.0004(19)
C57 0.017(2) 0.056(3) 0.091(4) -0.046(3) 0.010(2) -0.004(2)
C58 0.0199(19) 0.047(3) 0.045(3) -0.019(2) 0.0091(18) -0.0031(17)
C59 0.0177(17) 0.027(2) 0.029(2) -0.0016(15) 0.0047(15) 0.0012(14)
C60 0.0195(18) 0.044(3) 0.033(2) -0.0016(18) 0.0054(16) -0.0075(16)
C61 0.033(2) 0.065(3) 0.058(3) -0.007(3) 0.014(2) -0.021(2)
C62 0.049(3) 0.080(4) 0.071(4) -0.041(3) 0.017(3) -0.041(3)
C63 0.049(3) 0.078(4) 0.049(3) -0.036(3) 0.018(3) -0.018(3)
C64 0.022(2) 0.053(3) 0.037(2) -0.0068(19) 0.0121(18) -0.0035(18)
B1 0.025(2) 0.048(3) 0.032(2) 0.011(2) 0.015(2) 0.000(2)
B2 0.0136(18) 0.036(2) 0.024(2) -0.0009(16) 0.0071(16) 0.0033(16)
B3 0.022(2) 0.046(3) 0.035(3) 0.005(2) 0.0138(19) -0.0034(19)
B4 0.0139(18) 0.031(2) 0.029(2) -0.0032(16) 0.0073(16) -0.0035(15)
_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 O1 1.512(3) . ?
P1 O3 1.533(3) . ?
P1 O4 1.534(3) . ?
P1 C1 1.765(4) . ?
P2 O12 1.507(3) . ?
P2 O8 1.512(3) . ?
P2 O11 1.540(3) . ?
P2 C3 1.776(4) . ?
P3 O7 1.517(3) . ?
P3 O9 1.528(3) . ?
P3 O10 1.540(3) . ?
P3 C4 1.767(4) . ?
P4 O6 1.510(3) . ?
P4 O2 1.512(3) . ?
P4 O5 1.537(3) . ?
P4 C2 1.775(4) . ?
F1 C18 1.344(6) . ?
F2 C19 1.349(7) . ?
F3 C20 1.343(5) . ?
F4 C21 1.339(6) . ?
F5 C22 1.350(6) . ?
F6 C24 1.341(7) . ?
F7 C25 1.353(8) . ?
F8 C26 1.351(7) . ?
F9 C27 1.354(10) . ?
F10 C28 1.331(8) . ?
F11 C30 1.320(6) . ?
F12 C31 1.320(7) . ?
F13 C32 1.346(6) . ?
F14 C33 1.365(7) . ?
F15 C34 1.363(7) . ?
F16 C36 1.330(6) . ?
F17 C37 1.342(6) . ?
F18 C38 1.353(5) . ?
F19 C39 1.350(7) . ?
F20 C40 1.352(6) . ?
F21 C42 1.348(5) . ?
F22 C43 1.360(6) . ?
F23 C44 1.342(6) . ?
F24 C45 1.338(7) . ?
F25 C46 1.350(5) . ?
F26 C48 1.333(6) . ?
F27 C49 1.354(6) . ?
F28 C50 1.343(5) . ?
F29 C51 1.345(7) . ?
F30 C52 1.360(6) . ?
F31 C54 1.328(6) . ?
F32 C55 1.342(7) . ?
F33 C56 1.333(6) . ?
F34 C57 1.334(7) . ?
F35 C58 1.353(6) . ?
F36 C60 1.337(5) . ?
F37 C61 1.352(6) . ?
F38 C62 1.340(6) . ?
F39 C63 1.342(6) . ?
F40 C64 1.361(5) . ?
O1 B1 1.538(6) . ?
O2 B1 1.493(6) . ?
O3 C5 1.467(6) . ?
O4 C7 1.618(8) . ?
O5 C9 1.472(6) . ?
O6 B2 1.501(5) . ?
O7 B3 1.510(6) . ?
O8 B3 1.517(6) . ?
O9 C11 1.489(5) . ?
O10 C13 1.450(6) . ?
O11 C15 1.489(6) . ?
O12 B4 1.515(5) . ?
N1 N2 1.336(5) . ?
N1 C1 1.360(5) . ?
N2 N3 1.337(4) . ?
N2 B4 1.571(5) . ?
N3 C2 1.343(5) . ?
N4 N5 1.336(4) . ?
N4 C3 1.339(5) . ?
N5 N6 1.328(5) . ?
N5 B2 1.595(5) . ?
N6 C4 1.340(5) . ?
C1 C2 1.401(6) . ?
C3 C4 1.414(5) . ?
C5 C6 1.447(11) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.427(9) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.440(9) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.480(10) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.476(8) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.509(8) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C22 1.371(7) . ?
C17 C18 1.379(7) . ?
C17 B1 1.638(6) . ?
C18 C19 1.385(7) . ?
C19 C20 1.367(8) . ?
C20 C21 1.358(8) . ?
C21 C22 1.379(7) . ?
C23 C24 1.367(8) . ?
C23 C28 1.398(9) . ?
C23 B1 1.616(6) . ?
C24 C25 1.397(7) . ?
C25 C26 1.386(12) . ?
C26 C27 1.311(12) . ?
C27 C28 1.399(8) . ?
C29 C30 1.368(7) . ?
C29 C34 1.401(7) . ?
C29 B3 1.615(6) . ?
C30 C31 1.395(8) . ?
C31 C32 1.349(10) . ?
C32 C33 1.398(10) . ?
C33 C34 1.368(7) . ?
C35 C40 1.371(7) . ?
C35 C36 1.382(6) . ?
C35 B3 1.629(6) . ?
C36 C37 1.395(6) . ?
C37 C38 1.347(8) . ?
C38 C39 1.374(9) . ?
C39 C40 1.386(7) . ?
C41 C46 1.389(6) . ?
C41 C42 1.390(6) . ?
C41 B4 1.623(6) . ?
C42 C43 1.369(7) . ?
C43 C44 1.354(8) . ?
C44 C45 1.376(8) . ?
C45 C46 1.389(7) . ?
C47 C52 1.384(6) . ?
C47 C48 1.394(6) . ?
C47 B4 1.618(6) . ?
C48 C49 1.388(7) . ?
C49 C50 1.359(9) . ?
C50 C51 1.374(9) . ?
C51 C52 1.370(7) . ?
C53 C58 1.386(6) . ?
C53 C54 1.408(6) . ?
C53 B2 1.602(6) . ?
C54 C55 1.381(7) . ?
C55 C56 1.367(9) . ?
C56 C57 1.356(10) . ?
C57 C58 1.391(7) . ?
C59 C64 1.376(6) . ?
C59 C60 1.393(5) . ?
C59 B2 1.624(6) . ?
C60 C61 1.381(6) . ?
C61 C62 1.352(8) . ?
C62 C63 1.379(8) . ?
C63 C64 1.365(7) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 P1 O3 110.04(17) . . ?
O1 P1 O4 109.93(19) . . ?
O3 P1 O4 107.8(2) . . ?
O1 P1 C1 107.24(17) . . ?
O3 P1 C1 111.33(18) . . ?
O4 P1 C1 110.55(18) . . ?
O12 P2 O8 111.69(16) . . ?
O12 P2 O11 109.73(16) . . ?
O8 P2 O11 110.83(17) . . ?
O12 P2 C3 108.56(16) . . ?
O8 P2 C3 107.29(17) . . ?
O11 P2 C3 108.64(17) . . ?
O7 P3 O9 108.88(16) . . ?
O7 P3 O10 112.50(18) . . ?
O9 P3 O10 106.41(19) . . ?
O7 P3 C4 107.66(18) . . ?
O9 P3 C4 111.80(18) . . ?
O10 P3 C4 109.65(17) . . ?
O6 P4 O2 112.26(16) . . ?
O6 P4 O5 109.98(16) . . ?
O2 P4 O5 110.80(16) . . ?
O6 P4 C2 108.15(16) . . ?
O2 P4 C2 107.18(17) . . ?
O5 P4 C2 108.32(17) . . ?
P1 O1 B1 136.3(3) . . ?
B1 O2 P4 132.4(3) . . ?
C5 O3 P1 124.0(3) . . ?
P1 O4 C7 118.0(3) . . ?
C9 O5 P4 123.2(3) . . ?
B2 O6 P4 141.3(3) . . ?
B3 O7 P3 134.5(3) . . ?
P2 O8 B3 134.5(3) . . ?
C11 O9 P3 122.7(3) . . ?
C13 O10 P3 126.4(3) . . ?
C15 O11 P2 123.3(3) . . ?
P2 O12 B4 140.3(2) . . ?
N2 N1 C1 103.8(3) . . ?
N1 N2 N3 115.0(3) . . ?
N1 N2 B4 124.6(3) . . ?
N3 N2 B4 120.3(3) . . ?
N2 N3 C2 104.4(3) . . ?
N5 N4 C3 104.3(3) . . ?
N6 N5 N4 114.9(3) . . ?
N6 N5 B2 123.5(3) . . ?
N4 N5 B2 121.3(3) . . ?
N5 N6 C4 104.6(3) . . ?
N1 C1 C2 108.3(3) . . ?
N1 C1 P1 124.1(3) . . ?
C2 C1 P1 127.6(3) . . ?
N3 C2 C1 108.6(3) . . ?
N3 C2 P4 122.4(3) . . ?
C1 C2 P4 128.8(3) . . ?
N4 C3 C4 108.2(3) . . ?
N4 C3 P2 124.3(3) . . ?
C4 C3 P2 127.3(3) . . ?
N6 C4 C3 108.0(3) . . ?
N6 C4 P3 122.1(3) . . ?
C3 C4 P3 129.9(3) . . ?
C6 C5 O3 108.4(5) . . ?
C6 C5 H5A 110.0 . . ?
O3 C5 H5A 110.0 . . ?
C6 C5 H5B 110.0 . . ?
O3 C5 H5B 110.0 . . ?
H5A C5 H5B 108.4 . . ?
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 . . ?
C8 C7 O4 103.1(5) . . ?
C8 C7 H7A 111.1 . . ?
O4 C7 H7A 111.1 . . ?
C8 C7 H7B 111.1 . . ?
O4 C7 H7B 111.1 . . ?
H7A C7 H7B 109.1 . . ?
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 O5 111.1(5) . . ?
C10 C9 H9A 109.4 . . ?
O5 C9 H9A 109.4 . . ?
C10 C9 H9B 109.4 . . ?
O5 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
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 O9 106.8(5) . . ?
C12 C11 H11A 110.4 . . ?
O9 C11 H11A 110.4 . . ?
C12 C11 H11B 110.4 . . ?
O9 C11 H11B 110.4 . . ?
H11A C11 H11B 108.6 . . ?
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 . . ?
O10 C13 C14 110.6(4) . . ?
O10 C13 H13A 109.5 . . ?
C14 C13 H13A 109.5 . . ?
O10 C13 H13B 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 108.1 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O11 C15 C16 109.0(5) . . ?
O11 C15 H15A 109.9 . . ?
C16 C15 H15A 109.9 . . ?
O11 C15 H15B 109.9 . . ?
C16 C15 H15B 109.9 . . ?
H15A C15 H15B 108.3 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C22 C17 C18 115.3(4) . . ?
C22 C17 B1 119.3(4) . . ?
C18 C17 B1 125.3(4) . . ?
F1 C18 C17 121.7(4) . . ?
F1 C18 C19 116.7(5) . . ?
C17 C18 C19 121.6(5) . . ?
F2 C19 C20 119.9(5) . . ?
F2 C19 C18 119.4(5) . . ?
C20 C19 C18 120.6(5) . . ?
F3 C20 C21 120.3(5) . . ?
F3 C20 C19 120.2(5) . . ?
C21 C20 C19 119.5(5) . . ?
F4 C21 C20 119.5(5) . . ?
F4 C21 C22 122.0(5) . . ?
C20 C21 C22 118.5(5) . . ?
F5 C22 C17 119.7(4) . . ?
F5 C22 C21 115.8(5) . . ?
C17 C22 C21 124.4(5) . . ?
C24 C23 C28 115.0(5) . . ?
C24 C23 B1 127.2(5) . . ?
C28 C23 B1 117.8(5) . . ?
F6 C24 C23 121.2(4) . . ?
F6 C24 C25 115.4(6) . . ?
C23 C24 C25 123.4(6) . . ?
F7 C25 C26 122.0(5) . . ?
F7 C25 C24 119.5(7) . . ?
C26 C25 C24 118.5(7) . . ?
C27 C26 F8 122.9(8) . . ?
C27 C26 C25 120.1(6) . . ?
F8 C26 C25 116.9(9) . . ?
C26 C27 F9 120.2(6) . . ?
C26 C27 C28 121.0(8) . . ?
F9 C27 C28 118.7(8) . . ?
F10 C28 C23 120.2(5) . . ?
F10 C28 C27 118.0(6) . . ?
C23 C28 C27 121.8(7) . . ?
C30 C29 C34 113.5(4) . . ?
C30 C29 B3 127.1(4) . . ?
C34 C29 B3 119.4(4) . . ?
F11 C30 C29 120.9(5) . . ?
F11 C30 C31 115.1(5) . . ?
C29 C30 C31 124.0(5) . . ?
F12 C31 C32 119.0(6) . . ?
F12 C31 C30 121.4(7) . . ?
C32 C31 C30 119.6(5) . . ?
F13 C32 C31 121.0(6) . . ?
F13 C32 C33 119.1(6) . . ?
C31 C32 C33 119.9(5) . . ?
F14 C33 C34 121.7(6) . . ?
F14 C33 C32 120.4(5) . . ?
C34 C33 C32 117.9(6) . . ?
F15 C34 C33 116.0(5) . . ?
F15 C34 C29 119.0(5) . . ?
C33 C34 C29 125.0(6) . . ?
C40 C35 C36 114.8(4) . . ?
C40 C35 B3 118.9(4) . . ?
C36 C35 B3 126.3(4) . . ?
F16 C36 C35 122.0(4) . . ?
F16 C36 C37 115.1(4) . . ?
C35 C36 C37 122.9(5) . . ?
F17 C37 C38 119.5(4) . . ?
F17 C37 C36 121.0(5) . . ?
C38 C37 C36 119.5(5) . . ?
C37 C38 F18 120.1(5) . . ?
C37 C38 C39 120.3(4) . . ?
F18 C38 C39 119.6(5) . . ?
F19 C39 C38 121.2(5) . . ?
F19 C39 C40 120.2(6) . . ?
C38 C39 C40 118.6(5) . . ?
F20 C40 C35 119.2(4) . . ?
F20 C40 C39 116.9(5) . . ?
C35 C40 C39 123.9(5) . . ?
C46 C41 C42 114.0(4) . . ?
C46 C41 B4 127.4(4) . . ?
C42 C41 B4 118.5(4) . . ?
F21 C42 C43 117.5(4) . . ?
F21 C42 C41 118.7(4) . . ?
C43 C42 C41 123.8(4) . . ?
C44 C43 F22 119.6(5) . . ?
C44 C43 C42 120.4(5) . . ?
F22 C43 C42 120.1(5) . . ?
F23 C44 C43 120.6(6) . . ?
F23 C44 C45 120.3(5) . . ?
C43 C44 C45 119.0(5) . . ?
F24 C45 C44 119.8(5) . . ?
F24 C45 C46 120.6(5) . . ?
C44 C45 C46 119.6(5) . . ?
F25 C46 C45 116.1(4) . . ?
F25 C46 C41 120.8(4) . . ?
C45 C46 C41 123.1(4) . . ?
C52 C47 C48 114.2(4) . . ?
C52 C47 B4 119.6(4) . . ?
C48 C47 B4 126.0(4) . . ?
F26 C48 C49 117.4(4) . . ?
F26 C48 C47 120.9(4) . . ?
C49 C48 C47 121.7(5) . . ?
F27 C49 C50 120.1(5) . . ?
F27 C49 C48 118.5(5) . . ?
C50 C49 C48 121.4(5) . . ?
F28 C50 C49 121.1(6) . . ?
F28 C50 C51 120.0(6) . . ?
C49 C50 C51 118.9(4) . . ?
F29 C51 C52 121.0(5) . . ?
F29 C51 C50 120.1(5) . . ?
C52 C51 C50 118.9(5) . . ?
F30 C52 C51 115.7(5) . . ?
F30 C52 C47 119.3(4) . . ?
C51 C52 C47 125.0(5) . . ?
C58 C53 C54 113.6(4) . . ?
C58 C53 B2 126.3(4) . . ?
C54 C53 B2 120.0(4) . . ?
F31 C54 C55 117.3(5) . . ?
F31 C54 C53 119.4(4) . . ?
C55 C54 C53 123.3(5) . . ?
F32 C55 C56 120.3(5) . . ?
F32 C55 C54 119.7(6) . . ?
C56 C55 C54 120.0(6) . . ?
F33 C56 C57 120.0(6) . . ?
F33 C56 C55 120.4(7) . . ?
C57 C56 C55 119.6(5) . . ?
F34 C57 C56 120.7(5) . . ?
F34 C57 C58 119.5(6) . . ?
C56 C57 C58 119.8(5) . . ?
F35 C58 C53 120.4(4) . . ?
F35 C58 C57 115.9(4) . . ?
C53 C58 C57 123.8(5) . . ?
C64 C59 C60 114.5(4) . . ?
C64 C59 B2 128.5(4) . . ?
C60 C59 B2 116.9(3) . . ?
F36 C60 C61 116.8(4) . . ?
F36 C60 C59 119.8(4) . . ?
C61 C60 C59 123.4(4) . . ?
F37 C61 C62 120.5(5) . . ?
F37 C61 C60 119.9(5) . . ?
C62 C61 C60 119.6(5) . . ?
F38 C62 C61 120.6(5) . . ?
F38 C62 C63 120.4(6) . . ?
C61 C62 C63 118.9(4) . . ?
F39 C63 C64 121.2(5) . . ?
F39 C63 C62 118.4(5) . . ?
C64 C63 C62 120.4(5) . . ?
F40 C64 C63 116.6(4) . . ?
F40 C64 C59 120.3(4) . . ?
C63 C64 C59 123.1(4) . . ?
O2 B1 O1 106.5(3) . . ?
O2 B1 C23 108.1(4) . . ?
O1 B1 C23 109.5(4) . . ?
O2 B1 C17 111.7(4) . . ?
O1 B1 C17 108.8(4) . . ?
C23 B1 C17 112.1(3) . . ?
O6 B2 N5 104.5(3) . . ?
O6 B2 C53 113.6(3) . . ?
N5 B2 C53 109.4(3) . . ?
O6 B2 C59 106.9(3) . . ?
N5 B2 C59 112.0(3) . . ?
C53 B2 C59 110.4(3) . . ?
O7 B3 O8 106.9(3) . . ?
O7 B3 C29 109.8(4) . . ?
O8 B3 C29 110.0(4) . . ?
O7 B3 C35 109.3(4) . . ?
O8 B3 C35 108.0(3) . . ?
C29 B3 C35 112.6(3) . . ?
O12 B4 N2 104.5(3) . . ?
O12 B4 C47 112.6(3) . . ?
N2 B4 C47 111.2(3) . . ?
O12 B4 C41 106.6(3) . . ?
N2 B4 C41 111.8(3) . . ?
C47 B4 C41 110.0(3) . . ?
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.062
_iucr_refine_instructions_details 
;
TITL d12293a in Cc
CELL 0.71073 16.2500 20.5944 24.2619 90.000 107.673 90.000
ZERR 4 0.0022 0.0030 0.0039 0.000 0.003 0.000
LATT -7
SYMM X, -Y, 0.5+Z
SFAC C H B N O F P
UNIT 256 120 16 24 48 160 16
TEMP -126.160
SIZE 0.13 0.18 0.22
ACTA
L.S. 4
BOND $H
PLAN 20
FMAP 2
WGHT 0.054100 18.477797
FVAR 0.05733
P1 7 0.328258 0.903738 0.727009 11.00000 0.02600 0.03536 =
0.03412 -0.00362 0.01219 -0.00889
P2 7 0.161862 0.745104 0.877666 11.00000 0.01642 0.03101 =
0.02634 -0.00248 0.00915 -0.00082
P3 7 0.205325 0.572121 0.881245 11.00000 0.02294 0.03097 =
0.03260 -0.00352 0.01264 -0.00542
P4 7 0.358666 0.731092 0.724618 11.00000 0.01614 0.03528 =
0.02203 -0.00063 0.00755 0.00190
F1 6 0.264328 0.781239 0.574935 11.00000 0.05265 0.08926 =
0.07873 0.04271 -0.02043 -0.02351
F2 6 0.196371 0.842263 0.475201 11.00000 0.07987 0.11161 =
0.08680 0.04730 -0.04474 -0.02637
F3 6 0.268828 0.952647 0.449734 11.00000 0.05672 0.08342 =
0.04752 0.03269 0.00870 0.02038
F4 6 0.408227 1.003972 0.528321 11.00000 0.08388 0.08217 =
0.06488 0.03903 0.00826 -0.01949
F5 6 0.477233 0.944924 0.630229 11.00000 0.09286 0.09772 =
0.06290 0.04184 -0.01907 -0.04744
F6 6 0.572142 0.900513 0.752860 11.00000 0.02653 0.06340 =
0.09145 0.01468 0.00217 -0.01505
F7 6 0.737226 0.876254 0.769191 11.00000 0.02195 0.12665 =
0.11671 0.05324 0.00375 -0.01154
F8 6 0.786052 0.777866 0.711460 11.00000 0.03310 0.20143 =
0.18040 0.04908 0.05666 0.03473
F9 6 0.663549 0.707872 0.631849 11.00000 0.09017 0.22134 =
0.17894 -0.02835 0.08776 0.05304
F10 6 0.496161 0.734697 0.612468 11.00000 0.06219 0.13755 =
0.07679 -0.02884 0.04261 0.00970
F11 6 0.244980 0.695149 1.027845 11.00000 0.08559 0.05902 =
0.11047 0.02535 -0.05488 -0.02604
F12 6 0.304122 0.641632 1.131419 11.00000 0.13896 0.07378 =
0.08287 -0.00312 -0.06254 0.01568
F13 6 0.233135 0.533054 1.157833 11.00000 0.10286 0.13501 =
0.03950 0.03353 0.01844 0.06890
F14 6 0.103402 0.471761 1.074782 11.00000 0.07060 0.14219 =
0.10245 0.08025 0.01469 -0.01401
F15 6 0.044685 0.524522 0.968882 11.00000 0.06798 0.10346 =
0.08542 0.04509 -0.01335 -0.04329
F16 6 -0.042338 0.566069 0.840667 11.00000 0.02558 0.06567 =
0.06702 -0.01734 0.01583 -0.00858
F17 6 -0.211063 0.583978 0.817627 11.00000 0.02314 0.08510 =
0.07656 0.00189 0.00617 -0.01729
F18 6 -0.272360 0.680238 0.868784 11.00000 0.02096 0.10464 =
0.15348 -0.00954 0.02621 0.00836
F19 6 -0.160139 0.754217 0.952443 11.00000 0.04794 0.10534 =
0.17857 -0.05924 0.05968 -0.00040
F20 6 0.010071 0.733248 0.979651 11.00000 0.04452 0.08723 =
0.08477 -0.03430 0.03670 -0.00632
F21 6 -0.073221 0.708874 0.783585 11.00000 0.02725 0.07073 =
0.03944 0.00378 0.01221 -0.01421
F22 6 -0.180585 0.624051 0.714155 11.00000 0.05238 0.10878 =
0.08344 -0.00749 0.01481 -0.05132
F23 6 -0.168914 0.599815 0.607046 11.00000 0.07772 0.15063 =
0.10039 -0.07238 0.01845 -0.06682
F24 6 -0.052653 0.666460 0.568649 11.00000 0.07869 0.19739 =
0.05166 -0.06710 0.02705 -0.05860
F25 6 0.059882 0.747333 0.638409 11.00000 0.03349 0.10399 =
0.03454 -0.01563 0.01626 -0.01557
F26 6 -0.003803 0.825542 0.859513 11.00000 0.03265 0.06835 =
0.04537 -0.01227 0.02213 0.00631
F27 6 -0.095275 0.932673 0.856020 11.00000 0.04414 0.08514 =
0.08789 -0.04798 0.02569 0.00640
F28 6 -0.133294 1.012657 0.761837 11.00000 0.03977 0.04263 =
0.15481 -0.03227 0.00685 0.01852
F29 6 -0.076475 0.981287 0.670706 11.00000 0.04806 0.05856 =
0.11506 0.03783 0.01230 0.01731
F30 6 0.012336 0.872725 0.672244 11.00000 0.03655 0.06463 =
0.04901 0.01700 0.01113 0.00698
F31 6 0.513058 0.611376 0.933942 11.00000 0.03311 0.05712 =
0.05107 0.02026 0.00942 0.00592
F32 6 0.600115 0.501394 0.938422 11.00000 0.04815 0.05075 =
0.14993 0.04711 0.00599 0.01190
F33 6 0.652916 0.464558 0.846978 11.00000 0.04096 0.04040 =
0.19736 -0.03451 0.01344 0.01311
F34 6 0.611669 0.538424 0.750321 11.00000 0.03913 0.10145 =
0.12448 -0.07562 0.03165 0.00106
F35 6 0.522913 0.647055 0.743536 11.00000 0.03193 0.08981 =
0.04538 -0.02139 0.01788 0.00367
F36 6 0.596125 0.766490 0.813736 11.00000 0.02656 0.06707 =
0.03504 0.00194 0.01469 -0.00990
F37 6 0.707001 0.852266 0.877514 11.00000 0.05227 0.10601 =
0.08746 -0.01025 0.02705 -0.05289
F38 6 0.701541 0.882097 0.985585 11.00000 0.08285 0.14854 =
0.11306 -0.08272 0.03253 -0.07783
F39 6 0.584661 0.823591 1.027523 11.00000 0.07135 0.17074 =
0.06286 -0.07332 0.02906 -0.05275
F40 6 0.468437 0.740528 0.963307 11.00000 0.03245 0.08939 =
0.03535 -0.01438 0.01645 -0.01411
O1 5 0.405742 0.870840 0.717052 11.00000 0.01911 0.04762 =
0.03403 0.00011 0.00852 -0.00696
O2 5 0.384819 0.762289 0.676059 11.00000 0.02746 0.04706 =
0.03007 0.00587 0.01360 0.00548
O3 5 0.284991 0.948714 0.676132 11.00000 0.03909 0.03293 =
0.05197 0.00408 0.02375 0.00111
O4 5 0.356992 0.945461 0.781917 11.00000 0.05833 0.05024 =
0.04611 -0.01832 0.02049 -0.02484
O5 5 0.331554 0.660089 0.710138 11.00000 0.02358 0.03678 =
0.02884 -0.00577 0.00546 0.00417
O6 5 0.429399 0.734668 0.781747 11.00000 0.01535 0.04476 =
0.02399 0.00116 0.00646 -0.00091
O7 5 0.121347 0.600321 0.885769 11.00000 0.02033 0.04058 =
0.03231 0.00328 0.01036 -0.00565
O8 5 0.133969 0.710332 0.923915 11.00000 0.02121 0.04367 =
0.02890 -0.00293 0.01254 -0.00287
O9 5 0.249599 0.534606 0.936644 11.00000 0.03437 0.03801 =
0.04222 0.00832 0.01970 0.00377
O10 5 0.190927 0.523286 0.831124 11.00000 0.04493 0.04438 =
0.04542 -0.01338 0.02200 -0.01577
O11 5 0.184919 0.816390 0.894699 11.00000 0.02720 0.02945 =
0.03470 -0.00715 0.00865 -0.00207
O12 5 0.093138 0.742307 0.819748 11.00000 0.01913 0.03035 =
0.02750 0.00111 0.00715 -0.00034
N1 4 0.181250 0.853051 0.745666 11.00000 0.01844 0.03387 =
0.03127 -0.00330 0.00920 -0.00598
N2 4 0.149639 0.793603 0.748016 11.00000 0.01650 0.02712 =
0.02835 -0.00320 0.00552 0.00159
N3 4 0.199243 0.745004 0.739851 11.00000 0.01532 0.02855 =
0.02564 -0.00305 0.00796 -0.00070
N4 4 0.323246 0.735338 0.862678 11.00000 0.01536 0.02928 =
0.02615 -0.00221 0.00578 0.00355
N5 4 0.374721 0.687196 0.856303 11.00000 0.01552 0.02693 =
0.02572 -0.00181 0.00697 0.00001
N6 4 0.344903 0.627825 0.860023 11.00000 0.01845 0.02607 =
0.03180 0.00117 0.00804 -0.00015
C1 1 0.257123 0.841950 0.734467 11.00000 0.01647 0.02771 =
0.02893 -0.00178 0.00683 -0.00113
C2 1 0.268020 0.774703 0.731454 11.00000 0.01404 0.03878 =
0.01880 -0.00314 0.00601 -0.00089
C3 1 0.255628 0.705034 0.871795 11.00000 0.01795 0.02500 =
0.02401 -0.00026 0.00580 0.00101
C4 1 0.269560 0.637358 0.870638 11.00000 0.02015 0.02833 =
0.02384 -0.00243 0.00703 -0.00471
C5 1 0.204260 0.984001 0.669950 11.00000 0.04083 0.03296 =
0.08188 0.00720 0.02763 0.00591
AFIX 23
H5A 2 0.169720 0.961147 0.691262 11.00000 -1.20000
H5B 2 0.217058 1.028302 0.686125 11.00000 -1.20000
AFIX 0
C6 1 0.156391 0.987467 0.609064 11.00000 0.05820 0.24564 =
0.08928 0.02796 0.01791 0.05782
AFIX 33
H6A 2 0.102047 1.010763 0.604162 11.00000 -1.50000
H6B 2 0.143933 0.943440 0.593428 11.00000 -1.50000
H6C 2 0.190779 1.010545 0.588376 11.00000 -1.50000
AFIX 0
C7 1 0.415954 0.911697 0.840945 11.00000 0.08227 0.06012 =
0.07257 -0.00189 0.03405 0.01758
AFIX 23
H7A 2 0.420451 0.864260 0.835905 11.00000 -1.20000
H7B 2 0.474701 0.930657 0.853581 11.00000 -1.20000
AFIX 0
C8 1 0.370205 0.925933 0.881255 11.00000 0.08039 0.08323 =
0.11504 0.00379 0.04265 -0.00211
AFIX 33
H8A 2 0.400948 0.906975 0.918934 11.00000 -1.50000
H8B 2 0.311944 0.907502 0.867303 11.00000 -1.50000
H8C 2 0.366307 0.973098 0.885210 11.00000 -1.50000
AFIX 0
C9 1 0.271958 0.639503 0.654085 11.00000 0.07393 0.05528 =
0.03673 -0.01445 -0.00615 0.00116
AFIX 23
H9A 2 0.233683 0.604781 0.660437 11.00000 -1.20000
H9B 2 0.235312 0.676686 0.635593 11.00000 -1.20000
AFIX 0
C10 1 0.318563 0.615916 0.616248 11.00000 0.15822 0.06723 =
0.04191 -0.00313 0.02108 0.03859
AFIX 33
H10A 2 0.277492 0.602249 0.579436 11.00000 -1.50000
H10B 2 0.354476 0.578863 0.634373 11.00000 -1.50000
H10C 2 0.355434 0.650585 0.609189 11.00000 -1.50000
AFIX 0
C11 1 0.333798 0.500795 0.946356 11.00000 0.04058 0.05465 =
0.06042 0.01585 0.02539 0.01703
AFIX 23
H11A 2 0.324606 0.453567 0.939640 11.00000 -1.20000
H11B 2 0.364137 0.517744 0.919614 11.00000 -1.20000
AFIX 0
C12 1 0.385197 0.513426 1.007104 11.00000 0.05292 0.23081 =
0.06968 0.01527 0.00417 0.04440
AFIX 33
H12A 2 0.441365 0.491802 1.015390 11.00000 -1.50000
H12B 2 0.354340 0.496545 1.033055 11.00000 -1.50000
H12C 2 0.393923 0.560295 1.013095 11.00000 -1.50000
AFIX 0
C13 1 0.172670 0.538934 0.770310 11.00000 0.04232 0.07883 =
0.03984 -0.02223 0.01778 -0.01367
AFIX 23
H13A 2 0.184833 0.500641 0.749368 11.00000 -1.20000
H13B 2 0.210745 0.574806 0.765907 11.00000 -1.20000
AFIX 0
C14 1 0.081495 0.558364 0.745018 11.00000 0.08136 0.06289 =
0.07064 -0.00706 0.01740 0.01751
AFIX 33
H14A 2 0.070494 0.569027 0.704047 11.00000 -1.50000
H14B 2 0.069618 0.596472 0.765576 11.00000 -1.50000
H14C 2 0.043852 0.522490 0.748642 11.00000 -1.50000
AFIX 0
C15 1 0.232343 0.837326 0.954708 11.00000 0.05837 0.06781 =
0.04343 -0.02397 0.00454 -0.01617
AFIX 23
H15A 2 0.266674 0.876753 0.953627 11.00000 -1.20000
H15B 2 0.272401 0.802604 0.974804 11.00000 -1.20000
AFIX 0
C16 1 0.167987 0.851433 0.986786 11.00000 0.12447 0.06258 =
0.05180 -0.01663 0.04142 -0.00529
AFIX 33
H16A 2 0.198779 0.864964 1.026416 11.00000 -1.50000
H16B 2 0.134296 0.812217 0.987755 11.00000 -1.50000
H16C 2 0.129100 0.886280 0.967014 11.00000 -1.50000
AFIX 0
C17 1 0.376305 0.859539 0.606715 11.00000 0.02749 0.04896 =
0.03572 0.01120 0.01625 0.00570
C18 1 0.303472 0.835978 0.566053 11.00000 0.03089 0.06541 =
0.03824 0.01162 0.00468 0.01024
C19 1 0.267824 0.867058 0.513565 11.00000 0.03986 0.06972 =
0.05188 0.01592 -0.00107 0.00829
C20 1 0.303309 0.923193 0.500975 11.00000 0.03824 0.06759 =
0.03523 0.01516 0.00725 0.01907
C21 1 0.374384 0.948415 0.540285 11.00000 0.05122 0.05016 =
0.05040 0.01498 0.02291 0.00218
C22 1 0.408456 0.916357 0.592110 11.00000 0.04075 0.06057 =
0.03791 0.01466 0.00584 -0.00216
C23 1 0.525370 0.818121 0.682755 11.00000 0.02492 0.06789 =
0.04622 0.01989 0.01719 0.00269
C24 1 0.589913 0.852237 0.721144 11.00000 0.03050 0.05998 =
0.07098 0.03387 0.01920 0.00523
C25 1 0.677592 0.839614 0.730744 11.00000 0.02179 0.09850 =
0.07909 0.04750 0.01472 -0.00151
C26 1 0.700713 0.789410 0.700391 11.00000 0.03879 0.13135 =
0.11675 0.05182 0.04531 0.03072
C27 1 0.641054 0.756427 0.662053 11.00000 0.04899 0.14001 =
0.10098 0.01084 0.04855 0.02828
C28 1 0.553330 0.769137 0.652757 11.00000 0.04208 0.11415 =
0.07103 0.01500 0.03966 0.02044
C29 1 0.139302 0.615412 0.993475 11.00000 0.02312 0.05617 =
0.02924 0.00520 0.01270 0.00807
C30 1 0.206619 0.641234 1.036399 11.00000 0.04909 0.03660 =
0.04996 0.00217 0.00594 0.01185
C31 1 0.239421 0.614323 1.091497 11.00000 0.07351 0.05840 =
0.04484 -0.00973 -0.02247 0.03576
C32 1 0.204189 0.559430 1.104678 11.00000 0.06689 0.08943 =
0.03647 0.02205 0.01916 0.04509
C33 1 0.136794 0.528958 1.062697 11.00000 0.04759 0.10217 =
0.05414 0.04027 0.02313 0.01250
C34 1 0.107304 0.557533 1.009396 11.00000 0.03596 0.08575 =
0.04997 0.01778 0.01271 -0.00707
C35 1 -0.007284 0.649779 0.911070 11.00000 0.02276 0.04733 =
0.03475 0.00700 0.01222 0.00022
C36 1 -0.066589 0.612523 0.870505 11.00000 0.02186 0.04967 =
0.04397 0.00805 0.01079 -0.00868
C37 1 -0.155556 0.622164 0.856335 11.00000 0.02724 0.05961 =
0.05358 0.01020 0.01580 -0.00464
C38 1 -0.186261 0.669700 0.882793 11.00000 0.01792 0.07173 =
0.08932 0.01039 0.02178 -0.00054
C39 1 -0.130574 0.707407 0.924409 11.00000 0.04241 0.05922 =
0.10886 -0.00644 0.04472 0.00770
C40 1 -0.042621 0.696223 0.937517 11.00000 0.02966 0.05707 =
0.06252 -0.01168 0.02309 -0.00730
C41 1 0.001538 0.729648 0.716094 11.00000 0.01647 0.03907 =
0.03493 -0.00408 0.00839 -0.00220
C42 1 -0.063732 0.697495 0.731134 11.00000 0.02314 0.05135 =
0.03426 -0.00240 0.00683 -0.00410
C43 1 -0.119788 0.654748 0.695543 11.00000 0.03262 0.07422 =
0.06534 -0.01150 0.01512 -0.02305
C44 1 -0.114831 0.642355 0.641836 11.00000 0.04355 0.09704 =
0.06247 -0.03959 0.00910 -0.03166
C45 1 -0.054914 0.675220 0.622795 11.00000 0.04375 0.11084 =
0.04325 -0.03521 0.01237 -0.01920
C46 1 0.002101 0.717736 0.659874 11.00000 0.02732 0.06151 =
0.03616 -0.01014 0.00979 -0.00887
C47 1 0.012401 0.844831 0.766963 11.00000 0.01519 0.03624 =
0.03972 -0.00608 0.00657 0.00233
C48 1 -0.018738 0.862492 0.812409 11.00000 0.01547 0.04823 =
0.04816 -0.01459 0.00772 0.00113
C49 1 -0.067608 0.918244 0.810132 11.00000 0.02284 0.05717 =
0.06832 -0.03254 0.01554 -0.00437
C50 1 -0.086794 0.958389 0.763511 11.00000 0.01849 0.03443 =
0.10375 -0.01890 -0.00144 0.00755
C51 1 -0.058363 0.942394 0.717410 11.00000 0.02115 0.04022 =
0.08313 0.01109 0.00287 0.00630
C52 1 -0.010744 0.886881 0.720302 11.00000 0.01690 0.04606 =
0.05154 0.00192 0.00517 -0.00103
C53 1 0.510173 0.634561 0.838011 11.00000 0.01149 0.02874 =
0.04836 -0.00784 0.00661 -0.00326
C54 1 0.534048 0.594268 0.887179 11.00000 0.01794 0.02878 =
0.06239 0.00484 0.00363 0.00019
C55 1 0.580360 0.537501 0.890097 11.00000 0.02448 0.03009 =
0.10418 0.00810 0.00440 0.00112
C56 1 0.607442 0.518990 0.844346 11.00000 0.02404 0.03406 =
0.11770 -0.02136 0.00671 0.00043
C57 1 0.587082 0.556014 0.795843 11.00000 0.01717 0.05565 =
0.09099 -0.04605 0.01006 -0.00449
C58 1 0.539136 0.612544 0.793164 11.00000 0.01991 0.04669 =
0.04514 -0.01918 0.00913 -0.00314
C59 1 0.523611 0.752315 0.883798 11.00000 0.01767 0.02740 =
0.02909 -0.00159 0.00474 0.00125
C60 1 0.588052 0.781529 0.865448 11.00000 0.01948 0.04411 =
0.03296 -0.00156 0.00537 -0.00752
C61 1 0.647306 0.824921 0.898796 11.00000 0.03316 0.06524 =
0.05843 -0.00720 0.01389 -0.02079
C62 1 0.644543 0.840220 0.952416 11.00000 0.04892 0.07977 =
0.07118 -0.04051 0.01670 -0.04128
C63 1 0.584445 0.810007 0.973384 11.00000 0.04858 0.07817 =
0.04939 -0.03558 0.01790 -0.01803
C64 1 0.525882 0.767825 0.939414 11.00000 0.02190 0.05347 =
0.03662 -0.00679 0.01208 -0.00354
B1 3 0.422510 0.827095 0.670230 11.00000 0.02497 0.04811 =
0.03230 0.01131 0.01516 -0.00007
B2 3 0.460495 0.701449 0.839441 11.00000 0.01365 0.03626 =
0.02419 -0.00089 0.00707 0.00326
B3 3 0.097448 0.643531 0.928849 11.00000 0.02173 0.04623 =
0.03459 0.00485 0.01380 -0.00344
B4 3 0.063925 0.778696 0.762824 11.00000 0.01386 0.03104 =
0.02896 -0.00321 0.00733 -0.00352
HKLF 4
REM d12293a in Cc
REM R1 = 0.0528 for 12817 Fo > 4sig(Fo) and 0.0680 for all 15431 data
REM 1171 parameters refined using 2 restraints
END
WGHT 0.0488 19.3725
REM Highest difference peak 0.660, deepest hole -0.436, 1-sigma level 0.062
Q1 1 0.0242 0.5693 0.9955 11.00000 0.05 0.66
Q2 1 0.3558 0.9391 0.8356 11.00000 0.05 0.65
Q3 1 0.0954 0.5222 1.0997 11.00000 0.05 0.60
Q4 1 0.3388 0.6336 1.1039 11.00000 0.05 0.49
Q5 1 0.2682 0.6782 1.0000 11.00000 0.05 0.48
Q6 1 0.2826 0.6390 1.1322 11.00000 0.05 0.44
Q7 1 0.0941 0.5974 1.0200 11.00000 0.05 0.44
Q8 1 0.0372 0.9125 1.0005 11.00000 0.05 0.40
Q9 1 0.4715 0.5998 0.5980 11.00000 0.05 0.40
Q10 1 0.2441 0.6021 0.8806 11.00000 0.05 0.39
Q11 1 0.2550 0.8195 0.6015 11.00000 0.05 0.38
Q12 1 0.2281 0.7011 1.0319 11.00000 0.05 0.37
Q13 1 0.0598 0.5161 0.9665 11.00000 0.05 0.36
Q14 1 0.3156 0.9656 0.7769 11.00000 0.05 0.33
Q15 1 0.4504 0.9296 0.8720 11.00000 0.05 0.33
Q16 1 0.1869 0.8801 0.5004 11.00000 0.05 0.32
Q17 1 0.4177 0.9635 0.5000 11.00000 0.05 0.32
Q18 1 0.1194 0.5669 0.7775 11.00000 0.05 0.32
Q19 1 0.2200 0.6008 0.6377 11.00000 0.05 0.32
Q20 1 0.1340 0.5729 1.0797 11.00000 0.05 0.32
;
_vrf_PLAT213_d12293a             
;
PROBLEM: Atom F8 has ADP max/min Ratio ..... 4.1 oblat
RESPONSE: Several of the terminla F atoms have larger then normal
anisotripc displacement parameters with the ellipsoids having a greater
magnitude in one direction. This was not deemed severe enough to model
as disorder.
;
# end Validation Reply Form
_vrf_PLAT220_d12293a             
;
PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.9 Ratio
RESPONSE:
See above which applies to benzene ring C atoms also.
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# end Validation Reply Form