data_2009src0115

#Dr. M. A. Beckett
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C38 H52 B12 O27 P2'
_chemical_formula_weight          1132.46
 
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'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P'  'P'   0.1023   0.0942
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            triclinic
_symmetry_space_group_name_H-M    P-1
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    10.1076(10)
_cell_length_b                    13.0403(10)
_cell_length_c                    20.6260(15)
_cell_angle_alpha                 84.364(5)
_cell_angle_beta                  82.811(4)
_cell_angle_gamma                 76.492(4)
_cell_volume                      2615.9(4)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     1919
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        'Cut Block'
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.20
_exptl_crystal_size_mid           0.13
_exptl_crystal_size_min           0.07
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.438
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1172
_exptl_absorpt_coefficient_mu     0.172
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9665
_exptl_absorpt_correction_T_max   0.9881
_exptl_absorpt_process_details       'SADABS 2007/2 (Sheldrick, G.M., 2007)'

_exptl_special_details
;
SADABS was used to perform the Absorption correction
Parameter refinement on 30032 reflections reduced R(int) from 0.1230 to 0.0701
Ratio of minimum to maximum apparent transmission: 0.837756
The given Tmin and Tmax were generated using the SHELX SIZE command
;

_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    '10cm confocal mirrors'
_diffrn_measurement_device_type   
'Bruker-Nonius APEX II CCD camera on κ-goniostat'
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   '4096x4096pixels / 62x62mm'
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             35223
_diffrn_reflns_av_R_equivalents   0.0655
_diffrn_reflns_av_sigmaI/netI     0.0665
_diffrn_reflns_limit_h_min        -13
_diffrn_reflns_limit_h_max        13
_diffrn_reflns_limit_k_min        -16
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -26
_diffrn_reflns_limit_l_max        26
_diffrn_reflns_theta_min          2.99
_diffrn_reflns_theta_max          27.48
_reflns_number_total              11835
_reflns_number_gt                 8892
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997b)' 
_computing_molecular_graphics     'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material   'WinGX (Farrugia, 1999)'
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0323P)²+7.2955P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          11835
_refine_ls_number_parameters      739
_refine_ls_number_restraints      3
_refine_ls_R_factor_all           0.1042
_refine_ls_R_factor_gt            0.0749
_refine_ls_wR_factor_ref          0.1730
_refine_ls_wR_factor_gt           0.1527
_refine_ls_goodness_of_fit_ref    1.047
_refine_ls_restrained_S_all       1.047
_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
B1 B 0.0724(3) 0.9085(3) 0.13534(16) 0.0181(6) Uani 1 1 d . . .
B2 B 0.0496(3) 1.0658(3) 0.19709(16) 0.0188(7) Uani 1 1 d . . .
B3 B 0.2684(3) 0.9788(3) 0.15280(16) 0.0188(7) Uani 1 1 d . . .
B4 B -0.0438(4) 0.7598(3) 0.14879(16) 0.0206(7) Uani 1 1 d . . .
B5 B -0.0654(4) 0.8746(3) 0.05154(17) 0.0239(7) Uani 1 1 d . . .
O1 O -0.0072(2) 0.99659(16) 0.17343(10) 0.0198(4) Uani 1 1 d . . .
O2 O 0.1879(2) 1.05872(16) 0.19013(10) 0.0213(4) Uani 1 1 d . . .
O3 O 0.2158(2) 0.90672(16) 0.12963(10) 0.0207(4) Uani 1 1 d . . .
O4 O 0.0449(2) 0.81000(16) 0.16887(10) 0.0201(4) Uani 1 1 d . . .
O5 O -0.1000(2) 0.79033(18) 0.08997(11) 0.0283(5) Uani 1 1 d . . .
O6 O 0.0255(2) 0.92497(16) 0.06965(10) 0.0208(4) Uani 1 1 d . . .
O7 O -0.0280(2) 1.14731(17) 0.23091(11) 0.0244(5) Uani 1 1 d . . .
H7 H -0.1113 1.1488 0.2299 0.037 Uiso 1 1 calc R . .
O8 O 0.4030(2) 0.97560(19) 0.14131(11) 0.0266(5) Uani 1 1 d . . .
H8 H 0.4209 1.0251 0.1593 0.040 Uiso 1 1 calc R . .
O9 O -0.0835(2) 0.67681(18) 0.18436(11) 0.0277(5) Uani 1 1 d . . .
H9 H -0.0532 0.6688 0.2211 0.042 Uiso 1 1 calc R . .
O10 O -0.1241(3) 0.90430(19) -0.00488(11) 0.0322(6) Uani 1 1 d . . .
H10 H -0.1002 0.9588 -0.0227 0.048 Uiso 1 1 calc R . .
B11 B 0.9639(3) 0.5490(3) 0.35041(16) 0.0184(7) Uani 1 1 d . . .
B12 B 1.0908(4) 0.6911(3) 0.33018(17) 0.0217(7) Uani 1 1 d . . .
B13 B 1.0940(4) 0.5921(3) 0.43393(16) 0.0201(7) Uani 1 1 d . . .
B14 B 0.9933(3) 0.3771(3) 0.30231(16) 0.0175(6) Uani 1 1 d . . .
B15 B 0.7712(4) 0.4750(3) 0.33198(18) 0.0225(7) Uani 1 1 d . . .
O11 O 1.0004(2) 0.64050(16) 0.31195(10) 0.0201(4) Uani 1 1 d . . .
O12 O 1.1450(2) 0.66369(18) 0.39000(10) 0.0259(5) Uani 1 1 d . . .
O13 O 0.9963(2) 0.54594(16) 0.41874(10) 0.0188(4) Uani 1 1 d . . .
O14 O 1.0475(2) 0.45264(16) 0.32164(10) 0.0185(4) Uani 1 1 d . . .
O15 O 0.8558(2) 0.38675(16) 0.30514(11) 0.0231(5) Uani 1 1 d . . .
O16 O 0.8209(2) 0.55244(16) 0.35095(10) 0.0194(4) Uani 1 1 d . . .
O17 O 1.1338(3) 0.77044(19) 0.29297(11) 0.0307(5) Uani 1 1 d . . .
H17 H 1.1013 0.7786 0.2568 0.046 Uiso 1 1 calc R . .
O18 O 1.1463(2) 0.57269(18) 0.49271(10) 0.0245(5) Uani 1 1 d . . .
H18 H 1.1036 0.5336 0.5176 0.037 Uiso 1 1 calc R . .
O19 O 1.0787(2) 0.28829(16) 0.28015(11) 0.0232(5) Uani 1 1 d . . .
H19 H 1.0330 0.2505 0.2662 0.035 Uiso 1 1 calc R . .
O20 O 0.6371(2) 0.4754(2) 0.33723(15) 0.0389(6) Uani 1 1 d . . .
H20 H 0.5927 0.5262 0.3587 0.058 Uiso 1 1 calc R . .
C1 C 0.1443(3) 0.9935(3) 0.35971(17) 0.0311(8) Uani 1 1 d . . .
H1A H 0.1607 1.0335 0.3179 0.047 Uiso 1 1 calc R . .
H1B H 0.0564 1.0276 0.3825 0.047 Uiso 1 1 calc R . .
H1C H 0.1423 0.9211 0.3516 0.047 Uiso 1 1 calc R . .
C2 C 0.2939(3) 1.1214(2) 0.41883(14) 0.0213(6) Uani 1 1 d . . .
C3 C 0.1792(3) 1.1968(3) 0.43836(16) 0.0278(7) Uani 1 1 d . . .
H3 H 0.0913 1.1808 0.4426 0.033 Uiso 1 1 calc R . .
C4 C 0.1920(4) 1.2954(3) 0.45171(17) 0.0333(8) Uani 1 1 d . . .
H4 H 0.1128 1.3473 0.4650 0.040 Uiso 1 1 calc R . .
C5 C 0.3181(4) 1.3189(3) 0.44590(16) 0.0304(8) Uani 1 1 d . . .
H5 H 0.3263 1.3864 0.4561 0.036 Uiso 1 1 calc R . .
C6 C 0.4316(4) 1.2459(3) 0.42556(16) 0.0282(7) Uani 1 1 d . . .
H6 H 0.5189 1.2630 0.4207 0.034 Uiso 1 1 calc R . .
C7 C 0.4201(3) 1.1462(3) 0.41179(16) 0.0261(7) Uani 1 1 d . . .
H7A H 0.4994 1.0952 0.3975 0.031 Uiso 1 1 calc R . .
C8 C 0.2416(3) 0.9300(2) 0.48879(15) 0.0217(6) Uani 1 1 d . . .
C9 C 0.2448(3) 0.9807(2) 0.54482(15) 0.0224(6) Uani 1 1 d . . .
H9A H 0.2620 1.0498 0.5410 0.027 Uiso 1 1 calc R . .
C10 C 0.2229(3) 0.9302(3) 0.60603(16) 0.0248(7) Uani 1 1 d . . .
H10A H 0.2239 0.9648 0.6444 0.030 Uiso 1 1 calc R . .
C11 C 0.1996(3) 0.8290(3) 0.61131(16) 0.0248(7) Uani 1 1 d . . .
H11 H 0.1861 0.7939 0.6534 0.030 Uiso 1 1 calc R . .
C12 C 0.1956(3) 0.7787(3) 0.55586(16) 0.0265(7) Uani 1 1 d . . .
H12 H 0.1789 0.7095 0.5600 0.032 Uiso 1 1 calc R . .
C13 C 0.2159(3) 0.8288(3) 0.49419(16) 0.0258(7) Uani 1 1 d . . .
H13 H 0.2124 0.7946 0.4560 0.031 Uiso 1 1 calc R . .
C14 C 0.4330(3) 0.9167(2) 0.37201(15) 0.0233(6) Uani 1 1 d . . .
C15 C 0.4619(4) 0.9291(3) 0.30459(17) 0.0332(8) Uani 1 1 d . . .
H15 H 0.3979 0.9753 0.2789 0.040 Uiso 1 1 calc R . .
C16 C 0.5833(4) 0.8745(3) 0.27533(18) 0.0377(9) Uani 1 1 d . . .
H16 H 0.6035 0.8815 0.2291 0.045 Uiso 1 1 calc R . .
C17 C 0.6763(4) 0.8092(3) 0.31328(18) 0.0330(8) Uani 1 1 d . . .
H17A H 0.7613 0.7722 0.2930 0.040 Uiso 1 1 calc R . .
C18 C 0.6479(4) 0.7970(3) 0.37930(18) 0.0329(8) Uani 1 1 d . . .
H18A H 0.7126 0.7512 0.4048 0.039 Uiso 1 1 calc R . .
C19 C 0.5265(3) 0.8505(3) 0.40912(16) 0.0295(7) Uani 1 1 d . . .
H19A H 0.5067 0.8420 0.4553 0.035 Uiso 1 1 calc R . .
P1 P 0.27830(8) 0.99030(6) 0.40919(4) 0.02123(18) Uani 1 1 d . . .
C21 C 0.5478(5) 0.8645(3) 0.0044(2) 0.0534(12) Uani 1 1 d . . .
H21A H 0.6270 0.8717 0.0250 0.080 Uiso 1 1 calc R . .
H21B H 0.4636 0.9018 0.0287 0.080 Uiso 1 1 calc R . .
H21C H 0.5537 0.8950 -0.0410 0.080 Uiso 1 1 calc R . .
C22 C 0.4181(4) 0.7103(3) -0.04167(19) 0.0391(9) Uani 1 1 d . . .
C23 C 0.4480(4) 0.6348(3) -0.08828(19) 0.0371(9) Uani 1 1 d . . .
H23 H 0.5380 0.5921 -0.0945 0.044 Uiso 1 1 calc R . .
C24 C 0.3500(4) 0.6210(3) -0.1252(2) 0.0464(10) Uani 1 1 d . . .
H24 H 0.3723 0.5695 -0.1568 0.056 Uiso 1 1 calc R . .
C25 C 0.2201(5) 0.6821(5) -0.1160(2) 0.0629(15) Uani 1 1 d . . .
H25 H 0.1513 0.6732 -0.1411 0.076 Uiso 1 1 calc R . .
C26 C 0.1897(5) 0.7569(5) -0.0699(3) 0.0671(16) Uani 1 1 d . . .
H26 H 0.0993 0.7990 -0.0637 0.080 Uiso 1 1 calc R . .
C27 C 0.2869(5) 0.7719(4) -0.0328(2) 0.0542(12) Uani 1 1 d . . .
H27 H 0.2640 0.8238 -0.0016 0.065 Uiso 1 1 calc R . .
C28 C 0.5150(4) 0.6788(3) 0.08789(17) 0.0332(8) Uani 1 1 d . . .
C29 C 0.3939(4) 0.6476(3) 0.10944(18) 0.0348(8) Uani 1 1 d . . .
H29 H 0.3294 0.6469 0.0798 0.042 Uiso 1 1 calc R . .
C30 C 0.3696(4) 0.6175(3) 0.1750(2) 0.0408(9) Uani 1 1 d . . .
H30 H 0.2872 0.5959 0.1908 0.049 Uiso 1 1 calc R . .
C31 C 0.4630(4) 0.6183(3) 0.2178(2) 0.0439(10) Uani 1 1 d . . .
H31 H 0.4439 0.5984 0.2629 0.053 Uiso 1 1 calc R . .
C32 C 0.5839(5) 0.6477(3) 0.1959(2) 0.0438(10) Uani 1 1 d . . .
H32 H 0.6495 0.6460 0.2254 0.053 Uiso 1 1 calc R . .
C33 C 0.6091(4) 0.6797(3) 0.13059(19) 0.0409(9) Uani 1 1 d . . .
H33 H 0.6909 0.7024 0.1152 0.049 Uiso 1 1 calc R . .
C34 C 0.7033(4) 0.6566(3) -0.03072(17) 0.0319(8) Uani 1 1 d . . .
C35 C 0.7681(4) 0.7027(3) -0.08522(18) 0.0405(9) Uani 1 1 d . . .
H35 H 0.7342 0.7745 -0.0995 0.049 Uiso 1 1 calc R . .
C36 C 0.8805(4) 0.6438(4) -0.1179(2) 0.0500(11) Uani 1 1 d . . .
H36 H 0.9257 0.6748 -0.1552 0.060 Uiso 1 1 calc R . .
C37 C 0.9297(4) 0.5397(4) -0.0977(2) 0.0459(10) Uani 1 1 d . . .
H37 H 1.0078 0.4993 -0.1216 0.055 Uiso 1 1 calc R . .
C38 C 0.8674(4) 0.4934(3) -0.0434(2) 0.0426(9) Uani 1 1 d . . .
H38 H 0.9026 0.4218 -0.0292 0.051 Uiso 1 1 calc R . .
C39 C 0.7538(4) 0.5518(3) -0.00987(19) 0.0384(9) Uani 1 1 d . . .
H39 H 0.7094 0.5206 0.0277 0.046 Uiso 1 1 calc R . .
P21 P 0.54611(11) 0.72791(7) 0.00506(5) 0.0339(2) Uani 1 1 d . . .
B21 B 1.3973(3) 0.3538(3) 0.28286(17) 0.0213(7) Uani 1 1 d . . .
O21 O 1.3483(2) 0.27660(19) 0.25924(12) 0.0302(5) Uani 1 1 d . . .
H21 H 1.2625 0.2906 0.2658 0.045 Uiso 1 1 calc R . .
O22 O 1.3187(2) 0.44261(17) 0.30701(11) 0.0242(5) Uani 1 1 d . . .
H22 H 1.2360 0.4399 0.3096 0.036 Uiso 1 1 calc R . .
O23 O 1.5345(2) 0.33661(18) 0.28009(12) 0.0270(5) Uani 1 1 d . . .
H23A H 1.5556 0.3852 0.2977 0.041 Uiso 1 1 calc R . .
B31 B 1.6446(4) 0.1037(3) 0.19543(19) 0.0249(7) Uani 1 1 d . . .
O31 O 1.6996(2) 0.15764(18) 0.23577(11) 0.0265(5) Uani 1 1 d . . .
H31A H 1.6408 0.2113 0.2476 0.040 Uiso 1 1 calc R . .
O32 O 1.5094(2) 0.12588(19) 0.18816(12) 0.0303(5) Uani 1 1 d . . .
H32A H 1.4676 0.1732 0.2129 0.045 Uiso 1 1 calc R . .
O33 O 1.7238(2) 0.0253(2) 0.16163(13) 0.0340(6) Uani 1 1 d . . .
H33A H 1.8058 0.0188 0.1682 0.051 Uiso 1 1 calc R . .
O41 O 0.4401(16) 0.5448(12) 0.5081(8) 0.035(4) Uiso 0.157(4) 1 d PU A -1
O42 O 0.5288(13) 0.4485(10) 0.5363(7) 0.042(4) Uiso 0.215(8) 1 d PU B -1
O43 O 0.4506(8) 0.6014(8) 0.4145(6) 0.030(3) Uiso 0.313(13) 1 d PU C -1
O44 O 0.4449(7) 0.6310(7) 0.3858(5) 0.024(3) Uiso 0.314(13) 1 d PU D -1
 
 
_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
B1 O3 1.435(4) . ?
B1 O4 1.466(4) . ?
B1 O6 1.471(4) . ?
B1 O1 1.473(4) . ?
B2 O1 1.334(4) . ?
B2 O7 1.361(4) . ?
B2 O2 1.369(4) . ?
B3 O3 1.335(4) . ?
B3 O8 1.342(4) . ?
B3 O2 1.395(4) . ?
B4 O4 1.351(4) . ?
B4 O9 1.358(4) . ?
B4 O5 1.388(4) . ?
B5 O6 1.353(4) . ?
B5 O10 1.354(4) . ?
B5 O5 1.378(4) . ?
O7 H7 0.8400 . ?
O8 H8 0.8400 . ?
O9 H9 0.8400 . ?
O10 H10 0.8400 . ?
B11 O16 1.434(4) . ?
B11 O11 1.462(4) . ?
B11 O14 1.473(4) . ?
B11 O13 1.481(4) . ?
B12 O17 1.349(4) . ?
B12 O11 1.351(4) . ?
B12 O12 1.393(4) . ?
B13 O13 1.352(4) . ?
B13 O18 1.360(4) . ?
B13 O12 1.378(4) . ?
B14 O14 1.346(4) . ?
B14 O19 1.354(4) . ?
B14 O15 1.360(4) . ?
B15 O16 1.337(4) . ?
B15 O20 1.345(4) . ?
B15 O15 1.382(4) . ?
O17 H17 0.8400 . ?
O18 H18 0.8400 . ?
O19 H19 0.8400 . ?
O20 H20 0.8400 . ?
C1 P1 1.786(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C7 1.374(5) . ?
C2 C3 1.379(4) . ?
C2 P1 1.785(3) . ?
C3 C4 1.379(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.367(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.359(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.393(5) . ?
C6 H6 0.9500 . ?
C7 H7A 0.9500 . ?
C8 C9 1.394(4) . ?
C8 C13 1.395(4) . ?
C8 P1 1.784(3) . ?
C9 C10 1.383(4) . ?
C9 H9A 0.9500 . ?
C10 C11 1.386(5) . ?
C10 H10A 0.9500 . ?
C11 C12 1.382(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.386(5) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C19 1.376(4) . ?
C14 C15 1.386(4) . ?
C14 P1 1.760(3) . ?
C15 C16 1.367(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.379(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.357(5) . ?
C17 H17A 0.9500 . ?
C18 C19 1.366(5) . ?
C18 H18A 0.9500 . ?
C19 H19A 0.9500 . ?
C21 P21 1.783(4) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C27 1.381(5) . ?
C22 C23 1.400(6) . ?
C22 P21 1.774(5) . ?
C23 C24 1.376(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.369(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.387(8) . ?
C25 H25 0.9500 . ?
C26 C27 1.377(7) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C33 1.378(6) . ?
C28 C29 1.386(5) . ?
C28 P21 1.781(4) . ?
C29 C30 1.378(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.373(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.375(6) . ?
C31 H31 0.9500 . ?
C32 C33 1.381(5) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
C34 C35 1.385(5) . ?
C34 C39 1.388(5) . ?
C34 P21 1.757(4) . ?
C35 C36 1.356(6) . ?
C35 H35 0.9500 . ?
C36 C37 1.374(6) . ?
C36 H36 0.9500 . ?
C37 C38 1.373(6) . ?
C37 H37 0.9500 . ?
C38 C39 1.368(5) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
B21 O22 1.343(4) . ?
B21 O23 1.348(4) . ?
B21 O21 1.373(4) . ?
O21 H21 0.8400 . ?
O22 H22 0.8400 . ?
O23 H23A 0.8400 . ?
B31 O33 1.339(4) . ?
B31 O32 1.354(4) . ?
B31 O31 1.382(4) . ?
O31 H31A 0.8400 . ?
O32 H32A 0.8400 . ?
O33 H33A 0.8400 . ?
 
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
O3 B1 O4 110.7(2) . . ?
O3 B1 O6 109.2(2) . . ?
O4 B1 O6 110.7(2) . . ?
O3 B1 O1 110.9(2) . . ?
O4 B1 O1 107.8(2) . . ?
O6 B1 O1 107.5(2) . . ?
O1 B2 O7 121.2(3) . . ?
O1 B2 O2 122.8(3) . . ?
O7 B2 O2 116.0(3) . . ?
O3 B3 O8 120.4(3) . . ?
O3 B3 O2 122.0(3) . . ?
O8 B3 O2 117.6(3) . . ?
O4 B4 O9 122.6(3) . . ?
O4 B4 O5 121.6(3) . . ?
O9 B4 O5 115.8(3) . . ?
O6 B5 O10 121.5(3) . . ?
O6 B5 O5 120.7(3) . . ?
O10 B5 O5 117.9(3) . . ?
B2 O1 B1 123.1(2) . . ?
B2 O2 B3 116.7(2) . . ?
B3 O3 B1 124.2(2) . . ?
B4 O4 B1 122.3(2) . . ?
B5 O5 B4 119.0(3) . . ?
B5 O6 B1 123.0(2) . . ?
B2 O7 H7 109.5 . . ?
B3 O8 H8 109.5 . . ?
B4 O9 H9 109.5 . . ?
B5 O10 H10 109.5 . . ?
O16 B11 O11 110.9(2) . . ?
O16 B11 O14 110.7(2) . . ?
O11 B11 O14 108.2(2) . . ?
O16 B11 O13 109.0(2) . . ?
O11 B11 O13 110.4(2) . . ?
O14 B11 O13 107.6(2) . . ?
O17 B12 O11 123.3(3) . . ?
O17 B12 O12 115.7(3) . . ?
O11 B12 O12 121.0(3) . . ?
O13 B13 O18 122.9(3) . . ?
O13 B13 O12 120.9(3) . . ?
O18 B13 O12 116.1(3) . . ?
O14 B14 O19 118.8(3) . . ?
O14 B14 O15 122.1(3) . . ?
O19 B14 O15 119.1(3) . . ?
O16 B15 O20 123.8(3) . . ?
O16 B15 O15 121.8(3) . . ?
O20 B15 O15 114.4(3) . . ?
B12 O11 B11 122.4(2) . . ?
B13 O12 B12 119.0(3) . . ?
B13 O13 B11 121.5(2) . . ?
B14 O14 B11 123.1(2) . . ?
B14 O15 B15 117.8(2) . . ?
B15 O16 B11 124.2(3) . . ?
B12 O17 H17 109.5 . . ?
B13 O18 H18 109.5 . . ?
B14 O19 H19 109.5 . . ?
B15 O20 H20 109.5 . . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C7 C2 C3 119.4(3) . . ?
C7 C2 P1 120.8(2) . . ?
C3 C2 P1 119.6(3) . . ?
C2 C3 C4 120.0(3) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 120.3(3) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C6 C5 C4 120.2(3) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C7 120.0(3) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C2 C7 C6 120.0(3) . . ?
C2 C7 H7A 120.0 . . ?
C6 C7 H7A 120.0 . . ?
C9 C8 C13 120.3(3) . . ?
C9 C8 P1 120.8(2) . . ?
C13 C8 P1 118.8(2) . . ?
C10 C9 C8 119.8(3) . . ?
C10 C9 H9A 120.1 . . ?
C8 C9 H9A 120.1 . . ?
C9 C10 C11 119.8(3) . . ?
C9 C10 H10A 120.1 . . ?
C11 C10 H10A 120.1 . . ?
C12 C11 C10 120.6(3) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C11 C12 C13 120.3(3) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C12 C13 C8 119.2(3) . . ?
C12 C13 H13 120.4 . . ?
C8 C13 H13 120.4 . . ?
C19 C14 C15 120.1(3) . . ?
C19 C14 P1 120.9(2) . . ?
C15 C14 P1 118.9(2) . . ?
C16 C15 C14 119.5(3) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
C15 C16 C17 119.6(3) . . ?
C15 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
C18 C17 C16 120.9(3) . . ?
C18 C17 H17A 119.6 . . ?
C16 C17 H17A 119.6 . . ?
C17 C18 C19 120.1(3) . . ?
C17 C18 H18A 120.0 . . ?
C19 C18 H18A 120.0 . . ?
C18 C19 C14 119.8(3) . . ?
C18 C19 H19A 120.1 . . ?
C14 C19 H19A 120.1 . . ?
C14 P1 C8 109.09(15) . . ?
C14 P1 C2 110.13(15) . . ?
C8 P1 C2 107.73(14) . . ?
C14 P1 C1 109.19(16) . . ?
C8 P1 C1 110.32(16) . . ?
C2 P1 C1 110.36(16) . . ?
P21 C21 H21A 109.5 . . ?
P21 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
P21 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C27 C22 C23 118.8(4) . . ?
C27 C22 P21 120.3(4) . . ?
C23 C22 P21 120.9(3) . . ?
C24 C23 C22 121.5(4) . . ?
C24 C23 H23 119.2 . . ?
C22 C23 H23 119.2 . . ?
C25 C24 C23 119.3(5) . . ?
C25 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
C24 C25 C26 119.5(5) . . ?
C24 C25 H25 120.3 . . ?
C26 C25 H25 120.3 . . ?
C27 C26 C25 121.8(4) . . ?
C27 C26 H26 119.1 . . ?
C25 C26 H26 119.1 . . ?
C26 C27 C22 119.1(5) . . ?
C26 C27 H27 120.5 . . ?
C22 C27 H27 120.5 . . ?
C33 C28 C29 121.1(3) . . ?
C33 C28 P21 118.5(3) . . ?
C29 C28 P21 120.2(3) . . ?
C30 C29 C28 118.3(4) . . ?
C30 C29 H29 120.9 . . ?
C28 C29 H29 120.9 . . ?
C31 C30 C29 120.8(4) . . ?
C31 C30 H30 119.6 . . ?
C29 C30 H30 119.6 . . ?
C30 C31 C32 120.7(4) . . ?
C30 C31 H31 119.7 . . ?
C32 C31 H31 119.7 . . ?
C31 C32 C33 119.3(4) . . ?
C31 C32 H32 120.4 . . ?
C33 C32 H32 120.4 . . ?
C28 C33 C32 119.8(4) . . ?
C28 C33 H33 120.1 . . ?
C32 C33 H33 120.1 . . ?
C35 C34 C39 120.3(3) . . ?
C35 C34 P21 118.6(3) . . ?
C39 C34 P21 120.7(3) . . ?
C36 C35 C34 119.0(4) . . ?
C36 C35 H35 120.5 . . ?
C34 C35 H35 120.5 . . ?
C35 C36 C37 120.8(4) . . ?
C35 C36 H36 119.6 . . ?
C37 C36 H36 119.6 . . ?
C38 C37 C36 120.7(4) . . ?
C38 C37 H37 119.6 . . ?
C36 C37 H37 119.6 . . ?
C39 C38 C37 119.2(4) . . ?
C39 C38 H38 120.4 . . ?
C37 C38 H38 120.4 . . ?
C38 C39 C34 120.0(3) . . ?
C38 C39 H39 120.0 . . ?
C34 C39 H39 120.0 . . ?
C34 P21 C22 106.83(17) . . ?
C34 P21 C28 110.11(18) . . ?
C22 P21 C28 110.34(17) . . ?
C34 P21 C21 110.43(19) . . ?
C22 P21 C21 110.8(2) . . ?
C28 P21 C21 108.36(19) . . ?
O22 B21 O23 119.7(3) . . ?
O22 B21 O21 124.7(3) . . ?
O23 B21 O21 115.6(3) . . ?
B21 O21 H21 109.5 . . ?
B21 O22 H22 109.5 . . ?
B21 O23 H23A 109.5 . . ?
O33 B31 O32 116.4(3) . . ?
O33 B31 O31 121.0(3) . . ?
O32 B31 O31 122.6(3) . . ?
B31 O31 H31A 109.5 . . ?
B31 O32 H32A 109.5 . . ?
B31 O33 H33A 109.5 . . ?
 
loop_
 _geom_hbond_atom_site_label_D
 _geom_hbond_atom_site_label_H
 _geom_hbond_atom_site_label_A
 _geom_hbond_distance_DH
 _geom_hbond_distance_HA
 _geom_hbond_distance_DA
 _geom_hbond_angle_DHA
 _geom_hbond_site_symmetry_A
O7 H7 O31  0.84 1.88 2.714(3) 174.3 1_365
O8 H8 O32  0.84 1.93 2.747(3) 164.7 1_465
O9 H9 O11  0.84 1.99 2.828(3) 173.0 1_455
O10 H10 O6  0.84 1.97 2.803(3) 173.2 2_575
O17 H17 O4  0.84 1.95 2.779(3) 171.7 1_655
O18 H18 O13  0.84 1.93 2.763(3) 174.2 2_766
O19 H19 O7  0.84 1.85 2.673(3) 166.7 1_645
O20 H20 O44  0.84 1.84 2.639(8) 157.5 .
O20 H20 O43  0.84 1.87 2.666(8) 157.6 .
O20 H20 O42  0.84 2.36 3.040(14) 137.8 2_666
O21 H21 O19  0.84 1.85 2.676(3) 166.8 .
O22 H22 O14  0.84 1.86 2.695(3) 171.4 .
O23 H23A O20  0.84 1.88 2.710(3) 168.6 1_655
O31 H31A O23  0.84 1.87 2.699(3) 170.2 .
O32 H32A O21  0.84 1.84 2.671(3) 169.3 .
O33 H33A O1  0.84 1.86 2.695(3) 173.1 1_745
 
_diffrn_measured_fraction_theta_max    0.986
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.986
_refine_diff_density_max    1.057
_refine_diff_density_min   -0.945
_refine_diff_density_rms    0.085
