data_2010src0034

#Dr. M. Beckett/ James Timmis
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C3 H12 B5 N O10'
_chemical_formula_weight          276.19
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'B'  'B'   0.0013   0.0007
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_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                    8.0079(2)
_cell_length_b                    8.8634(3)
_cell_length_c                    8.8643(2)
_cell_angle_alpha                 67.429(2)
_cell_angle_beta                  88.975(2)
_cell_angle_gamma                 75.9650(10)
_cell_volume                      561.64(3)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     2522
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Slab
_exptl_crystal_colour             Colourless
_exptl_crystal_size_max           0.62
_exptl_crystal_size_mid           0.36
_exptl_crystal_size_min           0.14
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.633
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              284
_exptl_absorpt_coefficient_mu     0.149
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9131
_exptl_absorpt_correction_T_max   0.9794
_exptl_absorpt_process_details       'SADABS 2007/2 (Sheldrick, G.M., 2007)'

_exptl_special_details
;
SADABS was used to perform the Absorption correction
Estimated minimum and maximum transmission: 0.6932 0.7456
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    'graphite'
_diffrn_measurement_device_type   
'Bruker-Nonius Roper CCD camera on κ-goniostat'
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   '9.091'
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             12353
_diffrn_reflns_av_R_equivalents   0.0274
_diffrn_reflns_av_sigmaI/netI     0.0232
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_k_min        -11
_diffrn_reflns_limit_k_max        11
_diffrn_reflns_limit_l_min        -11
_diffrn_reflns_limit_l_max        11
_diffrn_reflns_theta_min          3.18
_diffrn_reflns_theta_max          27.48
_reflns_number_total              2571
_reflns_number_gt                 2284
_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, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_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)+(0.0383P)²+0.1789P] 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          2571
_refine_ls_number_parameters      177
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0361
_refine_ls_R_factor_gt            0.0317
_refine_ls_wR_factor_ref          0.0821
_refine_ls_wR_factor_gt           0.0792
_refine_ls_goodness_of_fit_ref    1.078
_refine_ls_restrained_S_all       1.078
_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
B1 B 0.26952(15) 0.36925(15) 0.28296(14) 0.0116(2) Uani 1 1 d . . .
B2 B 0.04071(16) 0.26914(15) 0.19142(15) 0.0141(2) Uani 1 1 d . . .
B3 B 0.26009(15) 0.06857(15) 0.39451(15) 0.0125(2) Uani 1 1 d . . .
B4 B 0.46353(15) 0.56396(15) 0.19625(15) 0.0125(2) Uani 1 1 d . . .
B5 B 0.28217(15) 0.57572(15) 0.40878(15) 0.0128(2) Uani 1 1 d . . .
O1 O 0.11912(10) 0.39461(9) 0.17607(9) 0.01426(17) Uani 1 1 d . . .
O2 O 0.10398(10) 0.10788(10) 0.30862(10) 0.01609(18) Uani 1 1 d . . .
O3 O 0.34556(9) 0.18877(9) 0.37801(9) 0.01269(17) Uani 1 1 d . . .
O4 O 0.39715(9) 0.44367(9) 0.17843(9) 0.01237(17) Uani 1 1 d . . .
O5 O 0.41242(10) 0.62744(9) 0.31457(9) 0.01453(18) Uani 1 1 d . . .
O6 O 0.21384(10) 0.45401(9) 0.39543(9) 0.01341(17) Uani 1 1 d . . .
O7 O -0.09579(11) 0.29593(10) 0.08845(11) 0.0210(2) Uani 1 1 d . . .
H7 H -0.1164 0.3947 0.0166 0.032 Uiso 1 1 calc R . .
O8 O 0.32840(10) -0.09597(9) 0.49333(10) 0.01643(18) Uani 1 1 d . . .
H8 H 0.4298 -0.1085 0.5282 0.025 Uiso 1 1 calc R . .
O9 O 0.58239(10) 0.62971(10) 0.09798(9) 0.01547(18) Uani 1 1 d . . .
H9 H 0.5946 0.5946 0.0219 0.023 Uiso 1 1 calc R . .
O10 O 0.21149(11) 0.64428(10) 0.51472(10) 0.01793(18) Uani 1 1 d . . .
H10 H 0.2530 0.7253 0.5065 0.027 Uiso 1 1 calc R . .
C1 C 0.84374(15) 0.86675(14) 0.20610(14) 0.0184(2) Uani 1 1 d . . .
H1 H 0.9397 0.8985 0.2477 0.022 Uiso 1 1 calc R . .
C2 C 0.66946(17) 0.98607(16) 0.17460(16) 0.0239(3) Uani 1 1 d . . .
H2A H 0.6576 1.0889 0.1974 0.029 Uiso 1 1 calc R . .
H2B H 0.5680 0.9378 0.1964 0.029 Uiso 1 1 calc R . .
C3 C 0.77014(17) 0.97321(16) 0.03425(15) 0.0241(3) Uani 1 1 d . . .
H3A H 0.7308 0.9169 -0.0305 0.029 Uiso 1 1 calc R . .
H3B H 0.8204 1.0681 -0.0295 0.029 Uiso 1 1 calc R . .
N1 N 0.85032(12) 0.68556(12) 0.26883(12) 0.0163(2) Uani 1 1 d . . .
H1A H 0.8388 0.6468 0.3785 0.024 Uiso 1 1 calc R . .
H1B H 0.9534 0.6278 0.2498 0.024 Uiso 1 1 calc R . .
H1C H 0.7629 0.6700 0.2169 0.024 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
B1 0.0127(5) 0.0106(5) 0.0121(5) -0.0042(4) 0.0001(4) -0.0043(4)
B2 0.0135(6) 0.0134(6) 0.0158(6) -0.0056(5) -0.0002(4) -0.0046(4)
B3 0.0132(5) 0.0123(6) 0.0132(5) -0.0060(4) 0.0013(4) -0.0039(4)
B4 0.0122(5) 0.0121(5) 0.0125(5) -0.0037(4) -0.0017(4) -0.0033(4)
B5 0.0123(5) 0.0116(5) 0.0135(6) -0.0036(4) -0.0008(4) -0.0034(4)
O1 0.0142(4) 0.0119(4) 0.0150(4) -0.0024(3) -0.0038(3) -0.0046(3)
O2 0.0152(4) 0.0121(4) 0.0196(4) -0.0033(3) -0.0041(3) -0.0057(3)
O3 0.0127(4) 0.0101(4) 0.0147(4) -0.0034(3) -0.0025(3) -0.0039(3)
O4 0.0140(4) 0.0131(4) 0.0120(4) -0.0054(3) 0.0024(3) -0.0064(3)
O5 0.0172(4) 0.0150(4) 0.0154(4) -0.0075(3) 0.0038(3) -0.0089(3)
O6 0.0145(4) 0.0131(4) 0.0163(4) -0.0077(3) 0.0042(3) -0.0071(3)
O7 0.0204(4) 0.0145(4) 0.0248(4) -0.0028(3) -0.0101(3) -0.0059(3)
O8 0.0151(4) 0.0113(4) 0.0216(4) -0.0040(3) -0.0051(3) -0.0047(3)
O9 0.0183(4) 0.0188(4) 0.0144(4) -0.0085(3) 0.0047(3) -0.0107(3)
O10 0.0215(4) 0.0165(4) 0.0231(4) -0.0122(3) 0.0090(3) -0.0111(3)
C1 0.0191(6) 0.0164(5) 0.0184(6) -0.0033(4) -0.0012(4) -0.0079(4)
C2 0.0270(6) 0.0193(6) 0.0223(6) -0.0081(5) 0.0015(5) -0.0003(5)
C3 0.0292(7) 0.0208(6) 0.0170(6) -0.0026(5) 0.0020(5) -0.0049(5)
N1 0.0143(4) 0.0163(5) 0.0174(5) -0.0048(4) 0.0010(4) -0.0056(4)
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
B1 O1 1.4645(13) . ?
B1 O3 1.4666(13) . ?
B1 O6 1.4676(13) . ?
B1 O4 1.4704(13) . ?
B2 O7 1.3519(14) . ?
B2 O1 1.3671(14) . ?
B2 O2 1.3808(14) . ?
B3 O8 1.3576(14) . ?
B3 O3 1.3621(14) . ?
B3 O2 1.3722(14) . ?
B4 O4 1.3607(14) . ?
B4 O9 1.3617(14) . ?
B4 O5 1.3820(14) . ?
B5 O10 1.3505(14) . ?
B5 O6 1.3652(14) . ?
B5 O5 1.3792(14) . ?
O7 H7 0.8400 . ?
O8 H8 0.8400 . ?
O9 H9 0.8400 . ?
O10 H10 0.8400 . ?
C1 N1 1.4716(15) . ?
C1 C2 1.4884(17) . ?
C1 C3 1.4891(16) . ?
C1 H1 1.0000 . ?
C2 C3 1.4964(17) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
 
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 B1 O3 110.86(8) . . ?
O1 B1 O6 108.55(8) . . ?
O3 B1 O6 109.39(9) . . ?
O1 B1 O4 107.81(8) . . ?
O3 B1 O4 109.64(8) . . ?
O6 B1 O4 110.57(8) . . ?
O7 B2 O1 121.52(10) . . ?
O7 B2 O2 117.66(10) . . ?
O1 B2 O2 120.75(10) . . ?
O8 B3 O3 121.23(10) . . ?
O8 B3 O2 117.29(10) . . ?
O3 B3 O2 121.45(10) . . ?
O4 B4 O9 122.08(10) . . ?
O4 B4 O5 121.66(10) . . ?
O9 B4 O5 116.26(9) . . ?
O10 B5 O6 116.20(10) . . ?
O10 B5 O5 122.79(10) . . ?
O6 B5 O5 120.98(10) . . ?
B2 O1 B1 123.05(9) . . ?
B3 O2 B2 119.04(9) . . ?
B3 O3 B1 122.58(9) . . ?
B4 O4 B1 123.50(8) . . ?
B5 O5 B4 118.80(9) . . ?
B5 O6 B1 124.10(8) . . ?
B2 O7 H7 109.5 . . ?
B3 O8 H8 109.5 . . ?
B4 O9 H9 109.5 . . ?
B5 O10 H10 109.5 . . ?
N1 C1 C2 116.77(10) . . ?
N1 C1 C3 117.71(10) . . ?
C2 C1 C3 60.34(8) . . ?
N1 C1 H1 116.7 . . ?
C2 C1 H1 116.7 . . ?
C3 C1 H1 116.7 . . ?
C1 C2 C3 59.85(8) . . ?
C1 C2 H2A 117.8 . . ?
C3 C2 H2A 117.8 . . ?
C1 C2 H2B 117.8 . . ?
C3 C2 H2B 117.8 . . ?
H2A C2 H2B 114.9 . . ?
C1 C3 C2 59.81(8) . . ?
C1 C3 H3A 117.8 . . ?
C2 C3 H3A 117.8 . . ?
C1 C3 H3B 117.8 . . ?
C2 C3 H3B 117.8 . . ?
H3A C3 H3B 114.9 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 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 O1  0.84 1.98 2.8082(11) 166.7 2_565
O8 H8 O3  0.84 1.85 2.6719(11) 166.7 2_656
O9 H9 O4  0.84 1.93 2.7586(11) 169.5 2_665
O10 H10 O8  0.84 1.79 2.6299(11) 176.2 1_565
N1 H1A O6  0.91 1.94 2.8423(12) 170.3 2_666
N1 H1B O6  0.91 2.32 3.0654(12) 138.5 1_655
N1 H1B O1  0.91 2.48 3.2912(12) 149.1 1_655
N1 H1C O9  0.91 1.98 2.8895(12) 176.8 .
 
_diffrn_measured_fraction_theta_max    0.996
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.996
_refine_diff_density_max    0.165
_refine_diff_density_min   -0.288
_refine_diff_density_rms    0.050
