data_2008src0818
 
#Dr. M. A. Beckett

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C6 H19 B5 N2 O10'
_chemical_formula_weight          333.28
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 '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                    8.8129(2)
_cell_length_b                    8.8960(2)
_cell_length_c                    10.3618(2)
_cell_angle_alpha                 74.0430(10)
_cell_angle_beta                  78.8540(10)
_cell_angle_gamma                 88.9620(10)
_cell_volume                      765.80(3)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     3398
_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           0.28
_exptl_crystal_size_mid           0.23
_exptl_crystal_size_min           0.18
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.445
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              348
_exptl_absorpt_coefficient_mu     0.125
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9659
_exptl_absorpt_correction_T_max   0.9779
_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: 0.6778 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             16010
_diffrn_reflns_av_R_equivalents   0.0281
_diffrn_reflns_av_sigmaI/netI     0.0232
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -11
_diffrn_reflns_limit_k_max        11
_diffrn_reflns_limit_l_min        -13
_diffrn_reflns_limit_l_max        12
_diffrn_reflns_theta_min          3.41
_diffrn_reflns_theta_max          27.48
_reflns_number_total              3493
_reflns_number_gt                 3204
_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)+(0.0379P)²+0.2418P] 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          3493
_refine_ls_number_parameters      214
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0358
_refine_ls_R_factor_gt            0.0322
_refine_ls_wR_factor_ref          0.0842
_refine_ls_wR_factor_gt           0.0817
_refine_ls_goodness_of_fit_ref    1.051
_refine_ls_restrained_S_all       1.051
_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 0.09288(12) 0.19162(12) 0.19128(11) 0.0134(2) Uani 1 1 d . . .
B2 B -0.09180(13) 0.40610(13) 0.20037(11) 0.0172(2) Uani 1 1 d . . .
B3 B -0.09675(12) 0.19512(13) 0.40321(11) 0.0152(2) Uani 1 1 d . . .
B4 B 0.37574(13) 0.14403(13) 0.13785(11) 0.0154(2) Uani 1 1 d . . .
B5 B 0.20020(13) -0.00021(13) 0.06597(11) 0.0153(2) Uani 1 1 d . . .
O1 O 0.02331(8) 0.33840(8) 0.13034(7) 0.01556(15) Uani 1 1 d . . .
O2 O -0.15004(9) 0.33765(8) 0.33798(7) 0.02142(17) Uani 1 1 d . . .
O3 O 0.01534(8) 0.12295(8) 0.33455(7) 0.01478(15) Uani 1 1 d . . .
O4 O 0.25695(8) 0.22491(8) 0.18879(7) 0.01562(15) Uani 1 1 d . . .
O5 O 0.34688(8) 0.02105(8) 0.08803(7) 0.01893(16) Uani 1 1 d . . .
O6 O 0.07928(8) 0.08214(8) 0.10982(7) 0.01492(15) Uani 1 1 d . . .
O7 O -0.15238(10) 0.54300(9) 0.14167(8) 0.0283(2) Uani 1 1 d . . .
H7 H -0.1090 0.5751 0.0589 0.042 Uiso 1 1 calc R . .
O8 O -0.16079(9) 0.13511(9) 0.53772(7) 0.02095(17) Uani 1 1 d . . .
H8 H -0.1156 0.0536 0.5704 0.031 Uiso 1 1 calc R . .
O9 O 0.52167(8) 0.19152(9) 0.13694(8) 0.02002(17) Uani 1 1 d . . .
H9 H 0.5858 0.1399 0.0971 0.030 Uiso 1 1 calc R . .
O10 O 0.18817(8) -0.10555(9) -0.00581(8) 0.01943(16) Uani 1 1 d . . .
H10 H 0.1014 -0.0991 -0.0288 0.029 Uiso 1 1 calc R . .
C11 C 0.46062(12) 0.25161(12) 0.46816(11) 0.0224(2) Uani 1 1 d . . .
H11A H 0.4142 0.1666 0.4419 0.027 Uiso 1 1 calc R . .
H11B H 0.5568 0.2136 0.5003 0.027 Uiso 1 1 calc R . .
C12 C 0.49852(12) 0.39270(13) 0.34548(11) 0.0229(2) Uani 1 1 d . . .
H12A H 0.5476 0.4769 0.3708 0.027 Uiso 1 1 calc R . .
H12B H 0.5724 0.3646 0.2715 0.027 Uiso 1 1 calc R . .
C13 C 0.23712(14) 0.48246(14) 0.40965(12) 0.0270(2) Uani 1 1 d . . .
H13A H 0.1387 0.5116 0.3783 0.032 Uiso 1 1 calc R . .
H13B H 0.2755 0.5717 0.4357 0.032 Uiso 1 1 calc R . .
C14 C 0.20883(13) 0.34053(14) 0.53237(12) 0.0259(2) Uani 1 1 d . . .
H14A H 0.1344 0.3654 0.6077 0.031 Uiso 1 1 calc R . .
H14B H 0.1629 0.2538 0.5081 0.031 Uiso 1 1 calc R . .
C15 C 0.32145(18) 0.16105(15) 0.70213(13) 0.0366(3) Uani 1 1 d . . .
H15A H 0.2724 0.0735 0.6833 0.055 Uiso 1 1 calc R . .
H15B H 0.2521 0.1939 0.7747 0.055 Uiso 1 1 calc R . .
H15C H 0.4189 0.1281 0.7317 0.055 Uiso 1 1 calc R . .
C16 C 0.3869(2) 0.58755(15) 0.17355(13) 0.0408(3) Uani 1 1 d . . .
H16A H 0.4284 0.6747 0.1986 0.061 Uiso 1 1 calc R . .
H16B H 0.2914 0.6183 0.1396 0.061 Uiso 1 1 calc R . .
H16C H 0.4632 0.5605 0.1019 0.061 Uiso 1 1 calc R . .
N11 N 0.35268(11) 0.29170(11) 0.57815(9) 0.02153(19) Uani 1 1 d . . .
N12 N 0.35315(11) 0.44951(10) 0.29594(9) 0.0217(2) Uani 1 1 d . . .
H12 H 0.3118 0.3695 0.2700 0.026 Uiso 1 1 calc R . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
B1 O1 1.4653(12) . ?
B1 O3 1.4725(12) . ?
B1 O6 1.4734(12) . ?
B1 O4 1.4752(12) . ?
B2 O7 1.3538(13) . ?
B2 O1 1.3609(12) . ?
B2 O2 1.3851(13) . ?
B3 O8 1.3578(13) . ?
B3 O3 1.3604(12) . ?
B3 O2 1.3838(13) . ?
B4 O9 1.3585(13) . ?
B4 O4 1.3638(12) . ?
B4 O5 1.3782(13) . ?
B5 O6 1.3588(12) . ?
B5 O10 1.3637(13) . ?
B5 O5 1.3806(13) . ?
O7 H7 0.8400 . ?
O8 H8 0.8400 . ?
O9 H9 0.8400 . ?
O10 H10 0.8400 . ?
C11 N11 1.4571(14) . ?
C11 C12 1.5089(16) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 N12 1.4995(14) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 N12 1.4944(14) . ?
C13 C14 1.5097(17) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 N11 1.4561(14) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 N11 1.4597(15) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 N12 1.4886(15) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
N12 H12 0.9300 . ?
 
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 111.17(7) . . ?
O1 B1 O6 108.26(8) . . ?
O3 B1 O6 109.99(8) . . ?
O1 B1 O4 108.52(8) . . ?
O3 B1 O4 108.34(8) . . ?
O6 B1 O4 110.56(7) . . ?
O7 B2 O1 122.58(9) . . ?
O7 B2 O2 116.89(9) . . ?
O1 B2 O2 120.52(9) . . ?
O8 B3 O3 123.04(9) . . ?
O8 B3 O2 116.22(9) . . ?
O3 B3 O2 120.73(9) . . ?
O9 B4 O4 117.17(9) . . ?
O9 B4 O5 122.17(9) . . ?
O4 B4 O5 120.65(9) . . ?
O6 B5 O10 123.31(9) . . ?
O6 B5 O5 121.69(9) . . ?
O10 B5 O5 114.97(9) . . ?
B2 O1 B1 123.94(8) . . ?
B3 O2 B2 119.84(8) . . ?
B3 O3 B1 123.55(8) . . ?
B4 O4 B1 123.50(8) . . ?
B4 O5 B5 118.78(8) . . ?
B5 O6 B1 122.66(8) . . ?
B2 O7 H7 109.5 . . ?
B3 O8 H8 109.5 . . ?
B4 O9 H9 109.5 . . ?
B5 O10 H10 109.5 . . ?
N11 C11 C12 110.29(9) . . ?
N11 C11 H11A 109.6 . . ?
C12 C11 H11A 109.6 . . ?
N11 C11 H11B 109.6 . . ?
C12 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
N12 C12 C11 109.65(9) . . ?
N12 C12 H12A 109.7 . . ?
C11 C12 H12A 109.7 . . ?
N12 C12 H12B 109.7 . . ?
C11 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
N12 C13 C14 110.51(9) . . ?
N12 C13 H13A 109.5 . . ?
C14 C13 H13A 109.5 . . ?
N12 C13 H13B 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 108.1 . . ?
N11 C14 C13 110.81(9) . . ?
N11 C14 H14A 109.5 . . ?
C13 C14 H14A 109.5 . . ?
N11 C14 H14B 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
N11 C15 H15A 109.5 . . ?
N11 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N11 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N12 C16 H16A 109.5 . . ?
N12 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N12 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 N11 C11 109.32(8) . . ?
C14 N11 C15 109.96(10) . . ?
C11 N11 C15 111.93(9) . . ?
C16 N12 C13 112.35(10) . . ?
C16 N12 C12 110.99(10) . . ?
C13 N12 C12 110.07(8) . . ?
C16 N12 H12 107.7 . . ?
C13 N12 H12 107.7 . . ?
C12 N12 H12 107.7 . . ?
 
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 1.90 2.7422(10) 175.0 2_565
O8 H8 O3  0.84 1.91 2.7466(10) 172.6 2_556
O9 H9 O10  0.84 2.09 2.8508(10) 150.6 2_655
O10 H10 O6  0.84 1.92 2.7570(10) 171.0 2
N12 H12 O4  0.93 1.84 2.7548(11) 169.2 .
 
_diffrn_measured_fraction_theta_max    0.991
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.991
_refine_diff_density_max    0.234
_refine_diff_density_min   -0.243
_refine_diff_density_rms    0.040
