data_2007src0217
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dr. M. A. Beckett
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C4 H14 B5 N O11'
_chemical_formula_weight          306.21
 
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'
 '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                    8.7992(3)
_cell_length_b                    9.0108(2)
_cell_length_c                    9.3873(3)
_cell_angle_alpha                 73.957(2)
_cell_angle_beta                  78.099(2)
_cell_angle_gamma                 63.845(2)
_cell_volume                      638.99(3)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     2878
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Plate
_exptl_crystal_colour             Colourless
_exptl_crystal_size_max           0.22
_exptl_crystal_size_mid           0.17
_exptl_crystal_size_min           0.04
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.592
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              316
_exptl_absorpt_coefficient_mu     0.146
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9687
_exptl_absorpt_correction_T_max   0.9942
_exptl_absorpt_process_details       'SADABS V2.10 (Sheldrick, G.M., 2003)'

_exptl_special_details
;
SADABS was used to perform the Absorption correction
Parameter refinement on 11082 reflections reduced R(int) from 0.1327 to 0.0361
Ratio of minimum to maximum apparent transmission: 0.925823
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 95mm 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             11693
_diffrn_reflns_av_R_equivalents   0.0354
_diffrn_reflns_av_sigmaI/netI     0.0326
_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        -12
_diffrn_reflns_limit_l_max        12
_diffrn_reflns_theta_min          3.05
_diffrn_reflns_theta_max          27.48
_reflns_number_total              2921
_reflns_number_gt                 2573
_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)+(0.0188P)²+0.4666P] 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          2921
_refine_ls_number_parameters      194
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0457
_refine_ls_R_factor_gt            0.0385
_refine_ls_wR_factor_ref          0.0865
_refine_ls_wR_factor_gt           0.0817
_refine_ls_goodness_of_fit_ref    1.066
_refine_ls_restrained_S_all       1.066
_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 0.34157(19) 0.88849(19) 0.30547(17) 0.0128(3) Uani 1 1 d . . .
B2 B 0.58518(19) 0.76730(19) 0.45705(17) 0.0141(3) Uani 1 1 d . . .
B3 B 0.5440(2) 0.5896(2) 0.33670(17) 0.0142(3) Uani 1 1 d . . .
B4 B 0.2812(2) 1.1455(2) 0.10697(17) 0.0146(3) Uani 1 1 d . . .
B5 B 0.07361(19) 1.1401(2) 0.31371(17) 0.0138(3) Uani 1 1 d . . .
O1 O 0.44465(12) 0.90081(12) 0.40466(11) 0.0156(2) Uani 1 1 d . . .
O2 O 0.64529(12) 0.61493(12) 0.41426(11) 0.0157(2) Uani 1 1 d . . .
O3 O 0.38646(12) 0.71196(11) 0.30520(11) 0.0137(2) Uani 1 1 d . . .
O4 O 0.37251(12) 0.97630(12) 0.15408(10) 0.0150(2) Uani 1 1 d . . .
O5 O 0.13706(12) 1.23173(12) 0.19442(11) 0.0154(2) Uani 1 1 d . . .
O6 O 0.16218(12) 0.96992(12) 0.36179(10) 0.0137(2) Uani 1 1 d . . .
O7 O 0.67708(13) 0.77714(12) 0.55237(12) 0.0186(2) Uani 1 1 d . . .
H7 H 0.6340 0.8756 0.5680 0.028 Uiso 1 1 calc R . .
O8 O 0.59696(12) 0.44033(12) 0.29548(11) 0.0172(2) Uani 1 1 d . . .
H8 H 0.6967 0.3781 0.3178 0.026 Uiso 1 1 calc R . .
O9 O 0.33204(13) 1.23496(12) -0.01936(11) 0.0192(2) Uani 1 1 d . . .
H9 H 0.4242 1.1708 -0.0581 0.029 Uiso 1 1 calc R . .
O10 O -0.08250(12) 1.22276(12) 0.38288(11) 0.0187(2) Uani 1 1 d . . .
H10 H -0.1016 1.1574 0.4605 0.028 Uiso 1 1 calc R . .
C11 C 1.06422(19) 0.18499(19) 0.79628(17) 0.0220(3) Uani 1 1 d . . .
H11A H 1.0187 0.1209 0.7599 0.026 Uiso 1 1 calc R . .
H11B H 1.1895 0.1354 0.7747 0.026 Uiso 1 1 calc R . .
C12 C 0.99283(18) 0.36805(19) 0.71432(18) 0.0218(3) Uani 1 1 d . . .
H12A H 1.0452 0.4311 0.7436 0.026 Uiso 1 1 calc R . .
H12B H 1.0193 0.3748 0.6056 0.026 Uiso 1 1 calc R . .
C13 C 0.7608(2) 0.42146(19) 0.91684(17) 0.0234(3) Uani 1 1 d . . .
H13A H 0.6357 0.4650 0.9402 0.028 Uiso 1 1 calc R . .
H13B H 0.8031 0.4851 0.9573 0.028 Uiso 1 1 calc R . .
C14 C 0.8422(2) 0.23459(19) 0.98658(17) 0.0224(3) Uani 1 1 d . . .
H14A H 0.8149 0.2177 1.0960 0.027 Uiso 1 1 calc R . .
H14B H 0.7953 0.1725 0.9491 0.027 Uiso 1 1 calc R . .
N11 N 0.80494(15) 0.44430(15) 0.75201(14) 0.0183(3) Uani 1 1 d . . .
H11C H 0.7556 0.3942 0.7139 0.022 Uiso 1 1 calc R . .
H11D H 0.7622 0.5578 0.7090 0.022 Uiso 1 1 calc R . .
O11 O 1.02213(14) 0.16900(13) 0.95186(12) 0.0227(2) Uani 1 1 d . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
B1 O4 1.4590(18) . ?
B1 O3 1.4609(17) . ?
B1 O6 1.4693(17) . ?
B1 O1 1.4820(18) . ?
B2 O1 1.3530(18) . ?
B2 O7 1.3667(18) . ?
B2 O2 1.3796(18) . ?
B3 O8 1.3553(18) . ?
B3 O3 1.3660(18) . ?
B3 O2 1.3840(18) . ?
B4 O9 1.3517(18) . ?
B4 O4 1.3635(18) . ?
B4 O5 1.3933(18) . ?
B5 O10 1.3641(18) . ?
B5 O6 1.3678(18) . ?
B5 O5 1.3731(18) . ?
O7 H7 0.8400 . ?
O8 H8 0.8400 . ?
O9 H9 0.8400 . ?
O10 H10 0.8400 . ?
C11 O11 1.4137(19) . ?
C11 C12 1.514(2) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 N11 1.4908(18) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 N11 1.4946(19) . ?
C13 C14 1.516(2) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 O11 1.4250(18) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
N11 H11C 0.9200 . ?
N11 H11D 0.9200 . ?
 
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
O4 B1 O3 108.96(11) . . ?
O4 B1 O6 110.29(11) . . ?
O3 B1 O6 110.35(11) . . ?
O4 B1 O1 109.24(11) . . ?
O3 B1 O1 110.87(11) . . ?
O6 B1 O1 107.12(11) . . ?
O1 B2 O7 121.92(13) . . ?
O1 B2 O2 121.58(13) . . ?
O7 B2 O2 116.49(12) . . ?
O8 B3 O3 118.80(13) . . ?
O8 B3 O2 120.47(13) . . ?
O3 B3 O2 120.69(12) . . ?
O9 B4 O4 121.65(13) . . ?
O9 B4 O5 118.47(13) . . ?
O4 B4 O5 119.78(13) . . ?
O10 B5 O6 120.30(13) . . ?
O10 B5 O5 118.22(13) . . ?
O6 B5 O5 121.48(13) . . ?
B2 O1 B1 121.93(11) . . ?
B2 O2 B3 118.69(11) . . ?
B3 O3 B1 121.09(11) . . ?
B4 O4 B1 121.32(11) . . ?
B5 O5 B4 118.81(11) . . ?
B5 O6 B1 119.58(11) . . ?
B2 O7 H7 109.5 . . ?
B3 O8 H8 109.5 . . ?
B4 O9 H9 109.5 . . ?
B5 O10 H10 109.5 . . ?
O11 C11 C12 111.73(12) . . ?
O11 C11 H11A 109.3 . . ?
C12 C11 H11A 109.3 . . ?
O11 C11 H11B 109.3 . . ?
C12 C11 H11B 109.3 . . ?
H11A C11 H11B 107.9 . . ?
N11 C12 C11 109.11(12) . . ?
N11 C12 H12A 109.9 . . ?
C11 C12 H12A 109.9 . . ?
N11 C12 H12B 109.9 . . ?
C11 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
N11 C13 C14 108.62(12) . . ?
N11 C13 H13A 110.0 . . ?
C14 C13 H13A 110.0 . . ?
N11 C13 H13B 110.0 . . ?
C14 C13 H13B 110.0 . . ?
H13A C13 H13B 108.3 . . ?
O11 C14 C13 110.73(12) . . ?
O11 C14 H14A 109.5 . . ?
C13 C14 H14A 109.5 . . ?
O11 C14 H14B 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
C12 N11 C13 111.00(12) . . ?
C12 N11 H11C 109.4 . . ?
C13 N11 H11C 109.4 . . ?
C12 N11 H11D 109.4 . . ?
C13 N11 H11D 109.4 . . ?
H11C N11 H11D 108.0 . . ?
C11 O11 C14 110.48(11) . . ?
 
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 1.89 2.7313(14) 174.9 2_676
O8 H8 O10  0.84 1.93 2.7681(14) 174.9 1_645
O9 H9 O4  0.84 1.92 2.7556(14) 176.9 2_675
O10 H10 O6  0.84 1.87 2.7076(14) 174.5 2_576
N11 H11C O3  0.92 1.94 2.8264(15) 162.1 2_666
N11 H11D O7  0.92 2.04 2.9259(16) 160.6 .
 
_diffrn_measured_fraction_theta_max    0.995
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.995
_refine_diff_density_max    0.276
_refine_diff_density_min   -0.235
_refine_diff_density_rms    0.052
