data_2009src0116

#Dr. M. A. Beckett
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C7 H14 B5 N O10'
_chemical_formula_weight          326.24
 
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            monoclinic
_symmetry_space_group_name_H-M    P2(1)/c
 
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                    9.3511(2)
_cell_length_b                    14.5157(4)
_cell_length_c                    10.4670(2)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.778(2)
_cell_angle_gamma                 90.00
_cell_volume                      1420.64(6)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     3287
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        block
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.16
_exptl_crystal_size_mid           0.16
_exptl_crystal_size_min           0.14
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.525
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              672
_exptl_absorpt_coefficient_mu     0.131
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9793
_exptl_absorpt_correction_T_max   0.9818
_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 15185 reflections reduced R(int) from 0.0537 to 0.0415
Ratio of minimum to maximum apparent transmission: 0.915404
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             15637
_diffrn_reflns_av_R_equivalents   0.0375
_diffrn_reflns_av_sigmaI/netI     0.0323
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -18
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -13
_diffrn_reflns_limit_l_max        13
_diffrn_reflns_theta_min          3.22
_diffrn_reflns_theta_max          27.48
_reflns_number_total              3244
_reflns_number_gt                 2877
_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)+(0.0265P)²+0.9485P] 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          3244
_refine_ls_number_parameters      213
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0457
_refine_ls_R_factor_gt            0.0391
_refine_ls_wR_factor_ref          0.0922
_refine_ls_wR_factor_gt           0.0874
_refine_ls_goodness_of_fit_ref    1.074
_refine_ls_restrained_S_all       1.074
_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 0.20809(15) 0.13669(11) 0.89975(14) 0.0133(3) Uani 1 1 d . . .
B2 B -0.05322(15) 0.11620(11) 0.90580(14) 0.0138(3) Uani 1 1 d . . .
B3 B 0.04152(15) 0.23241(11) 0.77239(14) 0.0141(3) Uani 1 1 d . . .
B4 B 0.38291(16) 0.19689(11) 1.05882(14) 0.0157(3) Uani 1 1 d . . .
B5 B 0.46139(15) 0.08942(11) 0.90077(14) 0.0142(3) Uani 1 1 d . . .
O1 O 0.08038(9) 0.08057(7) 0.92409(9) 0.0147(2) Uani 1 1 d . . .
O2 O -0.07352(9) 0.19727(7) 0.83950(9) 0.0154(2) Uani 1 1 d . . .
O3 O 0.17702(9) 0.20356(7) 0.79682(9) 0.0148(2) Uani 1 1 d . . .
O4 O 0.24479(10) 0.18549(7) 1.01912(9) 0.0149(2) Uani 1 1 d . . .
O5 O 0.49451(9) 0.15618(7) 0.99220(9) 0.0159(2) Uani 1 1 d . . .
O6 O 0.32322(9) 0.07553(7) 0.86173(9) 0.0143(2) Uani 1 1 d . . .
O7 O -0.16942(9) 0.07126(7) 0.95169(9) 0.0164(2) Uani 1 1 d . . .
H7 H -0.1433 0.0217 0.9863 0.025 Uiso 1 1 calc R . .
O8 O 0.00921(10) 0.29592(7) 0.67985(9) 0.0171(2) Uani 1 1 d . . .
H8 H 0.0828 0.3076 0.6377 0.026 Uiso 1 1 calc R . .
O9 O 0.42021(10) 0.24607(8) 1.16365(9) 0.0216(2) Uani 1 1 d . . .
H9 H 0.3461 0.2647 1.2001 0.032 Uiso 1 1 calc R . .
O10 O 0.56336(10) 0.03493(7) 0.85060(10) 0.0200(2) Uani 1 1 d . . .
H10 H 0.6443 0.0528 0.8761 0.030 Uiso 1 1 calc R . .
C1 C 0.64027(17) 0.13120(12) 0.33197(14) 0.0258(3) Uani 1 1 d . . .
H1D H 0.6477 0.1970 0.3563 0.031 Uiso 1 1 calc R . .
H1E H 0.5375 0.1150 0.3263 0.031 Uiso 1 1 calc R . .
C2 C 0.71238(16) 0.07289(11) 0.43264(14) 0.0213(3) Uani 1 1 d . . .
C3 C 0.66887(17) -0.01768(12) 0.45150(15) 0.0265(3) Uani 1 1 d . . .
H3 H 0.5941 -0.0430 0.4002 0.032 Uiso 1 1 calc R . .
C4 C 0.7346(2) -0.07108(12) 0.54527(16) 0.0314(4) Uani 1 1 d . . .
H4 H 0.7040 -0.1327 0.5589 0.038 Uiso 1 1 calc R . .
C5 C 0.8447(2) -0.03477(13) 0.61887(15) 0.0341(4) Uani 1 1 d . . .
H5 H 0.8884 -0.0711 0.6840 0.041 Uiso 1 1 calc R . .
C6 C 0.89132(19) 0.05397(12) 0.59826(15) 0.0309(4) Uani 1 1 d . . .
H6 H 0.9696 0.0778 0.6467 0.037 Uiso 1 1 calc R . .
C7 C 0.82396(17) 0.10855(11) 0.50681(14) 0.0255(3) Uani 1 1 d . . .
H7A H 0.8541 0.1704 0.4948 0.031 Uiso 1 1 calc R . .
N1 N 0.70796(12) 0.11683(9) 0.20383(11) 0.0181(3) Uani 1 1 d . . .
H1A H 0.7985 0.1399 0.2056 0.027 Uiso 1 1 calc R . .
H1B H 0.6555 0.1464 0.1425 0.027 Uiso 1 1 calc R . .
H1C H 0.7109 0.0555 0.1859 0.027 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 O6 1.4550(17) . ?
B1 O1 1.4706(17) . ?
B1 O4 1.4727(17) . ?
B1 O3 1.4761(17) . ?
B2 O7 1.3606(17) . ?
B2 O1 1.3632(17) . ?
B2 O2 1.3781(18) . ?
B3 O3 1.3556(17) . ?
B3 O8 1.3680(18) . ?
B3 O2 1.3897(17) . ?
B4 O9 1.3508(18) . ?
B4 O4 1.3615(17) . ?
B4 O5 1.3944(18) . ?
B5 O10 1.3506(18) . ?
B5 O6 1.3649(17) . ?
B5 O5 1.3938(18) . ?
O7 H7 0.8400 . ?
O8 H8 0.8400 . ?
O9 H9 0.8400 . ?
O10 H10 0.8400 . ?
C1 C2 1.504(2) . ?
C1 N1 1.5053(18) . ?
C1 H1D 0.9900 . ?
C1 H1E 0.9900 . ?
C2 C3 1.391(2) . ?
C2 C7 1.392(2) . ?
C3 C4 1.388(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.382(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.378(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.387(2) . ?
C6 H6 0.9500 . ?
C7 H7A 0.9500 . ?
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
O6 B1 O1 108.36(11) . . ?
O6 B1 O4 111.15(10) . . ?
O1 B1 O4 107.45(10) . . ?
O6 B1 O3 109.91(10) . . ?
O1 B1 O3 109.78(10) . . ?
O4 B1 O3 110.13(11) . . ?
O7 B2 O1 120.22(13) . . ?
O7 B2 O2 118.81(12) . . ?
O1 B2 O2 120.96(12) . . ?
O3 B3 O8 122.59(12) . . ?
O3 B3 O2 121.29(12) . . ?
O8 B3 O2 116.11(12) . . ?
O9 B4 O4 123.06(13) . . ?
O9 B4 O5 116.32(12) . . ?
O4 B4 O5 120.61(12) . . ?
O10 B5 O6 117.88(13) . . ?
O10 B5 O5 121.51(12) . . ?
O6 B5 O5 120.59(12) . . ?
B2 O1 B1 120.68(11) . . ?
B2 O2 B3 117.75(11) . . ?
B3 O3 B1 121.00(11) . . ?
B4 O4 B1 121.77(11) . . ?
B5 O5 B4 118.50(11) . . ?
B5 O6 B1 121.94(11) . . ?
B2 O7 H7 109.5 . . ?
B3 O8 H8 109.5 . . ?
B4 O9 H9 109.5 . . ?
B5 O10 H10 109.5 . . ?
C2 C1 N1 110.87(12) . . ?
C2 C1 H1D 109.5 . . ?
N1 C1 H1D 109.5 . . ?
C2 C1 H1E 109.5 . . ?
N1 C1 H1E 109.5 . . ?
H1D C1 H1E 108.1 . . ?
C3 C2 C7 119.39(14) . . ?
C3 C2 C1 120.14(14) . . ?
C7 C2 C1 120.47(14) . . ?
C4 C3 C2 120.04(15) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C5 C4 C3 120.05(16) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C6 C5 C4 120.29(16) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C7 120.02(16) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C6 C7 C2 120.16(16) . . ?
C6 C7 H7A 119.9 . . ?
C2 C7 H7A 119.9 . . ?
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 1.85 2.6855(14) 174.5 3_557
O8 H8 O4  0.84 1.97 2.8030(13) 169.1 4_565
O9 H9 O3  0.84 1.94 2.7812(13) 173.8 4_566
O10 H10 O7  0.84 1.92 2.7513(13) 168.9 1_655
N1 H1A O8  0.91 2.20 3.1019(15) 171.0 4_665
N1 H1B O5  0.91 2.17 3.0162(15) 154.9 1_554
N1 H1B O9  0.91 2.64 3.3024(16) 129.8 1_554
N1 H1C O6  0.91 1.99 2.8892(16) 168.8 3_656
 
_diffrn_measured_fraction_theta_max    0.998
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.998
_refine_diff_density_max    0.254
_refine_diff_density_min   -0.240
_refine_diff_density_rms    0.050
