data_2010src0035

#Dr. M. Beckett/ James Timmis
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          
 'B5 H4 O10, C5 H12 N'
_chemical_formula_sum
 'C5 H16 B5 N O10'
_chemical_formula_weight          304.24
 
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                    9.4446(4)
_cell_length_b                    13.9129(7)
_cell_length_c                    10.3330(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  92.517(3)
_cell_angle_gamma                 90.00
_cell_volume                      1356.46(10)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     3154
_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           0.42
_exptl_crystal_size_mid           0.38
_exptl_crystal_size_min           0.18
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.490
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              632
_exptl_absorpt_coefficient_mu     0.131
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9469
_exptl_absorpt_correction_T_max   0.9768
_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: 0.6419 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             15990
_diffrn_reflns_av_R_equivalents   0.0500
_diffrn_reflns_av_sigmaI/netI     0.0447
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -18
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -13
_diffrn_reflns_limit_l_max        13
_diffrn_reflns_theta_min          3.53
_diffrn_reflns_theta_max          27.48
_reflns_number_total              3110
_reflns_number_gt                 2319
_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)+(0.0627P)²+0.2571P] 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          3110
_refine_ls_number_parameters      215
_refine_ls_number_restraints      13
_refine_ls_R_factor_all           0.0665
_refine_ls_R_factor_gt            0.0447
_refine_ls_wR_factor_ref          0.1204
_refine_ls_wR_factor_gt           0.1078
_refine_ls_goodness_of_fit_ref    1.027
_refine_ls_restrained_S_all       1.029
_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 0.77962(16) 0.12458(14) 0.12862(15) 0.0173(4) Uani 1 1 d . . .
B2 B 0.52885(18) 0.07624(13) 0.11978(15) 0.0180(4) Uani 1 1 d . . .
B3 B 0.60536(18) 0.19021(14) -0.03373(16) 0.0197(4) Uani 1 1 d . . .
B4 B 1.03908(17) 0.09963(13) 0.13504(15) 0.0178(4) Uani 1 1 d . . .
B5 B 0.94297(18) 0.21472(14) 0.27745(15) 0.0189(4) Uani 1 1 d . . .
O1 O 0.66619(10) 0.05871(8) 0.15903(9) 0.0178(3) Uani 1 1 d . . .
O2 O 0.49579(10) 0.14768(8) 0.03025(9) 0.0203(3) Uani 1 1 d . . .
O3 O 0.74168(10) 0.18018(8) 0.01045(9) 0.0190(3) Uani 1 1 d . . .
O4 O 0.90652(10) 0.06810(8) 0.10102(9) 0.0184(3) Uani 1 1 d . . .
O5 O 1.05916(10) 0.17296(8) 0.22305(10) 0.0219(3) Uani 1 1 d . . .
O6 O 0.80916(10) 0.19007(8) 0.23814(9) 0.0191(3) Uani 1 1 d . . .
O7 O 0.42670(11) 0.02006(9) 0.16686(11) 0.0253(3) Uani 1 1 d . . .
H7 H 0.3469 0.0396 0.1389 0.038 Uiso 1 1 calc R . .
O8 O 0.56678(11) 0.24067(9) -0.14211(10) 0.0253(3) Uani 1 1 d . . .
H8 H 0.6396 0.2619 -0.1763 0.038 Uiso 1 1 calc R . .
O9 O 1.15528(11) 0.06005(9) 0.08402(10) 0.0239(3) Uani 1 1 d . . .
H9 H 1.1300 0.0194 0.0275 0.036 Uiso 1 1 calc R . .
O10 O 0.97380(11) 0.28146(9) 0.37054(10) 0.0247(3) Uani 1 1 d . . .
H10 H 0.8993 0.2970 0.4068 0.037 Uiso 1 1 calc R . .
C1 C 0.2586(4) 0.1578(4) 0.6626(5) 0.0223(7) Uani 0.741(3) 1 d PD A 1
H1 H 0.2472 0.2275 0.6409 0.027 Uiso 0.741(3) 1 calc PR A 1
C2 C 0.1304(5) 0.0996(3) 0.6056(5) 0.0336(10) Uani 0.741(3) 1 d PD A 1
H2A H 0.0899 0.0587 0.6731 0.040 Uiso 0.741(3) 1 calc PR A 1
H2B H 0.0555 0.1434 0.5704 0.040 Uiso 0.741(3) 1 calc PR A 1
C3 C 0.1887(5) 0.0373(3) 0.4970(3) 0.0461(9) Uani 0.741(3) 1 d PD A 1
H3A H 0.2019 -0.0299 0.5263 0.055 Uiso 0.741(3) 1 calc PR A 1
H3B H 0.1232 0.0380 0.4195 0.055 Uiso 0.741(3) 1 calc PR A 1
C4 C 0.3274(3) 0.0816(2) 0.4673(2) 0.0463(7) Uani 0.741(3) 1 d PD A 1
H4A H 0.3138 0.1360 0.4062 0.056 Uiso 0.741(3) 1 calc PR A 1
H4B H 0.3908 0.0337 0.4291 0.056 Uiso 0.741(3) 1 calc PR A 1
C5 C 0.3887(5) 0.1165(5) 0.5984(7) 0.0332(8) Uani 0.741(3) 1 d PD A 1
H5A H 0.4618 0.1666 0.5875 0.040 Uiso 0.741(3) 1 calc PR A 1
H5B H 0.4307 0.0627 0.6497 0.040 Uiso 0.741(3) 1 calc PR A 1
N1 N 0.2727(9) 0.1443(9) 0.8069(5) 0.0238(8) Uani 0.741(3) 1 d PD A 1
H1A H 0.2827 0.0807 0.8255 0.036 Uiso 0.741(3) 1 calc PR A 1
H1B H 0.1938 0.1673 0.8438 0.036 Uiso 0.741(3) 1 calc PR A 1
H1C H 0.3501 0.1769 0.8389 0.036 Uiso 0.741(3) 1 calc PR A 1
C21 C 0.2852(16) 0.1548(14) 0.6450(16) 0.0223(7) Uani 0.259(3) 1 d PD A 2
H21 H 0.2953 0.2248 0.6253 0.027 Uiso 0.259(3) 1 calc PR A 2
C22 C 0.1399(17) 0.1209(12) 0.5883(17) 0.0336(10) Uani 0.259(3) 1 d PD A 2
H22A H 0.0700 0.1149 0.6565 0.040 Uiso 0.259(3) 1 calc PR A 2
H22B H 0.1023 0.1652 0.5201 0.040 Uiso 0.259(3) 1 calc PR A 2
C23 C 0.1765(14) 0.0234(11) 0.5324(12) 0.0461(9) Uani 0.259(3) 1 d PD A 2
H23A H 0.1382 -0.0281 0.5870 0.055 Uiso 0.259(3) 1 calc PR A 2
H23B H 0.1322 0.0171 0.4442 0.055 Uiso 0.259(3) 1 calc PR A 2
C24 C 0.3278(9) 0.0126(6) 0.5270(7) 0.0463(7) Uani 0.259(3) 1 d PD A 2
H24A H 0.3540 0.0028 0.4362 0.056 Uiso 0.259(3) 1 calc PR A 2
H24B H 0.3597 -0.0441 0.5783 0.056 Uiso 0.259(3) 1 calc PR A 2
C25 C 0.3987(17) 0.1026(16) 0.581(2) 0.0332(8) Uani 0.259(3) 1 d PD A 2
H25A H 0.4766 0.0860 0.6448 0.040 Uiso 0.259(3) 1 calc PR A 2
H25B H 0.4376 0.1418 0.5114 0.040 Uiso 0.259(3) 1 calc PR A 2
N21 N 0.288(3) 0.143(3) 0.7880(16) 0.0238(8) Uani 0.259(3) 1 d PD A 2
H21A H 0.2874 0.0795 0.8081 0.036 Uiso 0.259(3) 1 calc PR A 2
H21B H 0.2095 0.1716 0.8197 0.036 Uiso 0.259(3) 1 calc PR A 2
H21C H 0.3670 0.1712 0.8238 0.036 Uiso 0.259(3) 1 calc PR A 2
 
 
_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 1.455(2) . ?
B1 O6 1.4701(19) . ?
B1 O4 1.4715(19) . ?
B1 O3 1.4763(19) . ?
B2 O7 1.349(2) . ?
B2 O1 1.3639(19) . ?
B2 O2 1.384(2) . ?
B3 O3 1.354(2) . ?
B3 O8 1.358(2) . ?
B3 O2 1.385(2) . ?
B4 O9 1.355(2) . ?
B4 O4 1.3581(19) . ?
B4 O5 1.374(2) . ?
B5 O6 1.354(2) . ?
B5 O10 1.359(2) . ?
B5 O5 1.383(2) . ?
O7 H7 0.8400 . ?
O8 H8 0.8400 . ?
O9 H9 0.8400 . ?
O10 H10 0.8400 . ?
C1 N1 1.504(5) . ?
C1 C5 1.533(4) . ?
C1 C2 1.551(5) . ?
C1 H1 1.0000 . ?
C2 C3 1.539(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.492(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.529(6) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
C21 C25 1.472(13) . ?
C21 N21 1.486(14) . ?
C21 C22 1.543(14) . ?
C21 H21 1.0000 . ?
C22 C23 1.520(15) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.441(13) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.517(15) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
N21 H21A 0.9100 . ?
N21 H21B 0.9100 . ?
N21 H21C 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 O6 109.93(11) . . ?
O1 B1 O4 108.62(13) . . ?
O6 B1 O4 110.58(11) . . ?
O1 B1 O3 110.76(11) . . ?
O6 B1 O3 110.05(13) . . ?
O4 B1 O3 106.84(11) . . ?
O7 B2 O1 118.37(14) . . ?
O7 B2 O2 120.87(13) . . ?
O1 B2 O2 120.72(14) . . ?
O3 B3 O8 123.23(14) . . ?
O3 B3 O2 120.95(14) . . ?
O8 B3 O2 115.81(13) . . ?
O9 B4 O4 121.41(14) . . ?
O9 B4 O5 117.94(13) . . ?
O4 B4 O5 120.65(14) . . ?
O6 B5 O10 123.59(14) . . ?
O6 B5 O5 121.22(14) . . ?
O10 B5 O5 115.18(13) . . ?
B2 O1 B1 121.53(13) . . ?
B2 O2 B3 118.32(12) . . ?
B3 O3 B1 121.70(12) . . ?
B4 O4 B1 121.79(12) . . ?
B4 O5 B5 119.47(12) . . ?
B5 O6 B1 122.06(12) . . ?
B2 O7 H7 109.5 . . ?
B3 O8 H8 109.5 . . ?
B4 O9 H9 109.5 . . ?
B5 O10 H10 109.5 . . ?
N1 C1 C5 110.2(5) . . ?
N1 C1 C2 110.2(5) . . ?
C5 C1 C2 105.5(3) . . ?
N1 C1 H1 110.3 . . ?
C5 C1 H1 110.3 . . ?
C2 C1 H1 110.3 . . ?
C3 C2 C1 105.8(3) . . ?
C3 C2 H2A 110.6 . . ?
C1 C2 H2A 110.6 . . ?
C3 C2 H2B 110.6 . . ?
C1 C2 H2B 110.6 . . ?
H2A C2 H2B 108.7 . . ?
C4 C3 C2 105.2(3) . . ?
C4 C3 H3A 110.7 . . ?
C2 C3 H3A 110.7 . . ?
C4 C3 H3B 110.7 . . ?
C2 C3 H3B 110.7 . . ?
H3A C3 H3B 108.8 . . ?
C3 C4 C5 104.5(3) . . ?
C3 C4 H4A 110.8 . . ?
C5 C4 H4A 110.8 . . ?
C3 C4 H4B 110.8 . . ?
C5 C4 H4B 110.8 . . ?
H4A C4 H4B 108.9 . . ?
C4 C5 C1 102.9(4) . . ?
C4 C5 H5A 111.2 . . ?
C1 C5 H5A 111.2 . . ?
C4 C5 H5B 111.2 . . ?
C1 C5 H5B 111.2 . . ?
H5A C5 H5B 109.1 . . ?
C25 C21 N21 114.2(16) . . ?
C25 C21 C22 109.5(12) . . ?
N21 C21 C22 108.5(15) . . ?
C25 C21 H21 108.2 . . ?
N21 C21 H21 108.2 . . ?
C22 C21 H21 108.2 . . ?
C23 C22 C21 101.7(11) . . ?
C23 C22 H22A 111.4 . . ?
C21 C22 H22A 111.4 . . ?
C23 C22 H22B 111.4 . . ?
C21 C22 H22B 111.4 . . ?
H22A C22 H22B 109.3 . . ?
C24 C23 C22 110.5(11) . . ?
C24 C23 H23A 109.6 . . ?
C22 C23 H23A 109.6 . . ?
C24 C23 H23B 109.6 . . ?
C22 C23 H23B 109.6 . . ?
H23A C23 H23B 108.1 . . ?
C23 C24 C25 108.8(10) . . ?
C23 C24 H24A 109.9 . . ?
C25 C24 H24A 109.9 . . ?
C23 C24 H24B 109.9 . . ?
C25 C24 H24B 109.9 . . ?
H24A C24 H24B 108.3 . . ?
C21 C25 C24 104.7(11) . . ?
C21 C25 H25A 110.8 . . ?
C24 C25 H25A 110.8 . . ?
C21 C25 H25B 110.8 . . ?
C24 C25 H25B 110.8 . . ?
H25A C25 H25B 108.9 . . ?
C21 N21 H21A 109.5 . . ?
C21 N21 H21B 109.5 . . ?
H21A N21 H21B 109.5 . . ?
C21 N21 H21C 109.5 . . ?
H21A N21 H21C 109.5 . . ?
H21B N21 H21C 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 O9  0.84 1.89 2.7241(15) 169.2 1_455
O8 H8 O6  0.84 1.98 2.8194(15) 178.2 4_565
O9 H9 O4  0.84 1.82 2.6603(15) 174.1 3_755
O10 H10 O3  0.84 1.90 2.7311(14) 171.0 4_566
N1 H1A O1  0.91 2.00 2.902(12) 168.9 3_656
N1 H1B O10  0.91 2.22 3.103(8) 162.0 4_466
N1 H1C O8  0.91 2.23 3.108(10) 161.7 1_556
N1 H1C O2  0.91 2.39 3.056(8) 129.8 1_556
N21 H21A O1  0.91 2.00 2.89(4) 166.8 3_656
N21 H21B O10  0.91 2.40 3.29(2) 166.0 4_466
N21 H21C O8  0.91 2.14 3.03(3) 165.5 1_556
N21 H21C O2  0.91 2.43 3.12(2) 132.2 1_556
 
_diffrn_measured_fraction_theta_max    0.998
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.998
_refine_diff_density_max    0.264
_refine_diff_density_min   -0.270
_refine_diff_density_rms    0.057
