data_2007src0218

#Dr. M. A. Beckett

#The structure was solved in C2, as there was only a pseudo mirror
#plane which the borate anion almost fitted, but the disordered
#cation would not.

 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C7 H20 B5 N O11'
_chemical_formula_weight          348.29
 
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   0.0000
 '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   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    C2
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y, -z'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z'
 
_cell_length_a                    14.7118(3)
_cell_length_b                    11.4599(3)
_cell_length_c                    9.8194(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  103.911(2)
_cell_angle_gamma                 90.00
_cell_volume                      1606.95(7)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     3593
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Plate
_exptl_crystal_colour             'Light Yellow'
_exptl_crystal_size_max           0.60
_exptl_crystal_size_mid           0.36
_exptl_crystal_size_min           0.16
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.440
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              728
_exptl_absorpt_coefficient_mu     0.125
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9286
_exptl_absorpt_correction_T_max   0.9802
_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 11787 reflections reduced R(int) from 0.1703 to 0.0383
Ratio of minimum to maximum apparent transmission: 0.888353
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             13456
_diffrn_reflns_av_R_equivalents   0.0430
_diffrn_reflns_av_sigmaI/netI     0.0293
_diffrn_reflns_limit_h_min        -19
_diffrn_reflns_limit_h_max        19
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_k_max        14
_diffrn_reflns_limit_l_min        -12
_diffrn_reflns_limit_l_max        12
_diffrn_reflns_theta_min          3.13
_diffrn_reflns_theta_max          27.48
_reflns_number_total              1932
_reflns_number_gt                 1589
_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)+(0.0854P)²+2.9712P] 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_abs_structure_details
 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack    ?
_refine_ls_number_reflns          1932
_refine_ls_number_parameters      473
_refine_ls_number_restraints      1371
_refine_ls_R_factor_all           0.0721
_refine_ls_R_factor_gt            0.0599
_refine_ls_wR_factor_ref          0.1702
_refine_ls_wR_factor_gt           0.1566
_refine_ls_goodness_of_fit_ref    1.077
_refine_ls_restrained_S_all       0.878
_refine_ls_shift/su_max           0.003
_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 0.19001(18) 0.6216(7) 0.4134(3) 0.0247(6) Uani 1 1 d U . .
B2 B 0.2987(5) 0.5179(6) 0.6102(6) 0.0309(12) Uani 1 1 d U . .
B3 B 0.2984(5) 0.7253(7) 0.6071(7) 0.0373(14) Uani 1 1 d U . .
B4 B 0.12292(19) 0.6214(8) 0.1551(3) 0.0299(6) Uani 1 1 d U . .
B5 B 0.0182(2) 0.6208(10) 0.3078(3) 0.0419(9) Uani 1 1 d U . .
O1 O 0.2340(2) 0.5143(3) 0.4836(4) 0.0285(8) Uani 1 1 d U . .
O2 O 0.32967(15) 0.6187(5) 0.6742(2) 0.0424(5) Uani 1 1 d U . .
O3 O 0.2360(3) 0.7247(3) 0.4828(3) 0.0279(8) Uani 1 1 d U . .
O4 O 0.19733(11) 0.6202(5) 0.26696(17) 0.0268(4) Uani 1 1 d U . .
O5 O 0.03235(12) 0.6192(7) 0.17295(19) 0.0458(6) Uani 1 1 d U . .
O6 O 0.09107(11) 0.6201(5) 0.42025(17) 0.0280(4) Uani 1 1 d U . .
O7 O 0.3361(4) 0.4159(4) 0.6722(5) 0.0576(16) Uani 1 1 d U . .
H7 H 0.3180 0.3600 0.6170 0.086 Uiso 1 1 calc R . .
O8 O 0.3340(4) 0.8224(4) 0.6752(5) 0.0518(14) Uani 1 1 d U . .
H8 H 0.3008 0.8799 0.6412 0.078 Uiso 1 1 calc R . .
O9 O 0.13881(12) 0.6201(6) 0.02546(18) 0.0404(5) Uani 1 1 d U . .
H9 H 0.0896 0.6389 -0.0337 0.061 Uiso 1 1 calc R . .
O10 O -0.07180(15) 0.6196(11) 0.3158(2) 0.0876(14) Uani 1 1 d U . .
H10 H -0.0762 0.6506 0.3915 0.131 Uiso 1 1 calc R . .
N11 N 0.3632(14) 0.6211(18) 0.1289(19) 0.050(4) Uani 0.225(3) 1 d PDU A 1
H11 H 0.3132 0.6074 0.1694 0.059 Uiso 0.225(3) 1 calc PR A 1
C12 C 0.4538(17) 0.625(2) 0.242(2) 0.051(5) Uani 0.225(3) 1 d PDU A 1
H12A H 0.4639 0.5494 0.2931 0.061 Uiso 0.225(3) 1 calc PR A 1
H12B H 0.5075 0.6386 0.1996 0.061 Uiso 0.225(3) 1 calc PR A 1
C13 C 0.446(2) 0.721(2) 0.3399(17) 0.066(5) Uani 0.225(3) 1 d PDU A 1
H13A H 0.4012 0.6965 0.3958 0.079 Uiso 0.225(3) 1 calc PR A 1
H13B H 0.5074 0.7320 0.4061 0.079 Uiso 0.225(3) 1 calc PR A 1
C14 C 0.415(3) 0.835(2) 0.278(3) 0.079(6) Uani 0.225(3) 1 d PDU A 1
H14A H 0.4706 0.8772 0.2643 0.094 Uiso 0.225(3) 1 calc PR A 1
H14B H 0.3899 0.8801 0.3472 0.094 Uiso 0.225(3) 1 calc PR A 1
C15 C 0.341(2) 0.837(2) 0.139(3) 0.070(5) Uani 0.225(3) 1 d PDU A 1
H15A H 0.2777 0.8376 0.1579 0.084 Uiso 0.225(3) 1 calc PR A 1
H15B H 0.3478 0.9097 0.0877 0.084 Uiso 0.225(3) 1 calc PR A 1
C16 C 0.349(2) 0.7360(19) 0.050(2) 0.057(4) Uani 0.225(3) 1 d PDU A 1
H16A H 0.4018 0.7489 0.0060 0.069 Uiso 0.225(3) 1 calc PR A 1
H16B H 0.2910 0.7306 -0.0266 0.069 Uiso 0.225(3) 1 calc PR A 1
C17 C 0.3643(18) 0.5304(17) 0.019(2) 0.052(4) Uani 0.225(3) 1 d PDU A 1
H17A H 0.2995 0.5161 -0.0363 0.062 Uiso 0.225(3) 1 calc PR A 1
H17B H 0.4009 0.5600 -0.0465 0.062 Uiso 0.225(3) 1 calc PR A 1
C18 C 0.405(2) 0.4205(19) 0.081(3) 0.062(5) Uani 0.225(3) 1 d PDU A 1
H18A H 0.4706 0.4324 0.1349 0.075 Uiso 0.225(3) 1 calc PR A 1
H18B H 0.4048 0.3614 0.0070 0.075 Uiso 0.225(3) 1 calc PR A 1
O19 O 0.3420(12) 0.3819(13) 0.1783(17) 0.041(3) Uani 0.225(3) 1 d PDU A 1
H19 H 0.2868 0.3733 0.1306 0.061 Uiso 0.225(3) 1 calc PR A 1
N21 N 0.3551(19) 0.6455(15) 0.152(2) 0.049(4) Uani 0.221(7) 1 d PDU B 2
H21 H 0.3052 0.6262 0.1907 0.059 Uiso 0.221(7) 1 calc PR B 2
C22 C 0.4438(19) 0.625(2) 0.265(3) 0.046(5) Uani 0.221(7) 1 d PDU B 2
H22A H 0.4502 0.6850 0.3390 0.056 Uiso 0.221(7) 1 calc PR B 2
H22B H 0.4990 0.6297 0.2241 0.056 Uiso 0.221(7) 1 calc PR B 2
C23 C 0.4379(19) 0.505(2) 0.326(2) 0.058(5) Uani 0.221(7) 1 d PDU B 2
H23A H 0.5009 0.4693 0.3476 0.070 Uiso 0.221(7) 1 calc PR B 2
H23B H 0.4189 0.5136 0.4158 0.070 Uiso 0.221(7) 1 calc PR B 2
C24 C 0.371(2) 0.426(2) 0.233(3) 0.075(5) Uani 0.221(7) 1 d PDU B 2
H24A H 0.3082 0.4385 0.2491 0.090 Uiso 0.221(7) 1 calc PR B 2
H24B H 0.3898 0.3443 0.2597 0.090 Uiso 0.221(7) 1 calc PR B 2
C25 C 0.367(3) 0.4424(19) 0.077(3) 0.064(5) Uani 0.221(7) 1 d PDU B 2
H25A H 0.4264 0.4149 0.0579 0.076 Uiso 0.221(7) 1 calc PR B 2
H25B H 0.3158 0.3933 0.0218 0.076 Uiso 0.221(7) 1 calc PR B 2
C26 C 0.351(3) 0.5647(19) 0.030(2) 0.055(5) Uani 0.221(7) 1 d PDU B 2
H26A H 0.2887 0.5714 -0.0368 0.066 Uiso 0.221(7) 1 calc PR B 2
H26B H 0.3990 0.5880 -0.0204 0.066 Uiso 0.221(7) 1 calc PR B 2
C27 C 0.3408(17) 0.7692(16) 0.103(2) 0.053(5) Uani 0.221(7) 1 d PDU B 2
H27A H 0.3279 0.7711 -0.0011 0.063 Uiso 0.221(7) 1 calc PR B 2
H27B H 0.2858 0.8023 0.1305 0.063 Uiso 0.221(7) 1 calc PR B 2
C28 C 0.423(2) 0.840(3) 0.162(3) 0.068(5) Uani 0.221(7) 1 d PDU B 2
H28A H 0.4141 0.9194 0.1202 0.082 Uiso 0.221(7) 1 calc PR B 2
H28B H 0.4785 0.8052 0.1370 0.082 Uiso 0.221(7) 1 calc PR B 2
O29 O 0.441(2) 0.850(3) 0.323(3) 0.135(10) Uani 0.221(7) 1 d PDU B 2
H29 H 0.4988 0.8574 0.3581 0.203 Uiso 0.221(7) 1 calc PR B 2
N31 N 0.3552(14) 0.5912(11) 0.1603(18) 0.035(3) Uani 0.250(6) 1 d PDU C 3
H31 H 0.2988 0.6117 0.1811 0.043 Uiso 0.250(6) 1 calc PR C 3
C32 C 0.356(2) 0.6589(16) 0.0276(18) 0.048(4) Uani 0.250(6) 1 d PDU C 3
H32A H 0.4174 0.6478 0.0038 0.058 Uiso 0.250(6) 1 calc PR C 3
H32B H 0.3067 0.6289 -0.0513 0.058 Uiso 0.250(6) 1 calc PR C 3
C33 C 0.341(2) 0.7864(17) 0.048(2) 0.062(5) Uani 0.250(6) 1 d PDU C 3
H33A H 0.3881 0.8307 0.0134 0.074 Uiso 0.250(6) 1 calc PR C 3
H33B H 0.2786 0.8075 -0.0116 0.074 Uiso 0.250(6) 1 calc PR C 3
C34 C 0.3439(19) 0.8266(19) 0.191(2) 0.060(5) Uani 0.250(6) 1 d PDU C 3
H34A H 0.2823 0.8131 0.2121 0.072 Uiso 0.250(6) 1 calc PR C 3
H34B H 0.3567 0.9114 0.1971 0.072 Uiso 0.250(6) 1 calc PR C 3
C35 C 0.4198(19) 0.7623(17) 0.298(2) 0.058(5) Uani 0.250(6) 1 d PDU C 3
H35A H 0.4808 0.7985 0.2977 0.069 Uiso 0.250(6) 1 calc PR C 3
H35B H 0.4083 0.7759 0.3921 0.069 Uiso 0.250(6) 1 calc PR C 3
C36 C 0.4284(18) 0.6364(17) 0.280(2) 0.055(4) Uani 0.250(6) 1 d PDU C 3
H36A H 0.4234 0.5961 0.3671 0.065 Uiso 0.250(6) 1 calc PR C 3
H36B H 0.4910 0.6190 0.2641 0.065 Uiso 0.250(6) 1 calc PR C 3
C37 C 0.3497(13) 0.4640(14) 0.142(3) 0.063(4) Uani 0.250(6) 1 d PDU C 3
H37A H 0.3033 0.4322 0.1900 0.075 Uiso 0.250(6) 1 calc PR C 3
H37B H 0.3279 0.4457 0.0406 0.075 Uiso 0.250(6) 1 calc PR C 3
C38 C 0.4395(15) 0.408(2) 0.197(3) 0.067(5) Uani 0.250(6) 1 d PDU C 3
H38A H 0.4320 0.3225 0.1902 0.080 Uiso 0.250(6) 1 calc PR C 3
H38B H 0.4628 0.4289 0.2973 0.080 Uiso 0.250(6) 1 calc PR C 3
O39 O 0.5105(12) 0.447(2) 0.1155(19) 0.100(6) Uani 0.250(6) 1 d PDU C 3
H39 H 0.5427 0.3898 0.1021 0.149 Uiso 0.250(6) 1 calc PR C 3
N41 N 0.3715(10) 0.6448(11) 0.1885(14) 0.052(3) Uani 0.304(7) 1 d PDU D 4
H41 H 0.3118 0.6453 0.2046 0.062 Uiso 0.304(7) 1 calc PR D 4
C42 C 0.3652(15) 0.6029(15) 0.0390(14) 0.054(3) Uani 0.304(7) 1 d PDU D 4
H42A H 0.3159 0.6467 -0.0279 0.065 Uiso 0.304(7) 1 calc PR D 4
H42B H 0.4256 0.6158 0.0136 0.065 Uiso 0.304(7) 1 calc PR D 4
C43 C 0.3419(16) 0.4745(16) 0.033(2) 0.064(5) Uani 0.304(7) 1 d PDU D 4
H43A H 0.2781 0.4644 0.0479 0.077 Uiso 0.304(7) 1 calc PR D 4
H43B H 0.3411 0.4449 -0.0620 0.077 Uiso 0.304(7) 1 calc PR D 4
C44 C 0.4080(16) 0.4032(18) 0.138(2) 0.072(5) Uani 0.304(7) 1 d PDU D 4
H44A H 0.4721 0.4106 0.1229 0.087 Uiso 0.304(7) 1 calc PR D 4
H44B H 0.3895 0.3200 0.1274 0.087 Uiso 0.304(7) 1 calc PR D 4
C45 C 0.4060(17) 0.4475(15) 0.2863(18) 0.068(5) Uani 0.304(7) 1 d PDU D 4
H45A H 0.3422 0.4390 0.3014 0.081 Uiso 0.304(7) 1 calc PR D 4
H45B H 0.4497 0.4011 0.3585 0.081 Uiso 0.304(7) 1 calc PR D 4
C46 C 0.4339(14) 0.5710(14) 0.2977(19) 0.065(4) Uani 0.304(7) 1 d PDU D 4
H46A H 0.4992 0.5778 0.2879 0.079 Uiso 0.304(7) 1 calc PR D 4
H46B H 0.4322 0.6003 0.3918 0.079 Uiso 0.304(7) 1 calc PR D 4
C47 C 0.4092(16) 0.7657(14) 0.2026(17) 0.079(4) Uani 0.304(7) 1 d PDU D 4
H47A H 0.3808 0.8064 0.2712 0.094 Uiso 0.304(7) 1 calc PR D 4
H47B H 0.4772 0.7600 0.2456 0.094 Uiso 0.304(7) 1 calc PR D 4
C48 C 0.3983(18) 0.8391(16) 0.0851(18) 0.063(4) Uani 0.304(7) 1 d PDU D 4
H48A H 0.4282 0.9145 0.1187 0.076 Uiso 0.304(7) 1 calc PR D 4
H48B H 0.3305 0.8545 0.0505 0.076 Uiso 0.304(7) 1 calc PR D 4
O49 O 0.4346(9) 0.8030(14) -0.0398(11) 0.080(4) Uani 0.304(7) 1 d PDU D 4
H49 H 0.3893 0.7928 -0.1094 0.120 Uiso 0.304(7) 1 calc PR D 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 O3 1.447(7) . ?
B1 O4 1.468(3) . ?
B1 O6 1.473(3) . ?
B1 O1 1.480(8) . ?
B2 O2 1.341(9) . ?
B2 O1 1.374(6) . ?
B2 O7 1.370(8) . ?
B3 O8 1.338(9) . ?
B3 O3 1.339(7) . ?
B3 O2 1.412(9) . ?
B4 O9 1.348(3) . ?
B4 O4 1.352(3) . ?
B4 O5 1.385(3) . ?
B5 O6 1.341(3) . ?
B5 O10 1.345(4) . ?
B5 O5 1.390(4) . ?
O7 H7 0.8400 . ?
O8 H8 0.8400 . ?
O9 H9 0.8400 . ?
O10 H10 0.8400 . ?
N11 C17 1.505(14) . ?
N11 C12 1.517(14) . ?
N11 C16 1.517(16) . ?
N11 H11 0.9300 . ?
C12 C13 1.494(16) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.462(16) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.528(16) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.473(16) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.464(16) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 O19 1.553(17) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
O19 H19 0.8400 . ?
N21 C27 1.498(14) . ?
N21 C26 1.508(16) . ?
N21 C22 1.512(14) . ?
N21 H21 0.9300 . ?
C22 C23 1.510(16) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.477(16) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.532(17) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.478(16) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.458(16) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 O29 1.547(17) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
O29 H29 0.8400 . ?
N31 C37 1.469(13) . ?
N31 C36 1.484(15) . ?
N31 C32 1.520(14) . ?
N31 H31 0.9300 . ?
C32 C33 1.502(15) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.460(16) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.529(16) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.463(15) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C38 1.451(15) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 O39 1.528(17) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
O39 H39 0.8400 . ?
N41 C47 1.486(14) . ?
N41 C46 1.495(14) . ?
N41 C42 1.526(12) . ?
N41 H41 0.9300 . ?
C42 C43 1.510(15) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.479(15) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.553(16) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C46 1.470(16) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.405(15) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 O49 1.508(15) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
O49 H49 0.8400 . ?
 
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
O3 B1 O4 109.5(4) . . ?
O3 B1 O6 110.0(5) . . ?
O4 B1 O6 110.52(18) . . ?
O3 B1 O1 110.92(19) . . ?
O4 B1 O1 108.6(4) . . ?
O6 B1 O1 107.2(4) . . ?
O2 B2 O1 122.2(5) . . ?
O2 B2 O7 118.2(4) . . ?
O1 B2 O7 119.6(6) . . ?
O8 B3 O3 124.1(6) . . ?
O8 B3 O2 116.2(5) . . ?
O3 B3 O2 119.8(6) . . ?
O9 B4 O4 118.5(2) . . ?
O9 B4 O5 120.7(2) . . ?
O4 B4 O5 120.8(2) . . ?
O6 B5 O10 123.7(3) . . ?
O6 B5 O5 120.8(2) . . ?
O10 B5 O5 115.5(2) . . ?
B2 O1 B1 121.8(4) . . ?
B2 O2 B3 119.4(2) . . ?
B3 O3 B1 125.0(5) . . ?
B4 O4 B1 124.1(2) . . ?
B4 O5 B5 119.3(2) . . ?
B5 O6 B1 124.4(2) . . ?
B2 O7 H7 109.5 . . ?
B3 O8 H8 109.5 . . ?
B4 O9 H9 109.5 . . ?
B5 O10 H10 109.5 . . ?
C17 N11 C12 112.6(13) . . ?
C17 N11 C16 104.8(13) . . ?
C12 N11 C16 110.1(14) . . ?
C17 N11 H11 109.8 . . ?
C12 N11 H11 109.8 . . ?
C16 N11 H11 109.8 . . ?
C13 C12 N11 107.3(13) . . ?
C13 C12 H12A 110.3 . . ?
N11 C12 H12A 110.3 . . ?
C13 C12 H12B 110.3 . . ?
N11 C12 H12B 110.3 . . ?
H12A C12 H12B 108.5 . . ?
C14 C13 C12 117.4(15) . . ?
C14 C13 H13A 108.0 . . ?
C12 C13 H13A 108.0 . . ?
C14 C13 H13B 108.0 . . ?
C12 C13 H13B 108.0 . . ?
H13A C13 H13B 107.2 . . ?
C13 C14 C15 117.9(16) . . ?
C13 C14 H14A 107.8 . . ?
C15 C14 H14A 107.8 . . ?
C13 C14 H14B 107.8 . . ?
C15 C14 H14B 107.8 . . ?
H14A C14 H14B 107.2 . . ?
C16 C15 C14 112.3(16) . . ?
C16 C15 H15A 109.1 . . ?
C14 C15 H15A 109.1 . . ?
C16 C15 H15B 109.1 . . ?
C14 C15 H15B 109.1 . . ?
H15A C15 H15B 107.9 . . ?
C15 C16 N11 113.6(15) . . ?
C15 C16 H16A 108.9 . . ?
N11 C16 H16A 108.9 . . ?
C15 C16 H16B 108.9 . . ?
N11 C16 H16B 108.9 . . ?
H16A C16 H16B 107.7 . . ?
C18 C17 N11 111.7(14) . . ?
C18 C17 H17A 109.3 . . ?
N11 C17 H17A 109.3 . . ?
C18 C17 H17B 109.3 . . ?
N11 C17 H17B 109.3 . . ?
H17A C17 H17B 107.9 . . ?
C17 C18 O19 104.7(15) . . ?
C17 C18 H18A 110.8 . . ?
O19 C18 H18A 110.8 . . ?
C17 C18 H18B 110.8 . . ?
O19 C18 H18B 110.8 . . ?
H18A C18 H18B 108.9 . . ?
C27 N21 C26 110.2(15) . . ?
C27 N21 C22 114.5(14) . . ?
C26 N21 C22 110.6(15) . . ?
C27 N21 H21 107.1 . . ?
C26 N21 H21 107.1 . . ?
C22 N21 H21 107.1 . . ?
N21 C22 C23 108.2(13) . . ?
N21 C22 H22A 110.1 . . ?
C23 C22 H22A 110.1 . . ?
N21 C22 H22B 110.1 . . ?
C23 C22 H22B 110.1 . . ?
H22A C22 H22B 108.4 . . ?
C24 C23 C22 113.9(13) . . ?
C24 C23 H23A 108.8 . . ?
C22 C23 H23A 108.8 . . ?
C24 C23 H23B 108.8 . . ?
C22 C23 H23B 108.8 . . ?
H23A C23 H23B 107.7 . . ?
C23 C24 C25 113.9(16) . . ?
C23 C24 H24A 108.8 . . ?
C25 C24 H24A 108.8 . . ?
C23 C24 H24B 108.8 . . ?
C25 C24 H24B 108.8 . . ?
H24A C24 H24B 107.7 . . ?
C26 C25 C24 113.5(15) . . ?
C26 C25 H25A 108.9 . . ?
C24 C25 H25A 108.9 . . ?
C26 C25 H25B 108.9 . . ?
C24 C25 H25B 108.9 . . ?
H25A C25 H25B 107.7 . . ?
C25 C26 N21 110.9(13) . . ?
C25 C26 H26A 109.5 . . ?
N21 C26 H26A 109.5 . . ?
C25 C26 H26B 109.4 . . ?
N21 C26 H26B 109.5 . . ?
H26A C26 H26B 108.0 . . ?
C28 C27 N21 111.1(15) . . ?
C28 C27 H27A 109.4 . . ?
N21 C27 H27A 109.4 . . ?
C28 C27 H27B 109.4 . . ?
N21 C27 H27B 109.4 . . ?
H27A C27 H27B 108.0 . . ?
C27 C28 O29 111.6(16) . . ?
C27 C28 H28A 109.3 . . ?
O29 C28 H28A 109.3 . . ?
C27 C28 H28B 109.3 . . ?
O29 C28 H28B 109.3 . . ?
H28A C28 H28B 108.0 . . ?
C28 O29 H29 109.5 . . ?
C37 N31 C36 116.9(13) . . ?
C37 N31 C32 114.3(14) . . ?
C36 N31 C32 110.2(13) . . ?
C37 N31 H31 104.7 . . ?
C36 N31 H31 104.7 . . ?
C32 N31 H31 104.7 . . ?
C33 C32 N31 110.3(12) . . ?
C33 C32 H32A 109.6 . . ?
N31 C32 H32A 109.6 . . ?
C33 C32 H32B 109.6 . . ?
N31 C32 H32B 109.6 . . ?
H32A C32 H32B 108.1 . . ?
C34 C33 C32 117.8(13) . . ?
C34 C33 H33A 107.9 . . ?
C32 C33 H33A 107.9 . . ?
C34 C33 H33B 107.9 . . ?
C32 C33 H33B 107.9 . . ?
H33A C33 H33B 107.2 . . ?
C33 C34 C35 111.0(15) . . ?
C33 C34 H34A 109.4 . . ?
C35 C34 H34A 109.4 . . ?
C33 C34 H34B 109.4 . . ?
C35 C34 H34B 109.4 . . ?
H34A C34 H34B 108.0 . . ?
C36 C35 C34 117.5(14) . . ?
C36 C35 H35A 107.9 . . ?
C34 C35 H35A 107.9 . . ?
C36 C35 H35B 107.9 . . ?
C34 C35 H35B 107.9 . . ?
H35A C35 H35B 107.2 . . ?
C35 C36 N31 111.9(12) . . ?
C35 C36 H36A 109.2 . . ?
N31 C36 H36A 109.2 . . ?
C35 C36 H36B 109.2 . . ?
N31 C36 H36B 109.2 . . ?
H36A C36 H36B 107.9 . . ?
C38 C37 N31 111.9(14) . . ?
C38 C37 H37A 109.2 . . ?
N31 C37 H37A 109.2 . . ?
C38 C37 H37B 109.2 . . ?
N31 C37 H37B 109.2 . . ?
H37A C37 H37B 107.9 . . ?
C37 C38 O39 110.5(15) . . ?
C37 C38 H38A 109.5 . . ?
O39 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
O39 C38 H38B 109.5 . . ?
H38A C38 H38B 108.1 . . ?
C47 N41 C46 108.0(12) . . ?
C47 N41 C42 108.5(11) . . ?
C46 N41 C42 113.4(12) . . ?
C47 N41 H41 108.9 . . ?
C46 N41 H41 108.9 . . ?
C42 N41 H41 108.9 . . ?
C43 C42 N41 107.8(11) . . ?
C43 C42 H42A 110.2 . . ?
N41 C42 H42A 110.2 . . ?
C43 C42 H42B 110.2 . . ?
N41 C42 H42B 110.2 . . ?
H42A C42 H42B 108.5 . . ?
C44 C43 C42 113.9(15) . . ?
C44 C43 H43A 108.8 . . ?
C42 C43 H43A 108.8 . . ?
C44 C43 H43B 108.8 . . ?
C42 C43 H43B 108.8 . . ?
H43A C43 H43B 107.7 . . ?
C43 C44 C45 108.3(14) . . ?
C43 C44 H44A 110.0 . . ?
C45 C44 H44A 110.0 . . ?
C43 C44 H44B 110.0 . . ?
C45 C44 H44B 110.0 . . ?
H44A C44 H44B 108.4 . . ?
C46 C45 C44 108.5(14) . . ?
C46 C45 H45A 110.0 . . ?
C44 C45 H45A 110.0 . . ?
C46 C45 H45B 110.0 . . ?
C44 C45 H45B 110.0 . . ?
H45A C45 H45B 108.4 . . ?
C45 C46 N41 112.2(12) . . ?
C45 C46 H46A 109.2 . . ?
N41 C46 H46A 109.2 . . ?
C45 C46 H46B 109.2 . . ?
N41 C46 H46B 109.2 . . ?
H46A C46 H46B 107.9 . . ?
C48 C47 N41 121.0(14) . . ?
C48 C47 H47A 107.1 . . ?
N41 C47 H47A 107.1 . . ?
C48 C47 H47B 107.1 . . ?
N41 C47 H47B 107.1 . . ?
H47A C47 H47B 106.8 . . ?
C47 C48 O49 120.7(15) . . ?
C47 C48 H48A 107.1 . . ?
O49 C48 H48A 107.1 . . ?
C47 C48 H48B 107.1 . . ?
O49 C48 H48B 107.1 . . ?
H48A C48 H48B 106.8 . . ?
 
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 O3  0.84 1.90 2.732(6) 169.2 4_546
O8 H8 O1  0.84 1.96 2.742(6) 154.9 4_556
O9 H9 O5  0.84 1.99 2.789(3) 158.6 2
O10 H10 O6  0.84 1.94 2.674(3) 144.6 2_556
N11 H11 O4  0.93 2.15 3.06(2) 166.3 .
N21 H21 O4  0.93 1.91 2.83(3) 168.3 .
O29 H29 O8  0.84 2.59 3.32(4) 145.9 2_656
N31 H31 O4  0.93 1.89 2.79(2) 162.6 .
N41 H41 O4  0.93 1.95 2.862(15) 167.7 .
O49 H49 O8  0.84 2.10 2.842(11) 146.7 1_554
 
_diffrn_measured_fraction_theta_max    0.996
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.996
_refine_diff_density_max    0.375
_refine_diff_density_min   -0.280
_refine_diff_density_rms    0.057
