# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2013


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#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
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#  fide research purposes only. It may contain copyright material 
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data_1
_database_code_depnum_ccdc_archive 'CCDC 892451'
#TrackingRef 'BO.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H36 B14 N6 O26'
_chemical_formula_weight         783.77
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   P21/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                   9.4493(7)
_cell_length_b                   8.7865(5)
_cell_length_c                   21.4735(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.836(5)
_cell_angle_gamma                90.00
_cell_volume                     1630.80(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3285
_cell_measurement_theta_min      2.0736
_cell_measurement_theta_max      27.4565
_exptl_crystal_description       Bulk
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.3000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.1500
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             808
_exptl_absorpt_coefficient_mu    0.143
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7544
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Mercury2 (1x1 bin mode) '
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            12453
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.07
_diffrn_reflns_theta_max         27.47
_reflns_number_total             3692
_reflns_number_gt                3008
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.1500P)^2^+2.6155P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3692
_refine_ls_number_parameters     244
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0896
_refine_ls_wR_factor_ref         0.2735
_refine_ls_wR_factor_gt          0.2532
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.001
_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
O1 O 0.4336(4) -0.3259(3) -0.05841(16) 0.0497(8) Uani 1 1 d . . .
H1A H 0.4294 -0.3668 -0.0249 0.060 Uiso 1 1 d R . .
O2 O 0.5880(3) -0.7687(2) -0.11733(12) 0.0327(6) Uani 1 1 d . . .
O3 O 0.5856(3) -0.3291(3) -0.11995(14) 0.0383(6) Uani 1 1 d . . .
O4 O 0.6839(3) -0.3502(3) -0.20456(12) 0.0344(6) Uani 1 1 d . . .
O5 O 0.7345(3) -0.5519(2) -0.12280(12) 0.0293(5) Uani 1 1 d . . .
O6 O 0.8160(3) -0.6929(2) -0.01788(12) 0.0309(6) Uani 1 1 d . . .
O7 O 0.5869(3) -0.5448(3) -0.05325(12) 0.0336(6) Uani 1 1 d . . .
O8 O 0.5212(5) -1.0242(3) -0.13371(18) 0.0808(14) Uani 1 1 d . . .
H8A H 0.5623 -1.1074 -0.1212 0.097 Uiso 1 1 d R . .
O9 O 0.8549(3) -0.1392(3) -0.17124(13) 0.0443(7) Uani 1 1 d . . .
O10 O 0.9519(3) -0.8843(3) 0.06217(13) 0.0459(8) Uani 1 1 d . . .
O11 O 0.7378(3) -0.9519(3) -0.03530(15) 0.0514(8) Uani 1 1 d . . .
O12 O 0.6769(3) -0.1564(3) -0.28312(13) 0.0454(7) Uani 1 1 d . . .
H12A H 0.5979 -0.2019 -0.3072 0.054 Uiso 1 1 d R . .
O13 O 0.8603(3) -0.3131(3) -0.08596(12) 0.0352(6) Uani 1 1 d . . .
B1 B 0.7147(4) -0.3903(4) -0.13378(18) 0.0289(7) Uani 1 1 d . . .
B2 B 0.6815(4) -0.6375(4) -0.07927(18) 0.0269(7) Uani 1 1 d . . .
B3 B 0.5355(5) -0.4027(4) -0.0773(2) 0.0326(8) Uani 1 1 d . . .
B4 B 0.7352(4) -0.2185(4) -0.22019(19) 0.0313(8) Uani 1 1 d . . .
B5 B 0.8353(4) -0.8395(4) 0.00260(19) 0.0334(8) Uani 1 1 d . . .
B6 B 0.6163(5) -0.9131(5) -0.0955(2) 0.0422(10) Uani 1 1 d . . .
B7 B 0.9197(5) -0.1930(4) -0.1055(2) 0.0353(9) Uani 1 1 d . . .
N1 N -0.0347(4) -0.8118(4) -0.1638(2) 0.0509(9) Uani 1 1 d . . .
H1D H -0.0989 -0.8403 -0.1469 0.061 Uiso 1 1 d R . .
N2 N 0.0761(4) -0.5904(4) -0.05383(16) 0.0396(7) Uani 1 1 d . . .
H2C H 0.1091 -0.4989 -0.0361 0.048 Uiso 1 1 d R . .
H2D H -0.0230 -0.5848 -0.0825 0.048 Uiso 1 1 d R . .
H2E H 0.0863 -0.6556 -0.0206 0.048 Uiso 1 1 d R . .
N3 N -0.3376(4) -0.6838(4) -0.25060(16) 0.0429(8) Uani 1 1 d . . .
H3C H -0.4189 -0.6509 -0.2867 0.051 Uiso 1 1 d R . .
H3D H -0.3657 -0.7622 -0.2319 0.051 Uiso 1 1 d R . .
H3E H -0.3024 -0.6090 -0.2202 0.051 Uiso 1 1 d R . .
C1 C 0.1691(7) -0.6448(9) -0.0907(4) 0.096(3) Uani 1 1 d . . .
H1B H 0.1614 -0.5708 -0.1255 0.116 Uiso 1 1 calc R . .
H1C H 0.2768 -0.6497 -0.0590 0.116 Uiso 1 1 calc R . .
C2 C 0.1244(6) -0.7895(6) -0.1220(3) 0.0662(14) Uani 1 1 d . . .
H2A H 0.1826 -0.8086 -0.1495 0.079 Uiso 1 1 calc R . .
H2B H 0.1554 -0.8659 -0.0864 0.079 Uiso 1 1 calc R . .
C3 C -0.0850(7) -0.7843(11) -0.2361(3) 0.094(2) Uani 1 1 d . . .
H3A H -0.0102 -0.7159 -0.2416 0.113 Uiso 1 1 calc R . .
H3B H -0.0772 -0.8802 -0.2568 0.113 Uiso 1 1 calc R . .
C4 C -0.2184(11) -0.730(2) -0.2713(4) 0.202(8) Uani 1 1 d . . .
H4A H -0.2671 -0.8049 -0.3069 0.242 Uiso 1 1 calc R . .
H4B H -0.1994 -0.6419 -0.2939 0.242 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0628(18) 0.0418(15) 0.0538(17) 0.0165(13) 0.0332(15) 0.0236(13)
O2 0.0316(11) 0.0208(10) 0.0311(12) 0.0016(9) -0.0023(9) -0.0025(9)
O3 0.0426(14) 0.0259(11) 0.0485(15) 0.0125(10) 0.0205(12) 0.0092(10)
O4 0.0377(12) 0.0323(12) 0.0233(11) 0.0032(9) 0.0022(10) -0.0084(10)
O5 0.0310(11) 0.0235(11) 0.0298(12) 0.0049(9) 0.0084(9) 0.0018(8)
O6 0.0304(11) 0.0219(10) 0.0268(11) 0.0015(8) -0.0025(9) -0.0030(8)
O7 0.0414(13) 0.0254(11) 0.0340(12) 0.0058(9) 0.0153(11) 0.0042(9)
O8 0.084(2) 0.0262(14) 0.065(2) 0.0108(13) -0.0395(18) -0.0173(14)
O9 0.0407(14) 0.0385(14) 0.0318(14) 0.0114(11) -0.0080(11) -0.0149(11)
O10 0.0428(14) 0.0290(12) 0.0366(14) 0.0098(10) -0.0142(11) -0.0100(10)
O11 0.0486(16) 0.0253(12) 0.0443(16) 0.0093(11) -0.0184(12) -0.0064(11)
O12 0.0441(14) 0.0476(15) 0.0261(13) 0.0097(11) -0.0048(11) -0.0173(12)
O13 0.0373(13) 0.0303(12) 0.0250(12) 0.0033(9) -0.0010(10) -0.0082(10)
B1 0.0290(16) 0.0247(16) 0.0258(17) 0.0021(13) 0.0036(13) -0.0025(13)
B2 0.0282(16) 0.0194(15) 0.0254(16) 0.0050(12) 0.0028(13) 0.0015(12)
B3 0.0361(19) 0.0261(17) 0.0307(18) 0.0041(14) 0.0083(15) 0.0041(14)
B4 0.0280(16) 0.0297(17) 0.0280(18) 0.0036(14) 0.0028(14) -0.0040(14)
B5 0.0336(18) 0.0247(16) 0.0275(18) 0.0013(13) -0.0027(15) -0.0039(14)
B6 0.043(2) 0.0238(17) 0.036(2) 0.0016(15) -0.0079(17) -0.0010(15)
B7 0.0334(18) 0.0266(17) 0.0300(19) 0.0059(14) -0.0037(15) -0.0031(14)
N1 0.0443(18) 0.051(2) 0.054(2) 0.0007(16) 0.0160(17) -0.0016(15)
N2 0.0366(15) 0.0415(16) 0.0353(16) -0.0063(13) 0.0088(13) -0.0047(13)
N3 0.0436(17) 0.0447(18) 0.0304(16) -0.0029(13) 0.0047(13) 0.0039(14)
C1 0.050(3) 0.140(6) 0.099(5) -0.075(5) 0.031(3) -0.029(3)
C2 0.056(3) 0.063(3) 0.080(4) -0.025(3) 0.027(3) -0.005(2)
C3 0.062(3) 0.164(7) 0.063(4) 0.019(4) 0.032(3) 0.039(4)
C4 0.107(6) 0.43(2) 0.047(3) 0.013(7) 0.011(4) 0.159(10)
_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
O1 B3 1.365(5) . ?
O1 H1A 0.8202 . ?
O2 B6 1.341(4) . ?
O2 B2 1.481(4) . ?
O3 B3 1.354(5) . ?
O3 B1 1.470(5) . ?
O4 B4 1.348(4) . ?
O4 B1 1.470(4) . ?
O5 B2 1.439(4) . ?
O5 B1 1.439(4) . ?
O6 B5 1.349(4) . ?
O6 B2 1.495(4) . ?
O7 B3 1.363(4) . ?
O7 B2 1.476(4) . ?
O8 B6 1.356(5) . ?
O8 H8A 0.8200 . ?
O9 B7 1.375(4) . ?
O9 B4 1.382(4) . ?
O10 B5 1.366(4) . ?
O10 B7 1.374(4) 3_745 ?
O11 B5 1.372(4) . ?
O11 B6 1.380(4) . ?
O12 B4 1.351(4) . ?
O12 H12A 0.8200 . ?
O13 B7 1.340(5) . ?
O13 B1 1.505(4) . ?
B7 O10 1.374(4) 3_745 ?
N1 C2 1.418(6) . ?
N1 C3 1.449(7) . ?
N1 H1D 0.8600 . ?
N2 C1 1.480(7) . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N2 H2E 0.8900 . ?
N3 C4 1.428(8) . ?
N3 H3C 0.8900 . ?
N3 H3D 0.8901 . ?
N3 H3E 0.8900 . ?
C1 C2 1.421(8) . ?
C1 H1B 0.9700 . ?
C1 H1C 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.271(9) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
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
B3 O1 H1A 109.5 . . ?
B6 O2 B2 123.6(3) . . ?
B3 O3 B1 120.5(3) . . ?
B4 O4 B1 121.5(3) . . ?
B2 O5 B1 124.5(3) . . ?
B5 O6 B2 123.6(2) . . ?
B3 O7 B2 122.7(3) . . ?
B6 O8 H8A 109.5 . . ?
B7 O9 B4 119.7(3) . . ?
B5 O10 B7 130.5(3) . 3_745 ?
B5 O11 B6 118.8(3) . . ?
B4 O12 H12A 109.4 . . ?
B7 O13 B1 121.6(3) . . ?
O5 B1 O3 113.0(3) . . ?
O5 B1 O4 111.4(3) . . ?
O3 B1 O4 106.7(3) . . ?
O5 B1 O13 108.1(3) . . ?
O3 B1 O13 107.6(3) . . ?
O4 B1 O13 110.0(3) . . ?
O5 B2 O7 112.4(2) . . ?
O5 B2 O2 109.6(3) . . ?
O7 B2 O2 108.8(3) . . ?
O5 B2 O6 110.3(3) . . ?
O7 B2 O6 106.0(3) . . ?
O2 B2 O6 109.8(2) . . ?
O3 B3 O7 121.7(3) . . ?
O3 B3 O1 116.5(3) . . ?
O7 B3 O1 121.8(3) . . ?
O4 B4 O12 123.6(3) . . ?
O4 B4 O9 120.6(3) . . ?
O12 B4 O9 115.8(3) . . ?
O6 B5 O10 122.1(3) . . ?
O6 B5 O11 121.6(3) . . ?
O10 B5 O11 116.2(3) . . ?
O2 B6 O8 118.6(3) . . ?
O2 B6 O11 122.3(3) . . ?
O8 B6 O11 119.0(3) . . ?
O13 B7 O10 122.9(3) . 3_745 ?
O13 B7 O9 121.6(3) . . ?
O10 B7 O9 115.5(3) 3_745 . ?
C2 N1 C3 117.4(5) . . ?
C2 N1 H1D 121.4 . . ?
C3 N1 H1D 121.2 . . ?
C1 N2 H2C 109.8 . . ?
C1 N2 H2D 109.6 . . ?
H2C N2 H2D 109.5 . . ?
C1 N2 H2E 109.1 . . ?
H2C N2 H2E 109.5 . . ?
H2D N2 H2E 109.5 . . ?
C4 N3 H3C 109.5 . . ?
C4 N3 H3D 109.6 . . ?
H3C N3 H3D 109.5 . . ?
C4 N3 H3E 109.4 . . ?
H3C N3 H3E 109.5 . . ?
H3D N3 H3E 109.5 . . ?
C2 C1 N2 114.5(5) . . ?
C2 C1 H1B 108.6 . . ?
N2 C1 H1B 108.6 . . ?
C2 C1 H1C 108.6 . . ?
N2 C1 H1C 108.6 . . ?
H1B C1 H1C 107.6 . . ?
N1 C2 C1 117.3(5) . . ?
N1 C2 H2A 108.0 . . ?
C1 C2 H2A 108.0 . . ?
N1 C2 H2B 108.0 . . ?
C1 C2 H2B 108.0 . . ?
H2A C2 H2B 107.2 . . ?
C4 C3 N1 121.2(6) . . ?
C4 C3 H3A 107.0 . . ?
N1 C3 H3A 107.0 . . ?
C4 C3 H3B 107.0 . . ?
N1 C3 H3B 107.0 . . ?
H3A C3 H3B 106.8 . . ?
C3 C4 N3 129.7(7) . . ?
C3 C4 H4A 104.9 . . ?
N3 C4 H4A 104.9 . . ?
C3 C4 H4B 104.9 . . ?
N3 C4 H4B 104.9 . . ?
H4A C4 H4B 105.8 . . ?
_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.146
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.098


data_1a
_database_code_depnum_ccdc_archive 'CCDC 892452'
#TrackingRef 'BOAl.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H38 Al2 B10 N6 O24'
_chemical_formula_weight         764.50
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'
Al Al 0.0645 0.0514 '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   P21
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
_cell_length_a                   10.066(3)
_cell_length_b                   10.325(3)
_cell_length_c                   14.786(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.456(5)
_cell_angle_gamma                90.00
_cell_volume                     1536.2(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4931
_cell_measurement_theta_min      2.0239
_cell_measurement_theta_max      27.4971
_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.3000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.1500
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             792
_exptl_absorpt_coefficient_mu    0.200
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.3330
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            12100
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_sigmaI/netI    0.0845
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.02
_diffrn_reflns_theta_max         27.50
_reflns_number_total             6301
_reflns_number_gt                4875
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXL
_computing_publication_material  SHELXL
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0820P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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   -0.5(2)
_refine_ls_number_reflns         6301
_refine_ls_number_parameters     445
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0509
_refine_ls_wR_factor_ref         0.1603
_refine_ls_wR_factor_gt          0.1305
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.004
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
Al1 Al 1.49192(10) 0.79132(12) 1.24487(7) 0.0077(2) Uani 1 1 d . . .
Al2 Al 1.00632(10) 1.28320(12) 1.25595(7) 0.0080(2) Uani 1 1 d . . .
O1 O 1.3464(2) 0.9937(3) 1.02882(16) 0.0142(6) Uani 1 1 d . . .
O2 O 1.4278(2) 0.8528(3) 1.14250(17) 0.0136(6) Uani 1 1 d . . .
O3 O 1.2717(3) 1.0178(3) 1.17896(16) 0.0131(6) Uani 1 1 d . . .
O4 O 1.3883(3) 0.6685(3) 1.27943(17) 0.0176(6) Uani 1 1 d . . .
O5 O 1.1872(2) 1.1600(3) 1.06453(16) 0.0132(6) Uani 1 1 d . . .
O6 O 1.3146(2) 0.6538(3) 1.43150(16) 0.0130(6) Uani 1 1 d . . .
O7 O 1.1410(3) 1.1934(3) 1.22005(17) 0.0150(6) Uani 1 1 d . . .
O8 O 1.1672(3) 0.4768(3) 1.46863(17) 0.0165(6) Uani 1 1 d . . .
O9 O 1.2287(3) 0.5131(3) 1.31630(17) 0.0177(6) Uani 1 1 d . . .
O10 O 1.0569(2) 0.3633(3) 1.35406(16) 0.0141(6) Uani 1 1 d . . .
O11 O 1.1371(2) 1.0048(3) 0.94947(16) 0.0121(5) Uani 1 1 d . . .
O12 O 1.1977(2) 0.6548(3) 1.57038(16) 0.0125(6) Uani 1 1 d . . .
O14 O 1.0492(3) 0.8868(3) 0.82792(18) 0.0180(6) Uani 1 1 d . . .
O15 O 1.2104(3) 1.0524(3) 0.80152(17) 0.0170(6) Uani 1 1 d . . .
O17 O 1.3497(2) 1.2324(3) 0.77654(16) 0.0141(6) Uani 1 1 d . . .
O18 O 1.3033(2) 1.1703(3) 0.92703(15) 0.0136(6) Uani 1 1 d . . .
O19 O 1.1206(3) 0.6741(3) 1.72104(17) 0.0186(6) Uani 1 1 d . . .
O20 O 1.3780(2) 0.5022(3) 1.54652(16) 0.0129(6) Uani 1 1 d . . .
B1 B 1.3528(4) 0.9555(4) 1.1167(3) 0.0102(8) Uiso 1 1 d . . .
B2 B 1.3129(4) 0.6163(5) 1.3424(3) 0.0130(9) Uani 1 1 d . . .
B3 B 1.1968(4) 1.1287(4) 1.1536(3) 0.0110(8) Uani 1 1 d . . .
B4 B 1.1517(4) 0.4515(4) 1.3790(3) 0.0119(8) Uiso 1 1 d . . .
B5 B 1.2454(4) 1.0819(5) 0.9924(3) 0.0110(8) Uiso 1 1 d . . .
B6 B 1.2638(4) 0.5729(4) 1.5032(3) 0.0092(8) Uani 1 1 d . . .
B7 B 1.1324(4) 0.9785(4) 0.8597(3) 0.0111(8) Uani 1 1 d . . .
B9 B 1.2903(4) 1.1536(4) 0.8358(3) 0.0084(8) Uani 1 1 d . . .
B10 B 1.2028(4) 0.6285(4) 1.6602(3) 0.0112(8) Uani 1 1 d . . .
N1 N 1.0024(3) 0.7878(4) 1.4531(2) 0.0170(7) Uani 1 1 d . . .
H1A H 1.0356 0.8373 1.4090 0.020 Uiso 1 1 d R . .
H1B H 1.0695 0.7483 1.4836 0.020 Uiso 1 1 d R . .
H1C H 0.9568 0.8378 1.4913 0.020 Uiso 1 1 d R . .
N2 N 0.5330(3) 0.3288(4) 1.4523(2) 0.0184(8) Uani 1 1 d . . .
H2A H 0.4908 0.2591 1.4309 0.028 Uiso 1 1 calc R . .
H2B H 0.4770 0.3770 1.4836 0.028 Uiso 1 1 calc R . .
H2C H 0.6005 0.3042 1.4884 0.028 Uiso 1 1 calc R . .
N3 N 0.7824(3) 0.4901(4) 1.4551(2) 0.0217(8) Uani 1 1 d . . .
H3A H 0.7632 0.4398 1.5028 0.026 Uiso 1 1 d R . .
C1 C 0.5845(4) 0.4059(4) 1.3758(3) 0.0171(8) Uani 1 1 d . . .
H1D H 0.5107 0.4309 1.3361 0.020 Uiso 1 1 calc R . .
H1E H 0.6441 0.3524 1.3413 0.020 Uiso 1 1 calc R . .
C2 C 0.6577(4) 0.5264(4) 1.4074(3) 0.0192(9) Uani 1 1 d . . .
H2D H 0.6771 0.5805 1.3558 0.023 Uiso 1 1 calc R . .
H2E H 0.6022 0.5756 1.4477 0.023 Uiso 1 1 calc R . .
C5 C 0.8568(4) 0.6037(5) 1.4878(3) 0.0262(10) Uani 1 1 d . . .
H5D H 0.9302 0.5748 1.5266 0.031 Uiso 1 1 calc R . .
H5E H 0.7990 0.6567 1.5241 0.031 Uiso 1 1 calc R . .
C6 C 0.9118(4) 0.6869(5) 1.4113(3) 0.0211(9) Uani 1 1 d . . .
H6B H 0.9606 0.6331 1.3699 0.025 Uiso 1 1 calc R . .
H6C H 0.8394 0.7283 1.3778 0.025 Uiso 1 1 calc R . .
N4 N 1.4574(3) 0.3415(4) 1.0519(2) 0.0150(7) Uani 1 1 d . . .
H4A H 1.5270 0.2978 1.0742 0.023 Uiso 1 1 calc R . .
H4B H 1.4847 0.3993 1.0118 0.023 Uiso 1 1 calc R . .
H4C H 1.4007 0.2868 1.0249 0.023 Uiso 1 1 calc R . .
N5 N 1.0002(3) 0.8091(3) 1.0374(2) 0.0143(7) Uani 1 1 d . . .
H5A H 0.9493 0.8432 1.0805 0.017 Uiso 1 1 d R . .
H5B H 0.9493 0.7617 0.9990 0.017 Uiso 1 1 d R . .
H5C H 1.0394 0.8734 1.0067 0.017 Uiso 1 1 d R . .
N6 N 1.3058(3) 0.5945(4) 1.0384(2) 0.0162(7) Uani 1 1 d . . .
H6A H 1.3496 0.5643 0.9905 0.019 Uiso 1 1 d R . .
C8 C 1.1054(4) 0.7263(4) 1.0796(2) 0.0146(8) Uani 1 1 d . . .
H8A H 1.0651 0.6570 1.1138 0.018 Uiso 1 1 calc R . .
H8B H 1.1604 0.7775 1.1208 0.018 Uiso 1 1 calc R . .
C10 C 1.1897(4) 0.6699(4) 1.0057(2) 0.0164(8) Uani 1 1 d . . .
H10A H 1.1341 0.6143 0.9678 0.020 Uiso 1 1 calc R . .
H10B H 1.2207 0.7402 0.9682 0.020 Uiso 1 1 calc R . .
C12 C 1.2708(4) 0.4853(4) 1.0949(3) 0.0171(8) Uani 1 1 d . . .
H12A H 1.2112 0.4285 1.0610 0.021 Uiso 1 1 calc R . .
H12B H 1.2239 0.5168 1.1470 0.021 Uiso 1 1 calc R . .
C13 C 1.3900(4) 0.4096(4) 1.1268(2) 0.0140(8) Uani 1 1 d . . .
H13A H 1.4528 0.4679 1.1564 0.017 Uiso 1 1 calc R . .
H13B H 1.3627 0.3463 1.1710 0.017 Uiso 1 1 calc R . .
O3W O 1.1754(5) 0.9003(5) 1.3382(3) 0.0286(11) Uani 0.70 1 d P . .
H3WA H 1.2453 0.8542 1.3372 0.034 Uiso 0.70 1 d PR . .
H3WB H 1.1912 0.9811 1.3416 0.034 Uiso 0.70 1 d PR . .
O1W O 1.4251(3) 0.6262(3) 0.86571(18) 0.0231(7) Uani 1 1 d . . .
H1WA H 1.3450 0.6502 0.8573 0.028 Uiso 1 1 d R . .
H1WB H 1.4866 0.6619 0.8362 0.028 Uiso 1 1 d R . .
O2W O 1.3660(3) 0.1674(3) 1.34403(19) 0.0271(7) Uani 1 1 d . . .
H2WA H 1.4042 0.2065 1.3013 0.033 Uiso 1 1 d R . .
H2WB H 1.4088 0.1126 1.3762 0.033 Uiso 1 1 d R . .
O4W O 0.8687(4) 0.9262(4) 1.1772(2) 0.0419(10) Uani 1 1 d . . .
H4WA H 0.8919 0.9111 1.2319 0.050 Uiso 1 1 d R . .
H4WB H 0.8048 0.9779 1.1653 0.050 Uiso 1 1 d R . .
O16 O 1.3035(3) 0.5438(3) 1.69425(17) 0.0159(6) Uani 1 1 d . . .
B8 B 1.3909(4) 0.4843(4) 1.6370(3) 0.0121(8) Uani 1 1 d . . .
O13 O 1.4915(2) 0.4100(3) 1.67162(16) 0.0125(6) Uani 1 1 d . . .
O3WA O 1.1000(11) 0.8731(13) 1.2947(8) 0.036(3) Uani 0.30 1 d P . .
H3WC H 1.0571 0.9353 1.2702 0.043 Uiso 0.30 1 d PR . .
H3WD H 1.1187 0.8142 1.2569 0.043 Uiso 0.30 1 d PR . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Al1 0.0107(5) 0.0061(6) 0.0064(5) 0.0004(4) -0.0019(4) -0.0006(4)
Al2 0.0102(5) 0.0072(6) 0.0064(5) -0.0001(4) -0.0022(4) -0.0005(4)
O1 0.0158(12) 0.0199(17) 0.0069(12) -0.0018(11) 0.0004(9) 0.0039(12)
O2 0.0159(12) 0.0141(16) 0.0105(13) -0.0049(11) -0.0032(9) 0.0036(11)
O3 0.0209(13) 0.0101(15) 0.0084(13) -0.0003(10) 0.0030(10) 0.0070(11)
O4 0.0260(14) 0.0144(16) 0.0123(13) 0.0042(12) 0.0008(10) -0.0067(13)
O5 0.0177(12) 0.0129(15) 0.0089(12) -0.0007(11) -0.0023(9) 0.0030(11)
O6 0.0196(13) 0.0134(15) 0.0060(12) 0.0038(10) -0.0020(9) -0.0036(11)
O7 0.0182(13) 0.0153(17) 0.0116(13) 0.0014(11) 0.0013(10) 0.0043(11)
O8 0.0204(14) 0.0195(17) 0.0096(13) -0.0025(11) -0.0007(10) -0.0064(12)
O9 0.0271(15) 0.0171(17) 0.0091(13) 0.0016(11) 0.0033(10) -0.0082(12)
O10 0.0161(12) 0.0165(16) 0.0095(13) -0.0011(11) -0.0010(9) -0.0043(11)
O11 0.0179(12) 0.0099(15) 0.0085(12) 0.0048(10) 0.0002(9) -0.0051(11)
O12 0.0147(12) 0.0161(16) 0.0064(12) -0.0002(11) -0.0049(9) 0.0035(11)
O14 0.0193(13) 0.0199(17) 0.0147(14) -0.0035(12) -0.0029(10) -0.0043(12)
O15 0.0246(14) 0.0200(17) 0.0064(12) -0.0043(11) 0.0021(10) -0.0100(12)
O17 0.0147(12) 0.0177(16) 0.0096(12) 0.0022(11) -0.0038(9) -0.0060(11)
O18 0.0181(13) 0.0163(16) 0.0060(12) -0.0002(11) -0.0055(9) -0.0046(11)
O19 0.0192(13) 0.0252(18) 0.0114(13) -0.0012(12) -0.0003(10) 0.0119(13)
O20 0.0198(13) 0.0121(15) 0.0070(12) -0.0013(11) -0.0001(9) 0.0055(12)
B2 0.0136(19) 0.014(2) 0.0110(19) 0.0004(17) -0.0009(15) -0.0020(17)
B3 0.0117(18) 0.013(2) 0.0086(18) 0.0035(16) -0.0030(14) 0.0019(16)
B6 0.0148(19) 0.006(2) 0.0066(19) 0.0050(15) -0.0027(14) -0.0027(16)
B7 0.0132(18) 0.008(2) 0.013(2) -0.0018(16) 0.0020(14) -0.0019(16)
B9 0.0110(17) 0.005(2) 0.0096(19) 0.0012(15) -0.0009(14) 0.0001(15)
B10 0.0123(18) 0.011(2) 0.0096(19) -0.0001(16) -0.0038(14) 0.0023(16)
N1 0.0231(16) 0.0129(19) 0.0153(16) 0.0007(14) 0.0041(12) 0.0000(15)
N2 0.0203(16) 0.020(2) 0.0150(17) 0.0013(14) -0.0005(13) 0.0057(14)
N3 0.0241(17) 0.0069(19) 0.034(2) 0.0068(15) -0.0043(14) -0.0008(15)
C1 0.0232(19) 0.013(2) 0.0144(19) 0.0022(16) -0.0015(15) 0.0032(17)
C2 0.0215(19) 0.013(2) 0.023(2) 0.0042(17) 0.0008(16) 0.0013(16)
C5 0.024(2) 0.033(3) 0.022(2) 0.000(2) -0.0032(16) -0.0017(19)
C6 0.024(2) 0.021(3) 0.018(2) -0.0017(17) 0.0008(15) 0.0033(18)
N4 0.0173(16) 0.0175(19) 0.0103(16) 0.0040(13) -0.0001(12) -0.0033(14)
N5 0.0143(15) 0.013(2) 0.0152(16) 0.0031(13) 0.0000(12) -0.0024(13)
N6 0.0207(16) 0.015(2) 0.0125(16) 0.0022(13) 0.0016(12) 0.0017(14)
C8 0.0149(17) 0.015(2) 0.0141(19) -0.0018(15) -0.0031(13) -0.0001(15)
C10 0.0245(19) 0.013(2) 0.0112(18) 0.0002(16) -0.0040(14) 0.0073(17)
C12 0.0212(19) 0.014(2) 0.017(2) 0.0044(16) 0.0036(15) -0.0060(17)
C13 0.0209(18) 0.009(2) 0.0125(19) 0.0032(15) -0.0009(14) 0.0031(16)
O3W 0.034(2) 0.027(3) 0.025(2) 0.004(2) 0.001(2) -0.008(2)
O1W 0.0206(14) 0.030(2) 0.0182(14) -0.0034(13) -0.0006(11) -0.0051(13)
O2W 0.0297(15) 0.0267(19) 0.0244(15) -0.0093(14) -0.0110(12) 0.0062(14)
O4W 0.050(2) 0.031(2) 0.046(2) -0.0171(18) 0.0249(17) -0.0047(17)
O16 0.0208(13) 0.0166(16) 0.0103(13) 0.0036(11) 0.0016(10) 0.0066(12)
B8 0.0152(19) 0.010(2) 0.012(2) 0.0020(16) 0.0016(15) -0.0026(17)
O13 0.0168(12) 0.0096(15) 0.0110(13) 0.0042(11) -0.0002(9) 0.0040(11)
O3WA 0.041(7) 0.034(7) 0.033(6) 0.017(5) -0.001(5) 0.014(6)
_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
Al1 O4 1.728(3) . ?
Al1 O17 1.743(3) 2_847 ?
Al1 O13 1.744(3) 2_858 ?
Al1 O2 1.750(3) . ?
Al2 O14 1.720(3) 2_757 ?
Al2 O10 1.735(3) 1_565 ?
Al2 O7 1.737(3) . ?
Al2 O19 1.743(3) 2_758 ?
O1 B1 1.358(5) . ?
O1 B5 1.458(5) . ?
O2 B1 1.351(5) . ?
O3 B1 1.403(5) . ?
O3 B3 1.416(5) . ?
O4 B2 1.329(5) . ?
O5 B3 1.356(5) . ?
O5 B5 1.470(5) . ?
O6 B2 1.373(5) . ?
O6 B6 1.453(5) . ?
O7 B3 1.325(5) . ?
O8 B4 1.355(5) . ?
O8 B6 1.471(5) . ?
O9 B4 1.379(5) . ?
O9 B2 1.409(5) . ?
O10 B4 1.364(5) . ?
O10 Al2 1.735(3) 1_545 ?
O11 B7 1.355(5) . ?
O11 B5 1.480(5) . ?
O12 B10 1.356(5) . ?
O12 B6 1.476(5) . ?
O14 B7 1.341(5) . ?
O14 Al2 1.720(3) 2_747 ?
O15 B7 1.405(5) . ?
O15 B9 1.405(5) . ?
O17 B9 1.348(5) . ?
O17 Al1 1.743(3) 2_857 ?
O18 B9 1.363(5) . ?
O18 B5 1.461(5) . ?
O19 B10 1.323(5) . ?
O19 Al2 1.743(3) 2_748 ?
O20 B8 1.354(5) . ?
O20 B6 1.492(5) . ?
B10 O16 1.421(5) . ?
N1 C6 1.507(5) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N1 H1C 0.9000 . ?
N2 C1 1.487(5) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N3 C5 1.467(6) . ?
N3 C2 1.473(5) . ?
N3 H3A 0.9001 . ?
C1 C2 1.514(6) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C2 H2D 0.9700 . ?
C2 H2E 0.9700 . ?
C5 C6 1.535(6) . ?
C5 H5D 0.9700 . ?
C5 H5E 0.9700 . ?
C6 H6B 0.9700 . ?
C6 H6C 0.9700 . ?
N4 C13 1.489(5) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 H4C 0.8900 . ?
N5 C8 1.486(5) . ?
N5 H5A 0.9000 . ?
N5 H5B 0.8999 . ?
N5 H5C 0.9000 . ?
N6 C12 1.452(5) . ?
N6 C10 1.476(5) . ?
N6 H6A 0.8998 . ?
C8 C10 1.517(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C12 C13 1.498(5) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
O3W O3WA 1.022(12) . ?
O3W H3WA 0.8500 . ?
O3W H3WB 0.8500 . ?
O1W H1WA 0.8499 . ?
O1W H1WB 0.8500 . ?
O2W H2WA 0.8500 . ?
O2W H2WB 0.8500 . ?
O4W H4WA 0.8499 . ?
O4W H4WB 0.8501 . ?
O16 B8 1.381(5) . ?
B8 O13 1.361(5) . ?
O13 Al1 1.744(3) 2_848 ?
O3WA H3WC 0.8499 . ?
O3WA H3WD 0.8500 . ?
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 Al1 O17 111.07(17) . 2_847 ?
O4 Al1 O13 110.71(13) . 2_858 ?
O17 Al1 O13 107.59(13) 2_847 2_858 ?
O4 Al1 O2 108.05(14) . . ?
O17 Al1 O2 106.77(13) 2_847 . ?
O13 Al1 O2 112.60(15) 2_858 . ?
O14 Al2 O10 112.91(16) 2_757 1_565 ?
O14 Al2 O7 110.70(14) 2_757 . ?
O10 Al2 O7 107.17(14) 1_565 . ?
O14 Al2 O19 108.43(14) 2_757 2_758 ?
O10 Al2 O19 110.23(13) 1_565 2_758 ?
O7 Al2 O19 107.25(17) . 2_758 ?
B1 O1 B5 123.4(3) . . ?
B1 O2 Al1 136.1(3) . . ?
B1 O3 B3 120.8(3) . . ?
B2 O4 Al1 149.8(3) . . ?
B3 O5 B5 123.6(3) . . ?
B2 O6 B6 122.8(3) . . ?
B3 O7 Al2 147.6(3) . . ?
B4 O8 B6 121.8(3) . . ?
B4 O9 B2 120.6(3) . . ?
B4 O10 Al2 137.2(3) . 1_545 ?
B7 O11 B5 122.3(3) . . ?
B10 O12 B6 122.6(3) . . ?
B7 O14 Al2 151.7(3) . 2_747 ?
B7 O15 B9 120.4(3) . . ?
B9 O17 Al1 138.7(2) . 2_857 ?
B9 O18 B5 123.0(3) . . ?
B10 O19 Al2 146.7(3) . 2_748 ?
B8 O20 B6 123.0(3) . . ?
O2 B1 O1 120.8(3) . . ?
O2 B1 O3 120.3(3) . . ?
O1 B1 O3 118.7(3) . . ?
O4 B2 O6 124.3(4) . . ?
O4 B2 O9 117.7(3) . . ?
O6 B2 O9 117.9(3) . . ?
O7 B3 O5 125.4(4) . . ?
O7 B3 O3 116.3(3) . . ?
O5 B3 O3 118.3(3) . . ?
O8 B4 O10 117.1(3) . . ?
O8 B4 O9 121.1(4) . . ?
O10 B4 O9 121.8(3) . . ?
O1 B5 O18 110.3(3) . . ?
O1 B5 O5 111.1(3) . . ?
O18 B5 O5 108.1(3) . . ?
O1 B5 O11 108.7(3) . . ?
O18 B5 O11 110.8(3) . . ?
O5 B5 O11 107.7(3) . . ?
O6 B6 O8 112.1(3) . . ?
O6 B6 O12 109.5(3) . . ?
O8 B6 O12 108.3(3) . . ?
O6 B6 O20 108.2(3) . . ?
O8 B6 O20 108.4(3) . . ?
O12 B6 O20 110.3(3) . . ?
O14 B7 O11 119.4(3) . . ?
O14 B7 O15 121.5(3) . . ?
O11 B7 O15 119.0(3) . . ?
O17 B9 O18 122.3(3) . . ?
O17 B9 O15 118.3(3) . . ?
O18 B9 O15 119.5(3) . . ?
O19 B10 O12 125.9(3) . . ?
O19 B10 O16 115.5(3) . . ?
O12 B10 O16 118.6(3) . . ?
C6 N1 H1A 109.2 . . ?
C6 N1 H1B 109.3 . . ?
H1A N1 H1B 109.5 . . ?
C6 N1 H1C 109.9 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N2 H2A 109.5 . . ?
C1 N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
C1 N2 H2C 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C5 N3 C2 112.1(3) . . ?
C5 N3 H3A 108.8 . . ?
C2 N3 H3A 108.9 . . ?
N2 C1 C2 112.4(3) . . ?
N2 C1 H1D 109.1 . . ?
C2 C1 H1D 109.1 . . ?
N2 C1 H1E 109.1 . . ?
C2 C1 H1E 109.1 . . ?
H1D C1 H1E 107.9 . . ?
N3 C2 C1 109.9(3) . . ?
N3 C2 H2D 109.7 . . ?
C1 C2 H2D 109.7 . . ?
N3 C2 H2E 109.7 . . ?
C1 C2 H2E 109.7 . . ?
H2D C2 H2E 108.2 . . ?
N3 C5 C6 113.3(3) . . ?
N3 C5 H5D 108.9 . . ?
C6 C5 H5D 108.9 . . ?
N3 C5 H5E 108.9 . . ?
C6 C5 H5E 108.9 . . ?
H5D C5 H5E 107.7 . . ?
N1 C6 C5 108.1(3) . . ?
N1 C6 H6B 110.1 . . ?
C5 C6 H6B 110.1 . . ?
N1 C6 H6C 110.1 . . ?
C5 C6 H6C 110.1 . . ?
H6B C6 H6C 108.4 . . ?
C13 N4 H4A 109.5 . . ?
C13 N4 H4B 109.5 . . ?
H4A N4 H4B 109.5 . . ?
C13 N4 H4C 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?
C8 N5 H5A 109.9 . . ?
C8 N5 H5B 109.9 . . ?
H5A N5 H5B 109.5 . . ?
C8 N5 H5C 108.6 . . ?
H5A N5 H5C 109.5 . . ?
H5B N5 H5C 109.5 . . ?
C12 N6 C10 113.3(3) . . ?
C12 N6 H6A 108.4 . . ?
C10 N6 H6A 108.9 . . ?
N5 C8 C10 108.9(3) . . ?
N5 C8 H8A 109.9 . . ?
C10 C8 H8A 109.9 . . ?
N5 C8 H8B 109.9 . . ?
C10 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
N6 C10 C8 114.8(3) . . ?
N6 C10 H10A 108.6 . . ?
C8 C10 H10A 108.6 . . ?
N6 C10 H10B 108.6 . . ?
C8 C10 H10B 108.6 . . ?
H10A C10 H10B 107.5 . . ?
N6 C12 C13 112.4(3) . . ?
N6 C12 H12A 109.1 . . ?
C13 C12 H12A 109.1 . . ?
N6 C12 H12B 109.1 . . ?
C13 C12 H12B 109.1 . . ?
H12A C12 H12B 107.8 . . ?
N4 C13 C12 112.9(3) . . ?
N4 C13 H13A 109.0 . . ?
C12 C13 H13A 109.0 . . ?
N4 C13 H13B 109.0 . . ?
C12 C13 H13B 109.0 . . ?
H13A C13 H13B 107.8 . . ?
O3WA O3W H3WA 115.9 . . ?
O3WA O3W H3WB 116.3 . . ?
H3WA O3W H3WB 113.4 . . ?
H1WA O1W H1WB 120.0 . . ?
H2WA O2W H2WB 120.0 . . ?
H4WA O4W H4WB 120.0 . . ?
B8 O16 B10 121.1(3) . . ?
O20 B8 O13 120.1(3) . . ?
O20 B8 O16 119.9(3) . . ?
O13 B8 O16 120.0(3) . . ?
B8 O13 Al1 136.0(2) . 2_848 ?
O3W O3WA H3WC 114.9 . . ?
O3W O3WA H3WD 116.0 . . ?
H3WC O3WA H3WD 112.3 . . ?
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
N1 H1A O3W 0.90 1.89 2.723(5) 153.1 .
N1 H1B O12 0.90 2.04 2.930(4) 169.9 .
N1 H1C O8 0.90 2.00 2.857(4) 158.3 2_758
N1 H1C O10 0.90 2.31 3.030(4) 137.0 2_758
N2 H2A O2W 0.89 2.01 2.834(5) 153.3 1_455
N2 H2B O20 0.89 1.89 2.773(4) 170.4 1_455
N2 H2C O6 0.89 2.12 2.904(4) 146.6 2_748
N3 H3A O3W 0.90 2.45 3.211(6) 142.5 2_748
N4 H4A O1W 0.89 2.03 2.784(5) 141.2 2_847
N4 H4B O1 0.89 2.06 2.813(4) 141.5 2_847
N4 H4B O2 0.89 2.51 3.127(4) 126.8 2_847
N4 H4C O18 0.89 2.10 2.965(4) 162.3 1_545
N4 H4C O5 0.89 2.60 3.312(4) 138.1 1_545
N5 H5A O4W 0.90 1.87 2.762(5) 170.8 .
N5 H5B O5 0.90 1.95 2.838(4) 168.3 2_747
N5 H5C O11 0.90 1.89 2.785(4) 174.3 .
N5 H5C O14 0.90 2.65 3.249(4) 124.6 .
N6 H6A O1W 0.90 2.11 2.868(4) 141.0 .
O3W H3WA O4 0.85 2.56 3.343(6) 154.0 .
O3W H3WA O6 0.85 2.58 3.201(6) 130.7 .
O3W H3WB O2W 0.85 2.61 3.359(6) 148.3 1_565
_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.118