##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in          #
# Acta Crystallographica Section C. It conforms to the requirements of       #
# Notes for Authors for Acta Crystallographica Section C, and has been       #
# peer reviewed under the auspices of the IUCr Commission on Journals.       #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic.                                       #
#                                                                            #
# Software is freely available for graphical display of the structure(s)     #
# in this CIF. For information consult the CIF software page                 #
# http://www.iucr.org/resources/cif/software.                                #
#                                                                            #
# This file may be used for bona fide research purposes within the           #
# scientific community so long as proper attribution is given to the journal # 
# article from which it was obtained.                                        #
#                                                                            #
##############################################################################
data_I
_audit_creation_method     SHELXL-97
_chemical_name_systematic
;
[1,5,9-tris(2-aminoethoxy)-3,7,11-trihydroxy-
3,7,11-tribora-1,5,9-triborata-2,4,6,8,10,12-hexaoxa-13-
oxoniatricyclo[7.3.1.0^5,13^]tridecane]cobalt(II)
;
_chemical_name_common
;
[tris(2-aminoethoxy)trihydroxyhexaborato]cobalt(II)
;
_chemical_formula_moiety     'C6 H21 B6 Co N3 O13'
_chemical_formula_sum     'C6 H21 B6 Co N3 O13'
_chemical_formula_iupac     '[Co (C6 H21 B6 N3 O13)]'
_chemical_formula_weight     467.05
_chemical_melting_point     ?
_symmetry_cell_setting     cubic
_symmetry_space_group_name_H-M     'P a -3'
_symmetry_space_group_name_Hall     '-P 2ac 2ab 3'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x+1/2, -y, z+1/2'
    '-x, y+1/2, -z+1/2'
    'x+1/2, -y+1/2, -z'
    'z, x, y'
    'z+1/2, -x+1/2, -y'
    '-z+1/2, -x, y+1/2'
    '-z, x+1/2, -y+1/2'
    'y, z, x'
    '-y, z+1/2, -x+1/2'
    'y+1/2, -z+1/2, -x'
    '-y+1/2, -z, x+1/2'
    '-x, -y, -z'
    'x-1/2, y, -z-1/2'
    'x, -y-1/2, z-1/2'
    '-x-1/2, y-1/2, z'
    '-z, -x, -y'
    '-z-1/2, x-1/2, y'
    'z-1/2, x, -y-1/2'
    'z, -x-1/2, y-1/2'
    '-y, -z, -x'
    'y, -z-1/2, x-1/2'
    '-y-1/2, z-1/2, x'
    'y-1/2, z, -x-1/2'
_cell_length_a     15.2796(18)
_cell_length_b     15.2796(18)
_cell_length_c     15.2796(18)
_cell_angle_alpha     90.00
_cell_angle_beta     90.00
_cell_angle_gamma     90.00
_cell_volume     3567.3(7)
_cell_formula_units_Z     8
_cell_measurement_reflns_used     25748
_cell_measurement_theta_min     3.27
_cell_measurement_theta_max     24.99
_cell_measurement_temperature     293(2)
_exptl_crystal_description     block
_exptl_crystal_colour     'pale pink'
_exptl_crystal_size_max     0.34
_exptl_crystal_size_mid     0.32
_exptl_crystal_size_min     0.27
_exptl_crystal_density_diffrn     1.739
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     ?
_exptl_crystal_F_000     1912
_exptl_absorpt_coefficient_mu     1.035
_exptl_absorpt_correction_type     empirical
_exptl_absorpt_process_details     '(ABSCOR; Higashi, 1995)'
_exptl_absorpt_correction_T_min     0.710
_exptl_absorpt_correction_T_max     0.756
_exptl_special_details     ?
_diffrn_ambient_temperature     293(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Rigaku R-AXIS RAPID'
_diffrn_measurement_method     ω
_diffrn_detector_area_resol_mean     0
_diffrn_reflns_number     25748
_diffrn_reflns_av_R_equivalents     0.0218
_diffrn_reflns_av_sigmaI/netI     0.0072
_diffrn_reflns_theta_min     3.27
_diffrn_reflns_theta_max     24.99
_diffrn_reflns_theta_full     24.99
_diffrn_measured_fraction_theta_max     0.997
_diffrn_measured_fraction_theta_full     0.997
_diffrn_reflns_limit_h_min     -18
_diffrn_reflns_limit_h_max     17
_diffrn_reflns_limit_k_min     -18
_diffrn_reflns_limit_k_max     18
_diffrn_reflns_limit_l_min     -18
_diffrn_reflns_limit_l_max     18
_diffrn_standards_number     0
_diffrn_standards_interval_count     0
_diffrn_standards_interval_time     0
_diffrn_standards_decay_%     0
_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.
;
_reflns_number_total     1057
_reflns_number_gt     1025
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0237
_refine_ls_R_factor_gt     0.0229
_refine_ls_wR_factor_gt     0.0639
_refine_ls_wR_factor_ref     0.0645
_refine_ls_goodness_of_fit_ref     1.110
_refine_ls_restrained_S_all     1.110
_refine_ls_number_reflns     1057
_refine_ls_number_parameters     91
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     mixed
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
         'calc w=1/[σ²(Fo²)+(0.0363P)²+1.7020P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.000
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     0.643
_refine_diff_density_min     -0.202
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
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'
    'Co' 'Co' 0.3494 0.9721
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'RAPID-AUTO (Rigaku, 1998)'
_computing_cell_refinement     'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction     'CrystalStructure (Rigaku/MSC, 2004)'
_computing_structure_solution     'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics     'SHELXTL (Sheldrick, 2008)'
_computing_publication_material     'SHELXL97 (Sheldrick, 2008)'
loop_
    _atom_site_type_symbol
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_symmetry_multiplicity
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    Co Co1 0.131061(13) 0.131061(13) 0.131061(13) 0.02009(15) Uani d S 1 3 . .
    O O1 0.32642(7) 0.12440(6) 0.30563(7) 0.0201(2) Uani d . 1 1 . .
    O O2 0.26659(7) 0.11257(7) 0.15998(7) 0.0213(2) Uani d . 1 1 . .
    O O3 0.38769(6) 0.21073(7) 0.19145(7) 0.0217(3) Uani d . 1 1 . .
    O O4 0.31865(8) 0.10226(8) 0.45622(7) 0.0269(3) Uani d . 1 1 . .
    O O5 0.24263(6) 0.24263(6) 0.24263(6) 0.0153(3) Uani d S 1 3 . .
    B B1 0.30894(10) 0.17090(10) 0.22458(10) 0.0172(3) Uani d . 1 1 . .
    B B2 0.28342(12) 0.14069(10) 0.38326(11) 0.0191(3) Uani d . 1 1 . .
    N N1 0.17831(10) 0.09872(10) 0.00375(9) 0.0318(3) Uani d . 1 1 . .
    C C1 0.31151(11) 0.07367(11) 0.08804(10) 0.0290(4) Uani d . 1 1 . .
    C C2 0.27420(12) 0.10950(13) 0.00365(11) 0.0342(4) Uani d . 1 1 . .
    H H1C 0.3044 0.0106 0.0897 0.035 Uiso calc R 1 1 . .
    H H1D 0.3735 0.0869 0.0916 0.035 Uiso calc R 1 1 . .
    H H2A 0.2889 0.1710 -0.0019 0.041 Uiso calc R 1 1 . .
    H H2B 0.2993 0.0785 -0.0458 0.041 Uiso calc R 1 1 . .
    H H4 0.3038(15) 0.1223(14) 0.4991(15) 0.041 Uiso d . 1 1 . .
    H H1A 0.1642 0.0431 -0.0095 0.038 Uiso calc R 1 1 . .
    H H1B 0.1539 0.1342 -0.0365 0.038 Uiso calc R 1 1 . .
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    Co1 0.02009(15) 0.02009(15) 0.02009(15) -0.00191(7) -0.00191(7) -0.00191(7)
    O1 0.0227(5) 0.0206(5) 0.0169(5) 0.0053(4) -0.0001(4) 0.0018(4)
    O2 0.0222(5) 0.0241(5) 0.0177(5) 0.0025(4) 0.0008(4) -0.0053(4)
    O3 0.0161(5) 0.0232(5) 0.0258(6) 0.0024(4) 0.0022(4) 0.0040(4)
    O4 0.0341(6) 0.0315(6) 0.0151(5) 0.0096(5) -0.0006(5) 0.0022(5)
    O5 0.0153(3) 0.0153(3) 0.0153(3) 0.0012(4) 0.0012(4) 0.0012(4)
    B1 0.0165(8) 0.0174(8) 0.0176(8) 0.0029(6) -0.0001(6) 0.0005(6)
    B2 0.0226(8) 0.0169(8) 0.0177(8) -0.0019(6) -0.0008(7) -0.0004(6)
    N1 0.0392(8) 0.0343(8) 0.0220(7) 0.0054(6) -0.0066(6) -0.0048(6)
    C1 0.0302(8) 0.0319(9) 0.0250(8) 0.0087(7) 0.0017(7) -0.0099(7)
    C2 0.0409(10) 0.0406(10) 0.0211(8) 0.0025(8) 0.0071(7) -0.0034(7)
_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_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Co1 N1 . 2.1330(14) no
    Co1 O2 . 2.1363(11) no
    O1 B1 . 1.4525(18) yes
    O1 B2 . 1.379(2) yes
    O2 B1 . 1.4790(19) yes
    O3 B1 . 1.4403(18) yes
    O3 B2 5 1.356(2) yes
    O4 B2 . 1.370(2) yes
    O5 B1 . 1.5179(15) yes
    O2 C1 . 1.4256(18) ?
    O4 H4 . 0.76(2) ?
    N1 C2 . 1.474(2) ?
    N1 H1A . 0.9000 ?
    N1 H1B . 0.9000 ?
    C1 C2 . 1.512(2) ?
    C1 H1C . 0.9700 ?
    C1 H1D . 0.9700 ?
    C2 H2A . 0.9700 ?
    C2 H2B . 0.9700 ?
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    N1 Co1 N1 5 . 100.13(5) ?
    N1 Co1 O2 . . 80.20(5) yes
    N1 Co1 O2 9 . 91.95(5) yes
    N1 Co1 O2 9 5 167.63(5) yes
    O2 Co1 O2 9 . 87.43(4) yes
    B1 O5 B1 5 . 118.17(4) ?
    B2 O1 B1 . . 123.89(12) ?
    B2 O3 B1 5 . 120.35(12) ?
    C1 O2 B1 . . 123.72(11) ?
    C1 O2 Co1 . . 111.24(9) ?
    B1 O2 Co1 . . 118.85(8) ?
    B2 O4 H4 . . 114.3(17) ?
    O1 B1 O2 . . 110.78(12) yes
    O1 B1 O5 . . 108.72(11) yes
    O2 B1 O5 . . 105.33(12) yes
    O3 B1 O1 . . 110.66(12) yes
    O3 B1 O2 . . 112.68(12) yes
    O3 B1 O5 . . 108.44(11) yes
    O3 B2 O1 9 . 122.45(14) yes
    O3 B2 O4 9 . 121.74(14) yes
    O4 B2 O1 . . 115.81(14) yes
    C2 N1 Co1 . . 108.15(10) no
    C2 N1 H1A . . 110.1 ?
    Co1 N1 H1A . . 110.1 ?
    C2 N1 H1B . . 110.1 ?
    Co1 N1 H1B . . 110.1 ?
    H6 N1 H1B . . 108.4 ?
    O2 C1 C2 . . 108.97(13) ?
    O2 C1 H1C . . 109.9 ?
    C2 C1 H1C . . 109.9 ?
    O2 C1 H1D . . 109.9 ?
    C2 C1 H1D . . 109.9 ?
    H1 C1 H1D . . 108.3 ?
    N1 C2 C1 . . 109.46(14) ?
    N1 C2 H2A . . 109.8 ?
    C1 C2 H2A . . 109.8 ?
    N1 C2 H2B . . 109.8 ?
    C1 C2 H2B . . 109.8 ?
    H3 C2 H2B . . 108.2 ?
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    O4 H4 O1 20_566 0.76(2) 2.07(2) 2.7982(15) 162(2)
    N1 H1B O1 22_565 0.90 2.33 3.1869(17) 158.6
    N1 H1A O4 2_554 0.90 2.30 3.1559(19) 159.6
_iucr_refine_instructions_details
;
TITL I minco in Pa-3
CELL 0.71073  15.2796  15.2796  15.2796  90.000  90.000  90.000
ZERR   8.00   0.0018   0.0018   0.0018   0.000   0.000   0.000
LATT  1
SYMM 0.5-X, -Y, 0.5+Z
SYMM -X, 0.5+Y, 0.5-Z
SYMM 0.5+X, 0.5-Y, -Z
SYMM Z, X, Y
SYMM 0.5+Z, 0.5-X, -Y
SYMM 0.5-Z, -X, 0.5+Y
SYMM -Z, 0.5+X, 0.5-Y
SYMM Y, Z, X
SYMM -Y, 0.5+Z, 0.5-X
SYMM 0.5+Y, 0.5-Z, -X
SYMM 0.5-Y, -Z, 0.5+X
SFAC C H B N O CO
UNIT 48 168 48 24 104 8
L.S. 4
ACTA
BOND $H
HTAB
EQIV $1  z, -x+1/2, y+1/2
EQIV $2  y, -z+1/2, x-1/2
EQIV $3  -x+1/2, -y, z-1/2
HTAB O4  O1_$1
HTAB N1  O1_$2
HTAB N1  O4_$3
FMAP 2
PLAN 10
WGHT    0.036300    1.702000
FVAR       0.32830
CO1   6    0.131061    0.131061    0.131061    10.33333    0.02009    0.02009 =
         0.02009   -0.00191   -0.00191   -0.00191
O1    5    0.326421    0.124396    0.305631    11.00000    0.02273    0.02059 =
         0.01690    0.00183   -0.00008    0.00525
O2    5    0.266592    0.112566    0.159978    11.00000    0.02217    0.02412 =
         0.01768   -0.00535    0.00085    0.00253
O3    5    0.387691    0.210730    0.191449    11.00000    0.01606    0.02315 =
         0.02580    0.00396    0.00220    0.00236
O4    5    0.318655    0.102260    0.456220    11.00000    0.03409    0.03153 =
         0.01514    0.00225   -0.00057    0.00957
AFIX  147
H4    2    0.303804    0.122327    0.499064    11.00000   -1.20000
AFIX  0
O5    5    0.242631    0.242631    0.242631    10.33333    0.01532    0.01532 =
         0.01532    0.00123    0.00123    0.00123
B2    3    0.283417    0.140688    0.383256    11.00000    0.02263    0.01691 =
         0.01765   -0.00043   -0.00081   -0.00193
B1    3    0.308942    0.170896    0.224580    11.00000    0.01655    0.01739 =
         0.01759    0.00046   -0.00009    0.00292
N1    4    0.178312    0.098716    0.003749    11.00000    0.03919    0.03431 =
         0.02200   -0.00476   -0.00658    0.00537
AFIX  23
H1A    2    0.164213    0.043086   -0.009515    11.00000   -1.20000
H1B    2    0.153939    0.134180   -0.036472    11.00000   -1.20000
AFIX   0
C1    1    0.311506    0.073674    0.088041    11.00000    0.03023    0.03186 =
         0.02501   -0.00992    0.00170    0.00872
AFIX  23
H1C    2    0.304449    0.010607    0.089720    11.00000   -1.20000
H1D    2    0.373496    0.086899    0.091583    11.00000   -1.20000
AFIX   0
C2    1    0.274198    0.109501    0.003647    11.00000    0.04088    0.04057 =
         0.02111   -0.00340    0.00706    0.00254
AFIX  23
H2A    2    0.288895    0.171006   -0.001939    11.00000   -1.20000
H2B    2    0.299250    0.078520   -0.045778    11.00000   -1.20000
AFIX   0
HKLF 4
;
data_II
_audit_creation_method     SHELXL-97
_chemical_name_systematic
;
[1,5,9-tris(2-aminoethoxy)-3,7,11-trihydroxy-
3,7,11-tribora-1,5,9-triborata-2,4,6,8,10,12-hexaoxa-13-
oxoniatricyclo[7.3.1.0^5,13^]tridecane]nickel(II)
;
_chemical_name_common
;
[tris(2-aminoethoxy)trihydroxyhexaborato]nickel(II)
;
_chemical_formula_moiety     'C6 H21 B6 Ni N3 O13'
_chemical_formula_sum     'C6 H21 B6 N3 Ni O13'
_chemical_formula_iupac     '[Ni (C6 H21 B6 N3 O13)]'
_chemical_formula_weight     466.83
_chemical_melting_point     ?
_symmetry_cell_setting     cubic
_symmetry_space_group_name_H-M     'P a -3'
_symmetry_space_group_name_Hall     '-P 2ac 2ab 3'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x+1/2, -y, z+1/2'
    '-x, y+1/2, -z+1/2'
    'x+1/2, -y+1/2, -z'
    'z, x, y'
    'z+1/2, -x+1/2, -y'
    '-z+1/2, -x, y+1/2'
    '-z, x+1/2, -y+1/2'
    'y, z, x'
    '-y, z+1/2, -x+1/2'
    'y+1/2, -z+1/2, -x'
    '-y+1/2, -z, x+1/2'
    '-x, -y, -z'
    'x-1/2, y, -z-1/2'
    'x, -y-1/2, z-1/2'
    '-x-1/2, y-1/2, z'
    '-z, -x, -y'
    '-z-1/2, x-1/2, y'
    'z-1/2, x, -y-1/2'
    'z, -x-1/2, y-1/2'
    '-y, -z, -x'
    'y, -z-1/2, x-1/2'
    '-y-1/2, z-1/2, x'
    'y-1/2, z, -x-1/2'
_cell_length_a     15.2217(18)
_cell_length_b     15.2217(18)
_cell_length_c     15.2217(18)
_cell_angle_alpha     90.00
_cell_angle_beta     90.00
_cell_angle_gamma     90.00
_cell_volume     3526.9(7)
_cell_formula_units_Z     8
_cell_measurement_reflns_used     25821
_cell_measurement_theta_min     2.99
_cell_measurement_theta_max     25.01
_cell_measurement_temperature     293(2)
_exptl_crystal_description     block
_exptl_crystal_colour     blue
_exptl_crystal_size_max     0.14
_exptl_crystal_size_mid     0.14
_exptl_crystal_size_min     0.14
_exptl_crystal_density_diffrn     1.758
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     ?
_exptl_crystal_F_000     1920
_exptl_absorpt_coefficient_mu     1.173
_exptl_absorpt_correction_type     empirical
_exptl_absorpt_process_details     '(ABSCOR; Higashi, 1995)'
_exptl_absorpt_correction_T_min     0.849
_exptl_absorpt_correction_T_max     0.849
_exptl_special_details     ?
_diffrn_ambient_temperature     293(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Rigaku R-AXIS RAPID'
_diffrn_measurement_method     ω
_diffrn_detector_area_resol_mean     0
_diffrn_reflns_number     25821
_diffrn_reflns_av_R_equivalents     0.0754
_diffrn_reflns_av_sigmaI/netI     0.0206
_diffrn_reflns_theta_min     2.99
_diffrn_reflns_theta_max     25.01
_diffrn_reflns_theta_full     25.01
_diffrn_measured_fraction_theta_max     0.998
_diffrn_measured_fraction_theta_full     0.998
_diffrn_reflns_limit_h_min     -18
_diffrn_reflns_limit_h_max     18
_diffrn_reflns_limit_k_min     -18
_diffrn_reflns_limit_k_max     18
_diffrn_reflns_limit_l_min     -18
_diffrn_reflns_limit_l_max     17
_diffrn_standards_number     0
_diffrn_standards_interval_count     0
_diffrn_standards_interval_time     0
_diffrn_standards_decay_%     0
_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.
;
_reflns_number_total     1042
_reflns_number_gt     885
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0536
_refine_ls_R_factor_gt     0.0438
_refine_ls_wR_factor_gt     0.0921
_refine_ls_wR_factor_ref     0.1070
_refine_ls_goodness_of_fit_ref     1.143
_refine_ls_restrained_S_all     1.143
_refine_ls_number_reflns     1042
_refine_ls_number_parameters     91
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     mixed
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
         'calc w=1/[σ²(Fo²)+(0.0353P)²+9.9478P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.000
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     0.375
_refine_diff_density_min     -0.503
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
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'
    'Ni' 'Ni' 0.3393 1.1124
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'RAPID-AUTO (Rigaku, 1998)'
_computing_cell_refinement     'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction     'CrystalStructure (Rigaku/MSC, 2004)'
_computing_structure_solution     'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics     'SHELXTL (Sheldrick, 2008)'
_computing_publication_material     'SHELXL97 (Sheldrick, 2008)'
loop_
    _atom_site_type_symbol
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_symmetry_multiplicity
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    Ni Ni1 0.13077(3) 0.13077(3) 0.13077(3) 0.0231(3) Uani d S 1 3 . .
    O O1 0.32601(16) 0.12309(15) 0.30443(15) 0.0239(6) Uani d . 1 1 . .
    O O2 0.26448(16) 0.11086(16) 0.15913(15) 0.0238(6) Uani d . 1 1 . .
    O O3 0.38667(15) 0.20905(16) 0.18920(16) 0.0245(6) Uani d . 1 1 . .
    O O4 0.31826(18) 0.10076(18) 0.45563(17) 0.0303(6) Uani d . 1 1 . .
    O O5 0.24183(14) 0.24183(14) 0.24183(14) 0.0182(9) Uani d S 1 3 . .
    B B1 0.3080(3) 0.1696(3) 0.2231(3) 0.0216(9) Uani d . 1 1 . .
    B B2 0.2828(3) 0.1388(3) 0.3823(3) 0.0218(8) Uani d . 1 1 . .
    N N1 0.1734(2) 0.1002(2) 0.0045(2) 0.0341(8) Uani d . 1 1 . .
    C C1 0.3090(3) 0.0726(3) 0.0856(2) 0.0313(9) Uani d . 1 1 . .
    C C2 0.2702(3) 0.1099(3) 0.0021(3) 0.0359(10) Uani d . 1 1 . .
    H H1C 0.3019 0.0093 0.0865 0.038 Uiso calc R 1 1 . .
    H H1D 0.3712 0.0859 0.0885 0.038 Uiso calc R 1 1 . .
    H H2A 0.2856 0.1715 -0.0033 0.043 Uiso calc R 1 1 . .
    H H2B 0.2937 0.0790 -0.0484 0.043 Uiso calc R 1 1 . .
    H H4 0.302(3) 0.119(3) 0.502(3) 0.043 Uiso d . 1 1 . .
    H H1A 0.1582 0.0448 -0.0091 0.041 Uiso calc R 1 1 . .
    H H1B 0.1484 0.1367 -0.0347 0.041 Uiso calc R 1 1 . .
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    Ni1 0.0231(3) 0.0231(3) 0.0231(3) -0.00170(18) -0.00170(18) -0.00170(18)
    O1 0.0275(13) 0.0247(13) 0.0194(12) 0.0053(10) -0.0015(10) 0.0034(10)
    O2 0.0256(13) 0.0267(13) 0.0189(12) 0.0017(10) -0.0004(10) -0.0048(10)
    O3 0.0188(12) 0.0249(13) 0.0298(14) 0.0004(10) 0.0039(10) 0.0046(11)
    O4 0.0355(15) 0.0372(15) 0.0181(13) 0.0094(12) -0.0013(12) 0.0031(12)
    O5 0.0182(9) 0.0182(9) 0.0182(9) 0.0011(10) 0.0011(10) 0.0011(10)
    B1 0.0188(19) 0.022(2) 0.024(2) 0.0030(16) -0.0022(16) -0.0028(16)
    B2 0.0214(19) 0.025(2) 0.019(2) -0.0014(16) 0.0009(16) -0.0032(16)
    N1 0.040(2) 0.0354(19) 0.0267(17) 0.0030(15) -0.0058(15) 0.0002(14)
    C1 0.030(2) 0.036(2) 0.028(2) 0.0088(17) 0.0017(16) -0.0098(17)
    C2 0.037(2) 0.040(2) 0.030(2) -0.0005(19) 0.0052(18) -0.0021(18)
_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_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Ni1 N1 . 2.081(3) ?
    Ni1 O2 . 2.102(2) ?
    O1 B1 . 1.453(4) yes
    O1 B2 . 1.377(5) yes
    O2 B1 . 1.479(4) yes
    O3 B1 . 1.435(5) yes
    O3 B2 5 1.361(5) yes
    O4 B2 . 1.369(5) yes
    O5 B1 . 1.518(4) yes
    O2 C1 . 1.432(4) ?
    O4 H4 . 0.79(5) ?
    N1 C2 . 1.481(5) ?
    N1 H1A . 0.9000 ?
    N1 H1B . 0.9000 ?
    C1 C2 . 1.513(6) ?
    C1 H1C . 0.9700 ?
    C1 H1D . 0.9700 ?
    C2 H2A . 0.9700 ?
    C2 H2B . 0.9700 ?
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    N1 Ni1 N1 . 5 98.72(12) ?
    N1 Ni1 O2 9 . 91.09(11) yes
    N1 Ni1 O2 5 5 81.68(11) yes
    N1 Ni1 O2 9 5 169.98(12) yes
    O2 Ni1 O2 9 . 88.30(9) yes
    B1 O1 B2 . . 124.0(3) ?
    B1 O5 B1 5 . 117.98(10) ?
    B2 O3 B1 5 . 120.4(3) ?
    C1 O2 B1 . . 123.3(3) ?
    C1 O2 Ni1 . . 110.9(2) ?
    B1 O2 Ni1 . . 118.8(2) ?
    B2 O4 H4 . . 117(3) ?
    O1 B1 O2 . . 110.5(3) yes
    O1 B1 O5 . . 108.5(3) yes
    O2 B1 O5 . . 105.3(3) yes
    O3 B1 O1 . . 110.7(3) yes
    O3 B1 O2 . . 113.0(3) yes
    O3 B1 O5 . . 108.6(3) yes
    O3 B2 O1 9 . 122.3(3) yes
    O3 B2 O4 9 . 121.6(3) yes
    O4 B2 O1 . . 116.1(3) yes
    C2 N1 Ni1 . . 108.2(2) ?
    C2 N1 H1A . . 110.1 ?
    Ni1 N1 H1A . . 110.1 ?
    C2 N1 H1B . . 110.1 ?
    Ni1 N1 H1B . . 110.1 ?
    H6 N1 H1B . . 108.4 ?
    O2 C1 C2 . . 108.7(3) ?
    O2 C1 H1C . . 110.0 ?
    C2 C1 H1C . . 110.0 ?
    O2 C1 H1D . . 110.0 ?
    C2 C1 H1D . . 110.0 ?
    H1 C1 H2D . . 108.3 ?
    N1 C2 C1 . . 109.2(3) ?
    N1 C2 H2A . . 109.8 ?
    C1 C2 H2A . . 109.8 ?
    N1 C2 H2B . . 109.8 ?
    C1 C2 H2B . . 109.8 ?
    H3 C2 H2B . . 108.3 ?
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    O4 H4 O1 20_566 0.79(5) 2.03(5) 2.790(3) 161(5)
    N1 H1B O1 22_565 0.90 2.33 3.175(4) 155.5
    N1 H1A O4 2_554 0.90 2.31 3.151(4) 156.2
_iucr_refine_instructions_details
;
TITL II in Pa-3
CELL 0.71073  15.2217  15.2217  15.2217  90.000  90.000  90.000
ZERR   8.00   0.0018   0.0018   0.0018   0.000   0.000   0.000
LATT  1
SYMM 0.5-X, -Y, 0.5+Z
SYMM -X, 0.5+Y, 0.5-Z
SYMM 0.5+X, 0.5-Y, -Z
SYMM Z, X, Y
SYMM 0.5+Z, 0.5-X, -Y
SYMM 0.5-Z, -X, 0.5+Y
SYMM -Z, 0.5+X, 0.5-Y
SYMM Y, Z, X
SYMM -Y, 0.5+Z, 0.5-X
SYMM 0.5+Y, 0.5-Z, -X
SYMM 0.5-Y, -Z, 0.5+X
SFAC C H B N O NI
UNIT 48 168 48 24 104 8
L.S. 4
ACTA
BOND $H
HTAB
EQIV $1  z, -x+1/2, y+1/2
EQIV $2  y, -z+1/2, x-1/2
EQIV $3  -x+1/2, -y, z-1/2
HTAB O4  O1_$1
HTAB N1  O1_$2
HTAB N1  O4_$3
FMAP 2
PLAN 10
WGHT    0.035300    9.947800
FVAR       0.33880
NI1   6    0.130769    0.130769    0.130769    10.33333    0.02307    0.02307 =
         0.02307   -0.00170   -0.00170   -0.00170
O1    5    0.326009    0.123090    0.304433    11.00000    0.02751    0.02473 =
         0.01943    0.00343   -0.00148    0.00535
O2    5    0.264475    0.110863    0.159132    11.00000    0.02558    0.02675 =
         0.01894   -0.00484   -0.00037    0.00170
O3    5    0.386666    0.209053    0.189203    11.00000    0.01879    0.02486 =
         0.02985    0.00461    0.00389    0.00035
O4    5    0.318264    0.100765    0.455633    11.00000    0.03551    0.03724 =
         0.01807    0.00310   -0.00125    0.00936
AFIX  147
H4    2    0.302405    0.119039    0.501628    11.00000   -1.20000
AFIX  0
O5    5    0.241829    0.241829    0.241829    10.33333    0.01822    0.01822 =
         0.01822    0.00105    0.00105    0.00105
B2    3    0.282776    0.138829    0.382313    11.00000    0.02139    0.02478 =
         0.01933   -0.00316    0.00090   -0.00135
B1    3    0.308005    0.169637    0.223081    11.00000    0.01882    0.02248 =
         0.02357   -0.00278   -0.00215    0.00303
N1    4    0.173423    0.100239    0.004545    11.00000    0.04011    0.03535 =
         0.02669    0.00022   -0.00576    0.00302
AFIX  23
H1A    2    0.158236    0.044758   -0.009137    11.00000   -1.20000
H1B    2    0.148366    0.136674   -0.034704    11.00000   -1.20000
AFIX   0
C1    1    0.308965    0.072607    0.085614    11.00000    0.03029    0.03590 =
         0.02772   -0.00975    0.00165    0.00876
AFIX  23
H1C    2    0.301917    0.009279    0.086470    11.00000   -1.20000
H1D    2    0.371220    0.085899    0.088538    11.00000   -1.20000
AFIX   0
C2    1    0.270188    0.109936    0.002052    11.00000    0.03728    0.04032 =
         0.03010   -0.00208    0.00522   -0.00046
AFIX  23
H2A    2    0.285616    0.171532   -0.003313    11.00000   -1.20000
H2B    2    0.293730    0.078975   -0.048426    11.00000   -1.20000
AFIX   0
HKLF 4
;
data_global
_journal_date_recd_electronic     2011-08-26
_journal_date_accepted     2011-10-05
_journal_name_full     'Acta Crystallographica, Section C'
_journal_year     2011
_journal_volume     67
_journal_issue     11
_journal_page_first     m338
_journal_page_last     m341
_journal_paper_category     FM
_journal_coeditor_code     BM3109
_publ_contact_author_name     'Professor Yun-Xiao Liang'
_publ_contact_author_address
;
State Key Laboratory Base of Novel Functional Materials and Preparation Science
Faculty of Materials Science and Chemical Engineering,
Ningbo University
Ningbo 315211
People's Republic of China
;
_publ_contact_author_email     liangyunxiao@nbu.edu.cn
_publ_contact_author_fax     '086 574 87600734'
_publ_contact_author_phone     '086 574 87600874'
_publ_section_title
;
Two new transition metal inorganic--organic hybrid borates:
[tris(2-aminoethoxy)trihydroxyhexaborato]cobalt(II) and its nickel(II)
analogue
;
loop_
    _publ_author_name
    _publ_author_address
    'Shao-Min Lan'
;
State Key Laboratory Base of Novel Functional Materials and Preparation Science
Faculty of Materials Science and Chemical Engineering
Ningbo University
Ningbo, Zhejiang 315211, People's Republic of China
;
    'Wen-Jing Di'
;
State Key Laboratory Base of Novel Functional Materials and Preparation Science
Faculty of Materials Science and Chemical Engineering
Ningbo University
Ningbo, Zhejiang 315211, People's Republic of China
;
    'Zhi-Dong Shao'
;
State Key Laboratory Base of Novel Functional Materials and Preparation Science
Faculty of Materials Science and Chemical Engineering
Ningbo University
Ningbo, Zhejiang 315211, People's Republic of China
;
    'Yun-Xiao Liang'
;
State Key Laboratory Base of Novel Functional Materials and Preparation Science
Faculty of Materials Science and Chemical Engineering
Ningbo University
Ningbo, Zhejiang 315211, People's Republic of China
;
