# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_exp_1968
#TrackingRef 'web_deposit_cif_file_0_Bernhardt_1343128735.exp_1968.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C4 B N4), H12 Mg O6'
_chemical_formula_sum            'C8 H12 B2 Mg N8 O6'
_chemical_formula_weight         362.19

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'
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.0078(8)
_cell_length_b                   9.7507(7)
_cell_length_c                   11.5888(12)
_cell_angle_alpha                82.034(7)
_cell_angle_beta                 68.642(9)
_cell_angle_gamma                72.303(7)
_cell_volume                     902.67(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    2699
_cell_measurement_theta_min      3.6265
_cell_measurement_theta_max      29.1782

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.8299
_exptl_crystal_size_mid          0.4167
_exptl_crystal_size_min          0.2061
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_crystal_face_indexfrac_h
_exptl_crystal_face_indexfrac_k
_exptl_crystal_face_indexfrac_l
_exptl_crystal_face_x
_exptl_crystal_face_y
_exptl_crystal_face_z
2 4 -14 0.0852 1.9712 3.9888 -14.0107 -0.5868 0.8520 0.0088
-2 -3 14 0.1169 -1.9718 -2.9908 14.0102 0.5613 -0.8432 -0.0803
-2 -5 13 0.1247 -1.9722 -4.9873 13.0107 0.5879 -0.8014 0.0765
-3 11 2 0.3934 -2.9992 10.9706 1.9956 -0.0171 0.0018 -0.9651
3 -11 -3 0.4544 2.9976 -10.9712 -2.9962 -0.0073 0.0576 0.9789
7 2 16 0.0836 7.0151 2.0249 16.0067 -0.1620 -0.9893 -0.0114
7 -1 15 0.1077 7.0154 -0.9696 15.0078 -0.1098 -0.9563 0.2168
-6 -4 -16 0.1711 -6.0153 -4.0181 -16.0058 0.1414 0.9637 0.2047
-7 8 -8 0.3197 -7.0081 7.9596 -8.0077 0.1019 0.6017 -0.8140
-10 -9 2 0.1452 -9.9763 -9.0078 2.0082 0.9945 -0.1191 0.1112
10 0 -3 0.2468 9.9803 0.0256 -3.0038 -0.7892 0.0992 0.5458
-9 -11 2 0.1907 -8.9765 -11.0010 2.0092 0.9739 -0.1447 0.3045
-8 6 3 0.3241 -7.9871 5.9677 3.0000 0.4929 -0.0621 -0.8737
10 9 -2 0.1862 9.9763 9.0078 -2.0082 -0.9945 0.1191 -0.1112
11 -2 6 0.2373 10.9951 -1.9621 6.0024 -0.5902 -0.4616 0.6146
1 -7 12 0.1806 1.0230 -6.9756 12.0107 0.3997 -0.7833 0.3846
-3 7 10 0.3121 -2.9834 6.9836 10.0025 0.2801 -0.5092 -0.7900
-11 -10 -6 0.1857 -10.9875 -10.0134 -5.9956 0.8965 0.3557 0.2429
0 1 -15 0.0988 -0.0257 0.9888 -15.0092 -0.3914 0.9009 0.1362
-8 -8 6 0.1182 -7.9732 -8.0019 6.0096 0.9233 -0.3640 0.0852
-6 -12 4 0.2400 -5.9769 -11.9895 4.0103 0.8334 -0.2962 0.4996
-11 -9 -10 0.1869 -10.9948 -9.0179 -9.9985 0.7734 0.6024 0.2269
-8 8 -2 0.3332 -7.9967 7.9605 -2.0040 0.3199 0.2528 -0.9475
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             372
_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_T_min  0.938
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.2705
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7336
_diffrn_reflns_av_R_equivalents  0.0172
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.63
_diffrn_reflns_theta_max         29.24
_reflns_number_total             4137
_reflns_number_gt                3508
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro171.34.49, Oxford Diffraction'
_computing_cell_refinement       'CrysAlisPro171.34.49, Oxford Diffraction'
_computing_data_reduction        'CrysAlisPro171.34.49, Oxford Diffraction'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond, v.2.1e (Brandenburg, 2001)'
_computing_publication_material  ?

_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)+(0.0295P)²+0.2009P] where P=(Fo²+2Fc²)/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         4137
_refine_ls_number_parameters     274
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0308
_refine_ls_wR_factor_ref         0.0759
_refine_ls_wR_factor_gt          0.0716
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mg Mg 0.21892(4) 0.35521(4) 0.17427(3) 0.01518(10) Uani 1 1 d . . .
O1 O 0.00005(11) 0.42124(10) 0.13689(8) 0.02130(19) Uani 1 1 d . . .
H11 H -0.047(2) 0.505(2) 0.1273(16) 0.049(5) Uiso 1 1 d . . .
H12 H -0.060(2) 0.3701(19) 0.1384(16) 0.043(5) Uiso 1 1 d . . .
O2 O 0.43284(11) 0.28204(10) 0.21389(9) 0.0224(2) Uani 1 1 d . . .
H21 H 0.468(2) 0.196(2) 0.2354(17) 0.054(5) Uiso 1 1 d . . .
H22 H 0.492(2) 0.3282(19) 0.2091(16) 0.044(5) Uiso 1 1 d . . .
O3 O 0.29941(11) 0.52075(10) 0.05922(9) 0.02238(19) Uani 1 1 d . . .
H31 H 0.335(2) 0.5180(19) -0.0163(19) 0.047(5) Uiso 1 1 d . . .
H32 H 0.300(2) 0.598(2) 0.0791(18) 0.057(6) Uiso 1 1 d . . .
O4 O 0.12332(12) 0.20160(10) 0.29215(8) 0.0230(2) Uani 1 1 d . . .
H41 H 0.157(2) 0.159(2) 0.3468(18) 0.050(5) Uiso 1 1 d . . .
H42 H 0.022(2) 0.2289(19) 0.3249(16) 0.047(5) Uiso 1 1 d . . .
O5 O 0.32689(12) 0.22755(9) 0.02342(8) 0.02098(19) Uani 1 1 d . . .
H51 H 0.425(2) 0.2001(18) -0.0106(16) 0.044(5) Uiso 1 1 d . . .
H52 H 0.280(2) 0.2305(19) -0.0273(17) 0.051(5) Uiso 1 1 d . . .
O6 O 0.12337(12) 0.50441(10) 0.31449(9) 0.0249(2) Uani 1 1 d . . .
H61 H 0.028(2) 0.5349(19) 0.3473(16) 0.043(5) Uiso 1 1 d . . .
H62 H 0.162(2) 0.4743(18) 0.3709(17) 0.044(5) Uiso 1 1 d . . .
B1 B 0.01910(16) 0.07258(14) 0.78680(12) 0.0171(3) Uani 1 1 d . . .
C11 C 0.08329(14) 0.18622(12) 0.82922(10) 0.0174(2) Uani 1 1 d . . .
N11 N 0.12807(13) 0.26896(11) 0.85815(10) 0.0234(2) Uani 1 1 d . . .
C12 C 0.09678(14) -0.08470(13) 0.83479(11) 0.0190(2) Uani 1 1 d . . .
N12 N 0.15225(14) -0.19757(11) 0.86815(11) 0.0282(2) Uani 1 1 d . . .
C13 C -0.17858(15) 0.11698(13) 0.84691(11) 0.0213(3) Uani 1 1 d . . .
N13 N -0.31919(14) 0.15496(13) 0.89188(11) 0.0307(3) Uani 1 1 d . . .
C14 C 0.07782(15) 0.07952(12) 0.63986(11) 0.0204(2) Uani 1 1 d . . .
N14 N 0.12300(15) 0.08700(12) 0.53435(10) 0.0310(3) Uani 1 1 d . . .
B2 B 0.51091(16) 0.71767(14) 0.38624(12) 0.0177(3) Uani 1 1 d . . .
C21 C 0.65846(15) 0.65782(12) 0.44066(11) 0.0192(2) Uani 1 1 d . . .
N21 N 0.76325(14) 0.61051(12) 0.47965(11) 0.0293(3) Uani 1 1 d . . .
C22 C 0.34096(15) 0.71804(13) 0.49550(12) 0.0224(3) Uani 1 1 d . . .
N22 N 0.22003(14) 0.71712(13) 0.57383(11) 0.0348(3) Uani 1 1 d . . .
C23 C 0.50653(14) 0.87715(13) 0.33097(12) 0.0215(3) Uani 1 1 d . . .
N23 N 0.50513(14) 0.99126(12) 0.29287(12) 0.0330(3) Uani 1 1 d . . .
C24 C 0.54080(14) 0.61164(12) 0.28182(11) 0.0190(2) Uani 1 1 d . . .
N24 N 0.56406(13) 0.53326(12) 0.20860(10) 0.0256(2) Uani 1 1 d . . .

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
Mg 0.01308(19) 0.01694(19) 0.01411(19) 0.00027(15) -0.00392(14) -0.00336(14)
O1 0.0184(4) 0.0169(4) 0.0309(5) 0.0027(4) -0.0122(4) -0.0051(4)
O2 0.0189(4) 0.0174(4) 0.0341(5) 0.0034(4) -0.0135(4) -0.0059(4)
O3 0.0285(5) 0.0194(5) 0.0178(5) -0.0006(4) -0.0037(4) -0.0099(4)
O4 0.0177(5) 0.0289(5) 0.0193(5) 0.0076(4) -0.0051(4) -0.0071(4)
O5 0.0157(4) 0.0269(5) 0.0190(5) -0.0052(4) -0.0046(4) -0.0037(4)
O6 0.0210(5) 0.0304(5) 0.0187(5) -0.0058(4) -0.0071(4) 0.0021(4)
B1 0.0161(6) 0.0176(6) 0.0179(6) -0.0014(5) -0.0059(5) -0.0048(5)
C11 0.0141(5) 0.0190(5) 0.0158(6) -0.0005(4) -0.0035(4) -0.0020(4)
N11 0.0208(5) 0.0241(5) 0.0254(6) -0.0051(4) -0.0066(4) -0.0062(4)
C12 0.0187(6) 0.0224(6) 0.0176(6) -0.0024(5) -0.0048(5) -0.0089(5)
N12 0.0324(6) 0.0216(6) 0.0313(6) 0.0023(5) -0.0124(5) -0.0079(5)
C13 0.0222(6) 0.0213(6) 0.0224(6) -0.0033(5) -0.0090(5) -0.0058(5)
N13 0.0204(6) 0.0359(6) 0.0343(6) -0.0080(5) -0.0074(5) -0.0049(5)
C14 0.0221(6) 0.0182(6) 0.0226(7) -0.0012(5) -0.0094(5) -0.0056(5)
N14 0.0375(7) 0.0337(6) 0.0230(6) 0.0010(5) -0.0112(5) -0.0111(5)
B2 0.0162(6) 0.0166(6) 0.0180(6) -0.0011(5) -0.0037(5) -0.0037(5)
C21 0.0223(6) 0.0171(5) 0.0168(6) -0.0028(4) -0.0038(5) -0.0062(5)
N21 0.0312(6) 0.0275(6) 0.0320(6) -0.0028(5) -0.0168(5) -0.0041(5)
C22 0.0213(6) 0.0169(6) 0.0252(6) -0.0019(5) -0.0035(5) -0.0049(5)
N22 0.0275(6) 0.0305(6) 0.0359(7) -0.0034(5) 0.0036(5) -0.0100(5)
C23 0.0152(6) 0.0211(6) 0.0240(6) -0.0011(5) -0.0041(5) -0.0020(4)
N23 0.0273(6) 0.0223(6) 0.0443(7) 0.0057(5) -0.0101(5) -0.0052(5)
C24 0.0165(5) 0.0192(6) 0.0206(6) 0.0035(5) -0.0066(5) -0.0055(4)
N24 0.0280(6) 0.0269(6) 0.0243(6) -0.0024(5) -0.0099(5) -0.0089(5)

_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
Mg O2 2.0373(9) . ?
Mg O5 2.0446(10) . ?
Mg O4 2.0521(9) . ?
Mg O1 2.0645(9) . ?
Mg O3 2.0784(9) . ?
Mg O6 2.0912(10) . ?
O1 H11 0.815(19) . ?
O1 H12 0.833(18) . ?
O2 H21 0.84(2) . ?
O2 H22 0.776(19) . ?
O3 H31 0.82(2) . ?
O3 H32 0.82(2) . ?
O4 H41 0.81(2) . ?
O4 H42 0.823(19) . ?
O5 H51 0.800(19) . ?
O5 H52 0.83(2) . ?
O6 H61 0.784(19) . ?
O6 H62 0.830(19) . ?
B1 C14 1.5868(18) . ?
B1 C12 1.5954(17) . ?
B1 C11 1.5972(17) . ?
B1 C13 1.5985(17) . ?
C11 N11 1.1390(15) . ?
C12 N12 1.1397(15) . ?
C13 N13 1.1403(16) . ?
C14 N14 1.1389(16) . ?
B2 C22 1.5915(17) . ?
B2 C23 1.5921(17) . ?
B2 C21 1.5944(17) . ?
B2 C24 1.5956(18) . ?
C21 N21 1.1384(16) . ?
C22 N22 1.1376(16) . ?
C23 N23 1.1369(16) . ?
C24 N24 1.1405(16) . ?

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
O2 Mg O5 89.33(4) . . ?
O2 Mg O4 90.96(4) . . ?
O5 Mg O4 94.36(4) . . ?
O2 Mg O1 177.61(4) . . ?
O5 Mg O1 90.06(4) . . ?
O4 Mg O1 86.79(4) . . ?
O2 Mg O3 92.14(4) . . ?
O5 Mg O3 88.18(4) . . ?
O4 Mg O3 176.01(4) . . ?
O1 Mg O3 90.14(4) . . ?
O2 Mg O6 89.77(4) . . ?
O5 Mg O6 172.84(4) . . ?
O4 Mg O6 92.76(4) . . ?
O1 Mg O6 91.12(4) . . ?
O3 Mg O6 84.75(4) . . ?
Mg O1 H11 123.7(13) . . ?
Mg O1 H12 126.9(12) . . ?
H11 O1 H12 109.0(17) . . ?
Mg O2 H21 122.6(12) . . ?
Mg O2 H22 124.9(13) . . ?
H21 O2 H22 112.4(18) . . ?
Mg O3 H31 123.1(12) . . ?
Mg O3 H32 128.1(13) . . ?
H31 O3 H32 108.7(18) . . ?
Mg O4 H41 124.3(13) . . ?
Mg O4 H42 112.7(12) . . ?
H41 O4 H42 105.1(17) . . ?
Mg O5 H51 123.3(13) . . ?
Mg O5 H52 122.1(13) . . ?
H51 O5 H52 108.9(17) . . ?
Mg O6 H61 121.1(13) . . ?
Mg O6 H62 111.4(12) . . ?
H61 O6 H62 106.0(17) . . ?
C14 B1 C12 110.16(10) . . ?
C14 B1 C11 108.09(9) . . ?
C12 B1 C11 109.06(9) . . ?
C14 B1 C13 111.34(10) . . ?
C12 B1 C13 110.62(9) . . ?
C11 B1 C13 107.47(10) . . ?
N11 C11 B1 178.84(12) . . ?
N12 C12 B1 179.37(13) . . ?
N13 C13 B1 176.45(13) . . ?
N14 C14 B1 177.91(13) . . ?
C22 B2 C23 109.78(10) . . ?
C22 B2 C21 108.52(10) . . ?
C23 B2 C21 109.80(10) . . ?
C22 B2 C24 109.56(10) . . ?
C23 B2 C24 111.18(10) . . ?
C21 B2 C24 107.95(9) . . ?
N21 C21 B2 177.68(12) . . ?
N22 C22 B2 179.43(14) . . ?
N23 C23 B2 178.66(14) . . ?
N24 C24 B2 178.39(12) . . ?

_diffrn_measured_fraction_theta_max 0.843
_diffrn_reflns_theta_full        26.40
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.250
_refine_diff_density_min         -0.186
_refine_diff_density_rms         0.038
_database_code_depnum_ccdc_archive 'CCDC 893429'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Mg_BCN_H2O

_audit_creation_method           'ct.exe (M. Köckerling, 1996)'

_chemical_name_systematic        
;
Magnesium-bis-aqua-bis-tetracyanidoborate
;
_chemical_formula_moiety         '(Mg1 2+), 2(B C4 N4 1-), 2(H2 O1)'
_chemical_formula_sum            'C8 H4 B2 Mg1 N8 O2'
_chemical_formula_weight         290.12

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'
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I -4 2 d'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y, -z+3/4'
'x+1/2, -y, -z+3/4'
'-y+1/2, -x, z+3/4'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1, y+1/2, -z+5/4'
'x+1, -y+1/2, -z+5/4'
'-y+1, -x+1/2, z+5/4'
'y+1, x+1/2, z+5/4'

_cell_length_a                   12.3940(4)
_cell_length_b                   12.3940(4)
_cell_length_c                   9.2041(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1413.85(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    4236
_cell_measurement_theta_min      2.76
_cell_measurement_theta_max      31.13

_exptl_crystal_description       irregular
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             584
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9579
_exptl_absorpt_correction_T_max  0.9917
_exptl_absorpt_process_details   Bruker-Nonius


_diffrn_ambient_temperature      295(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            10358
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0174
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.29
_diffrn_reflns_theta_max         31.99
_reflns_number_total             1233
_reflns_number_gt                1123
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0374P)²+0.0378P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     none
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.18(19)
_refine_ls_number_reflns         1233
_refine_ls_number_parameters     52
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0253
_refine_ls_wR_factor_ref         0.0621
_refine_ls_wR_factor_gt          0.0604
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        31.99
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.177
_refine_diff_density_min         -0.098
_refine_diff_density_rms         0.031


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
Mg1 Mg 1.0000 -0.5000 0.2500 0.02050(11) Uani 1 4 d S . .
O1 O 1.0000 -0.5000 0.02865(9) 0.0441(2) Uani 1 2 d S . .
N1 N 0.85434(6) -0.59803(6) 0.22935(8) 0.03188(17) Uani 1 1 d . . .
C2 C 0.64212(6) -0.80300(7) 0.24894(9) 0.02985(16) Uani 1 1 d . . .
B1 B 0.71432(10) -0.7500 0.1250 0.0248(2) Uani 1 2 d S . .
C1 C 0.79245(6) -0.65944(6) 0.19013(9) 0.02772(16) Uani 1 1 d . . .
N2 N 0.59335(8) -0.84381(8) 0.33771(9) 0.0459(2) Uani 1 1 d . . .
H1 H 1.0259(14) -0.4565(11) -0.0241(17) 0.069 Uiso 1 1 d . . .

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
Mg1 0.02074(14) 0.02074(14) 0.0200(2) 0.000 0.000 0.000
O1 0.0627(7) 0.0460(5) 0.0235(4) 0.000 0.000 -0.0290(6)
N1 0.0301(3) 0.0299(3) 0.0357(4) 0.0033(3) 0.0004(3) -0.0052(3)
C2 0.0292(4) 0.0296(3) 0.0307(3) 0.0004(3) -0.0009(3) -0.0041(3)
B1 0.0224(5) 0.0244(5) 0.0275(5) 0.0033(4) 0.000 0.000
C1 0.0261(3) 0.0279(4) 0.0291(3) 0.0059(3) 0.0016(3) 0.0007(3)
N2 0.0506(5) 0.0469(5) 0.0401(4) 0.0027(4) 0.0097(4) -0.0137(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
Mg1 O1 2.0373(8) 11_655
Mg1 O1 2.0374(8) .
Mg1 N1 2.1843(7) 12_535
Mg1 N1 2.1843(7) 2_745
Mg1 N1 2.1843(7) .
Mg1 N1 2.1844(7) 11_655
N1 C1 1.1393(11) .
C2 N2 1.1353(11) .
C2 B1 1.5917(11) .
B1 C2 1.5917(11) 14_434
B1 C1 1.5991(11) .
B1 C1 1.5991(11) 14_434

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
O1 Mg1 O1 180.0 11_655 .
O1 Mg1 N1 85.01(2) 11_655 12_535
O1 Mg1 N1 94.99(2) . 12_535
O1 Mg1 N1 94.99(2) 11_655 2_745
O1 Mg1 N1 85.01(2) . 2_745
N1 Mg1 N1 90.432(4) 12_535 2_745
O1 Mg1 N1 94.99(2) 11_655 .
O1 Mg1 N1 85.01(2) . .
N1 Mg1 N1 90.435(4) 12_535 .
N1 Mg1 N1 170.02(4) 2_745 .
O1 Mg1 N1 85.01(2) 11_655 11_655
O1 Mg1 N1 94.99(2) . 11_655
N1 Mg1 N1 170.01(4) 12_535 11_655
N1 Mg1 N1 90.434(4) 2_745 11_655
N1 Mg1 N1 90.434(4) . 11_655
C1 N1 Mg1 162.87(7) . .
N2 C2 B1 177.45(9) . .
C2 B1 C2 111.58(9) . 14_434
C2 B1 C1 111.19(4) . .
C2 B1 C1 108.63(4) 14_434 .
C2 B1 C1 108.63(4) . 14_434
C2 B1 C1 111.19(4) 14_434 14_434
C1 B1 C1 105.46(9) . 14_434
N1 C1 B1 174.53(8) . .

# eof


_chemical_name_common            Magnesium-bis-aqua-bis-tetracyanidoborate
_database_code_depnum_ccdc_archive 'CCDC 705243'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Ca_BCN_Aceto

_audit_creation_method           'ct.exe (M. Köckerling, 1996)'

_chemical_name_systematic        
;
Calcium bis-aqua bis-tetracyanoborate acetronitrile solvate
;
_chemical_formula_moiety         '(Ca 2+), (C4 N4 B -1)2, (C2 H3 N), 2(H2 O)'
_chemical_formula_sum            'C10 H7 B2 Ca N9 O2'
_chemical_formula_weight         346.95

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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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                   12.2203(2)
_cell_length_b                   12.6637(2)
_cell_length_c                   13.5191(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.538(1)
_cell_angle_gamma                90.00
_cell_volume                     1871.71(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    213(2)
_cell_measurement_reflns_used    9930
_cell_measurement_theta_min      3.04
_cell_measurement_theta_max      35.96

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.09
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             704
_exptl_absorpt_coefficient_mu    0.356
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9164
_exptl_absorpt_correction_T_max  0.9687
_exptl_absorpt_process_details   'Bruker-Nonius SADABS'

_diffrn_ambient_temperature      213(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            37481
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.44
_diffrn_reflns_theta_max         36.51
_reflns_number_total             8728
_reflns_number_gt                6825
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0490P)²+0.1313P] where P=(Fo²+2Fc²)/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_number_reflns         8728
_refine_ls_number_parameters     234
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0346
_refine_ls_wR_factor_ref         0.0944
_refine_ls_wR_factor_gt          0.0867
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

_diffrn_measured_fraction_theta_max 0.948
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.052


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
Ca1 Ca 0.221247(13) 0.483452(11) 0.834516(11) 0.01858(4) Uani 1 1 d . . .
B1 B -0.03413(8) 0.25157(7) 0.98462(7) 0.02084(14) Uani 1 1 d . . .
N1 N 0.09999(7) 0.35543(7) 0.89831(6) 0.03255(16) Uani 1 1 d . . .
C1 C 0.04418(8) 0.31150(6) 0.93422(6) 0.02488(14) Uani 1 1 d . . .
N2 N 0.11664(8) 0.14397(7) 1.17146(7) 0.03658(18) Uani 1 1 d . . .
C2 C 0.05497(8) 0.18960(7) 1.09352(7) 0.02680(15) Uani 1 1 d . . .
N3 N -0.16067(8) 0.39632(6) 1.04339(7) 0.03412(16) Uani 1 1 d . . .
C3 C -0.11006(8) 0.33577(6) 1.01644(6) 0.02480(14) Uani 1 1 d . . .
N4 N -0.18074(8) 0.10955(7) 0.82988(7) 0.03833(18) Uani 1 1 d . . .
C4 C -0.12282(8) 0.16965(7) 0.89549(7) 0.02650(15) Uani 1 1 d . . .
B2 B -0.25898(9) 0.52285(8) 0.63382(8) 0.02745(17) Uani 1 1 d . . .
N5 N -0.00975(8) 0.52944(8) 0.73141(7) 0.03878(19) Uani 1 1 d . . .
C5 C -0.11397(9) 0.52839(7) 0.68962(8) 0.03182(17) Uani 1 1 d . . .
N6 N -0.33428(12) 0.32741(8) 0.54458(11) 0.0592(3) Uani 1 1 d . . .
C6 C -0.30292(10) 0.40995(8) 0.57928(9) 0.03685(19) Uani 1 1 d . . .
N7 N -0.33570(13) 0.54661(12) 0.79336(11) 0.0658(3) Uani 1 1 d . . .
C7 C -0.30389(11) 0.53839(10) 0.72632(9) 0.0415(2) Uani 1 1 d . . .
N8 N -0.35172(11) 0.68157(8) 0.48286(9) 0.0556(3) Uani 1 1 d . . .
C8 C -0.31416(9) 0.61386(7) 0.54417(8) 0.03370(18) Uani 1 1 d . . .
N9 N 0.38856(9) 0.39287(8) 0.80496(7) 0.0435(2) Uani 1 1 d . . .
C9 C 0.46043(9) 0.34375(9) 0.79461(7) 0.0356(2) Uani 1 1 d . . .
C10 C 0.55341(11) 0.28067(11) 0.78278(10) 0.0469(3) Uani 1 1 d . . .
H10A H 0.6330 0.2967 0.8428 0.070 Uiso 1 1 calc R . .
H10B H 0.5536 0.2969 0.7127 0.070 Uiso 1 1 calc R . .
H10C H 0.5356 0.2063 0.7849 0.070 Uiso 1 1 calc R . .
O1 O 0.37958(7) 0.61012(6) 0.91291(7) 0.03687(15) Uani 1 1 d . . .
H1 H 0.3667(15) 0.6727(13) 0.9275(13) 0.061(4) Uiso 1 1 d . . .
H2 H 0.4597(16) 0.6006(12) 0.9377(13) 0.058(4) Uiso 1 1 d . . .
O2 O 0.36390(6) 0.40646(5) 1.01410(5) 0.02702(12) Uani 1 1 d . . .
H3 H 0.3506(14) 0.4295(13) 1.0655(14) 0.063(5) Uiso 1 1 d . . .
H4 H 0.3508(14) 0.3394(13) 1.0160(13) 0.062(5) Uiso 1 1 d . . .

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
Ca1 0.01654(7) 0.01989(7) 0.01938(6) -0.00060(4) 0.00808(5) 0.00037(4)
B1 0.0216(4) 0.0213(3) 0.0210(3) -0.0001(3) 0.0109(3) 0.0008(3)
N1 0.0286(4) 0.0380(4) 0.0318(3) 0.0060(3) 0.0143(3) -0.0025(3)
C1 0.0235(4) 0.0269(3) 0.0246(3) 0.0027(3) 0.0110(3) 0.0012(3)
N2 0.0354(4) 0.0411(4) 0.0327(4) 0.0127(3) 0.0147(3) 0.0062(3)
C2 0.0279(4) 0.0269(4) 0.0275(3) 0.0038(3) 0.0141(3) 0.0013(3)
N3 0.0325(4) 0.0329(4) 0.0408(4) -0.0096(3) 0.0199(3) -0.0002(3)
C3 0.0240(4) 0.0252(3) 0.0260(3) -0.0035(3) 0.0118(3) -0.0017(3)
N4 0.0368(5) 0.0363(4) 0.0382(4) -0.0132(3) 0.0134(3) -0.0018(3)
C4 0.0268(4) 0.0265(4) 0.0274(3) -0.0037(3) 0.0132(3) 0.0016(3)
B2 0.0243(4) 0.0280(4) 0.0302(4) 0.0025(3) 0.0123(3) 0.0031(3)
N5 0.0272(4) 0.0487(5) 0.0373(4) 0.0049(3) 0.0115(3) 0.0062(3)
C5 0.0270(4) 0.0355(4) 0.0316(4) 0.0047(3) 0.0118(3) 0.0052(3)
N6 0.0684(8) 0.0323(5) 0.0807(8) -0.0053(5) 0.0367(6) -0.0068(5)
C6 0.0385(5) 0.0294(4) 0.0454(5) 0.0024(4) 0.0212(4) 0.0002(4)
N7 0.0687(8) 0.0881(9) 0.0566(7) -0.0037(6) 0.0423(6) 0.0066(7)
C7 0.0376(6) 0.0502(6) 0.0411(5) -0.0014(4) 0.0216(4) 0.0040(4)
N8 0.0570(7) 0.0373(5) 0.0534(6) 0.0108(4) 0.0077(5) 0.0059(4)
C8 0.0284(4) 0.0284(4) 0.0368(4) 0.0002(3) 0.0078(3) 0.0010(3)
N9 0.0323(5) 0.0609(6) 0.0376(4) -0.0109(4) 0.0158(3) 0.0082(4)
C9 0.0277(5) 0.0496(5) 0.0282(4) -0.0055(4) 0.0113(3) 0.0051(4)
C10 0.0355(6) 0.0597(7) 0.0470(6) -0.0019(5) 0.0198(4) 0.0173(5)
O1 0.0223(3) 0.0265(3) 0.0560(4) -0.0069(3) 0.0122(3) -0.0038(2)
O2 0.0260(3) 0.0276(3) 0.0264(3) 0.0014(2) 0.0108(2) 0.0009(2)

_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O1 2.3680(7) .
Ca1 O2 2.4702(6) .
Ca1 N9 2.5271(9) .
Ca1 N2 2.5650(8) 4_565
Ca1 N3 2.5849(8) 3_567
Ca1 N1 2.5904(8) .
Ca1 N5 2.5951(9) .
Ca1 N4 2.5983(8) 2_556
B1 C4 1.5924(12) .
B1 C2 1.5926(12) .
B1 C1 1.5935(12) .
B1 C3 1.5937(11) .
N1 C1 1.1428(11) .
N2 C2 1.1413(11) .
N2 Ca1 2.5650(8) 4_566
N3 C3 1.1422(11) .
N3 Ca1 2.5849(8) 3_567
N4 C4 1.1428(11) .
N4 Ca1 2.5983(8) 2_546
B2 C7 1.5865(15) .
B2 C5 1.5874(14) .
B2 C8 1.5880(13) .
B2 C6 1.5881(14) .
N5 C5 1.1395(13) .
N6 C6 1.1397(14) .
N7 C7 1.1394(15) .
N8 C8 1.1371(13) .
N9 C9 1.1347(12) .
C9 C10 1.4551(14) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C10 H10C 0.9700 .
O1 H1 0.848(17) .
O1 H2 0.890(17) .
O2 H3 0.834(17) .
O2 H4 0.866(17) .

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
O1 Ca1 O2 75.57(3) . .
O1 Ca1 N9 79.70(3) . .
O2 Ca1 N9 73.18(3) . .
O1 Ca1 N2 143.57(3) . 4_565
O2 Ca1 N2 117.27(3) . 4_565
N9 Ca1 N2 72.92(3) . 4_565
O1 Ca1 N3 74.04(3) . 3_567
O2 Ca1 N3 83.26(3) . 3_567
N9 Ca1 N3 148.33(3) . 3_567
N2 Ca1 N3 138.10(3) 4_565 3_567
O1 Ca1 N1 138.55(3) . .
O2 Ca1 N1 71.53(2) . .
N9 Ca1 N1 113.09(3) . .
N2 Ca1 N1 75.69(3) 4_565 .
N3 Ca1 N1 77.67(3) 3_567 .
O1 Ca1 N5 124.30(3) . .
O2 Ca1 N5 137.48(3) . .
N9 Ca1 N5 141.24(3) . .
N2 Ca1 N5 71.02(3) 4_565 .
N3 Ca1 N5 69.98(3) 3_567 .
N1 Ca1 N5 70.88(3) . .
O1 Ca1 N4 76.81(3) . 2_556
O2 Ca1 N4 149.81(3) . 2_556
N9 Ca1 N4 90.12(3) . 2_556
N2 Ca1 N4 79.64(3) 4_565 2_556
N3 Ca1 N4 100.64(3) 3_567 2_556
N1 Ca1 N4 138.65(3) . 2_556
N5 Ca1 N4 69.93(3) . 2_556
C4 B1 C2 109.37(7) . .
C4 B1 C1 108.81(6) . .
C2 B1 C1 109.69(7) . .
C4 B1 C3 111.02(7) . .
C2 B1 C3 108.68(6) . .
C1 B1 C3 109.27(6) . .
C1 N1 Ca1 170.00(8) . .
N1 C1 B1 179.32(9) . .
C2 N2 Ca1 169.09(8) . 4_566
N2 C2 B1 178.48(9) . .
C3 N3 Ca1 161.70(8) . 3_567
N3 C3 B1 177.26(9) . .
C4 N4 Ca1 152.68(8) . 2_546
N4 C4 B1 175.78(9) . .
C7 B2 C5 109.01(8) . .
C7 B2 C8 109.45(8) . .
C5 B2 C8 109.50(8) . .
C7 B2 C6 108.26(8) . .
C5 B2 C6 109.55(8) . .
C8 B2 C6 111.03(8) . .
C5 N5 Ca1 166.00(8) . .
N5 C5 B2 177.81(10) . .
N6 C6 B2 176.88(12) . .
N7 C7 B2 178.09(13) . .
N8 C8 B2 177.59(11) . .
C9 N9 Ca1 173.61(10) . .
N9 C9 C10 179.31(11) . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
Ca1 O1 H1 122.6(11) . .
Ca1 O1 H2 128.1(10) . .
H1 O1 H2 109.0(14) . .
Ca1 O2 H3 111.5(11) . .
Ca1 O2 H4 110.9(11) . .
H3 O2 H4 102.1(15) . .


# eof
_database_code_depnum_ccdc_archive 'CCDC 705244'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Ca_BCN_H2O

_audit_creation_method           'ct.exe (M. Köckerling, 1996)'

_chemical_name_systematic        
;
Calcium tris-aqua bis-tetracyanoborate
;


_chemical_formula_moiety         '(Ca 2+) (C4 B N4 1-)2 3(H2 O)'
_chemical_formula_sum            'C8 H6 B2 Ca N8 O3'
_chemical_formula_weight         323.91

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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.5347(2)
_cell_length_b                   10.2205(2)
_cell_length_c                   10.4874(2)
_cell_angle_alpha                68.283(1)
_cell_angle_beta                 89.223(1)
_cell_angle_gamma                63.152(1)
_cell_volume                     832.45(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9962
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      42.81

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             328
_exptl_absorpt_coefficient_mu    0.397
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9072
_exptl_absorpt_correction_T_max  0.9651
_exptl_absorpt_process_details   'Bruker-Nonius SADABS'


_diffrn_ambient_temperature      173(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            44979
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0180
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.52
_diffrn_reflns_theta_max         42.81
_reflns_number_total             11424
_reflns_number_gt                10189
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0403P)²+0.0935P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_number_reflns         11424
_refine_ls_number_parameters     223
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0279
_refine_ls_wR_factor_ref         0.0785
_refine_ls_wR_factor_gt          0.0763
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

_diffrn_measured_fraction_theta_max 0.937
_diffrn_reflns_theta_full        42.81
_diffrn_measured_fraction_theta_full 0.937
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.058



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
Ca1 Ca 0.864416(10) 0.588309(10) 0.309936(9) 0.01251(2) Uani 1 1 d . . .
O1 O 1.13314(4) 0.38366(4) 0.46201(4) 0.01485(5) Uani 1 1 d . . .
H1 H 1.1495(14) 0.2910(14) 0.4787(12) 0.035(3) Uiso 1 1 d . . .
H2 H 1.2129(15) 0.3865(14) 0.4257(13) 0.038(3) Uiso 1 1 d . . .
O2 O 1.03464(6) 0.67635(6) 0.17945(5) 0.02577(8) Uani 1 1 d . . .
H3 H 0.9919(17) 0.7687(18) 0.1115(15) 0.051(4) Uiso 1 1 d . . .
H4 H 1.1138(17) 0.6210(17) 0.1520(14) 0.052(4) Uiso 1 1 d . . .
O3 O 0.96397(7) 0.39662(7) 0.20393(6) 0.03481(12) Uani 1 1 d . . .
H5 H 0.9038(17) 0.4047(17) 0.1371(15) 0.052(4) Uiso 1 1 d . . .
H6 H 1.023(2) 0.300(2) 0.2528(17) 0.071(5) Uiso 1 1 d . . .
B1 B 0.55335(6) 1.21722(6) 0.12973(5) 0.01531(7) Uani 1 1 d . . .
N1 N 0.73957(6) 0.88998(6) 0.24321(5) 0.02304(8) Uani 1 1 d . . .
C1 C 0.66286(6) 1.02723(6) 0.19804(5) 0.01777(7) Uani 1 1 d . . .
N2 N 0.32430(7) 1.29550(7) -0.08021(6) 0.02633(9) Uani 1 1 d . . .
C2 C 0.42118(6) 1.26266(6) 0.00694(5) 0.01980(8) Uani 1 1 d . . .
N3 N 0.39445(8) 1.33246(9) 0.31570(7) 0.03352(12) Uani 1 1 d . . .
C3 C 0.46418(6) 1.28074(7) 0.24053(6) 0.02042(8) Uani 1 1 d . . .
N4 N 0.74019(8) 1.35944(8) 0.03337(8) 0.03147(11) Uani 1 1 d . . .
C4 C 0.66129(6) 1.29983(6) 0.07140(6) 0.02013(8) Uani 1 1 d . . .
B2 B 0.73910(6) 0.14521(6) 0.64978(6) 0.01647(8) Uani 1 1 d . . .
N5 N 0.84684(7) 0.34767(7) 0.48959(6) 0.02645(9) Uani 1 1 d . . .
C5 C 0.80569(6) 0.26059(6) 0.56061(6) 0.01948(8) Uani 1 1 d . . .
N6 N 0.42105(6) 0.31819(7) 0.64845(6) 0.02551(9) Uani 1 1 d . . .
C6 C 0.55416(6) 0.24839(6) 0.64554(6) 0.01916(8) Uani 1 1 d . . .
N7 N 0.79310(9) -0.08078(7) 0.54726(8) 0.03581(13) Uani 1 1 d . . .
C7 C 0.76653(7) 0.01804(7) 0.58621(6) 0.02325(9) Uani 1 1 d . . .
N8 N 0.88444(10) -0.03273(10) 0.92421(7) 0.04181(16) Uani 1 1 d . . .
C8 C 0.82700(7) 0.04624(7) 0.80855(6) 0.02492(10) Uani 1 1 d . . .

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
Ca1 0.01128(3) 0.01225(3) 0.01140(3) -0.00422(2) 0.00117(2) -0.00406(2)
O1 0.01331(12) 0.01428(12) 0.01545(13) -0.00735(10) 0.00257(10) -0.00442(10)
O2 0.02302(18) 0.02328(18) 0.02317(18) -0.00391(15) 0.00973(14) -0.00944(15)
O3 0.0372(3) 0.0239(2) 0.0312(2) -0.01652(19) -0.0093(2) -0.00044(19)
B1 0.01557(18) 0.01398(17) 0.01385(17) -0.00555(14) 0.00172(14) -0.00517(15)
N1 0.0254(2) 0.01463(16) 0.02194(18) -0.00517(14) 0.00256(15) -0.00571(15)
C1 0.01900(18) 0.01513(16) 0.01573(16) -0.00536(13) 0.00138(13) -0.00617(14)
N2 0.0233(2) 0.0261(2) 0.0221(2) -0.01084(17) -0.00449(16) -0.00494(17)
C2 0.01943(18) 0.01793(18) 0.01703(18) -0.00725(15) -0.00074(14) -0.00481(15)
N3 0.0316(3) 0.0404(3) 0.0283(2) -0.0205(2) 0.0137(2) -0.0122(2)
C3 0.01924(19) 0.0221(2) 0.01798(18) -0.00949(16) 0.00471(15) -0.00741(16)
N4 0.0291(2) 0.0274(2) 0.0422(3) -0.0148(2) 0.0145(2) -0.0168(2)
C4 0.02003(19) 0.01715(18) 0.0222(2) -0.00850(16) 0.00583(16) -0.00783(16)
B2 0.01452(18) 0.01355(17) 0.0186(2) -0.00468(15) 0.00321(15) -0.00609(15)
N5 0.0251(2) 0.02146(19) 0.0326(2) -0.00775(18) 0.01048(18) -0.01379(17)
C5 0.01655(17) 0.01592(17) 0.0238(2) -0.00647(15) 0.00565(15) -0.00742(15)
N6 0.01571(17) 0.0299(2) 0.0268(2) -0.01086(18) 0.00499(15) -0.00829(16)
C6 0.01558(17) 0.02026(19) 0.01980(18) -0.00717(15) 0.00392(14) -0.00796(15)
N7 0.0410(3) 0.0218(2) 0.0404(3) -0.0165(2) 0.0012(3) -0.0086(2)
C7 0.0239(2) 0.01576(18) 0.0263(2) -0.00784(17) 0.00305(18) -0.00703(17)
N8 0.0443(4) 0.0435(4) 0.0248(3) 0.0022(2) -0.0061(2) -0.0234(3)
C8 0.0231(2) 0.0232(2) 0.0221(2) -0.00287(18) 0.00004(17) -0.01103(19)

_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
Ca1 O2 2.3800(4) .
Ca1 O3 2.4246(5) .
Ca1 O1 2.5070(4) .
Ca1 O1 2.5135(4) 2_766
Ca1 N6 2.5375(5) 2_666
Ca1 N2 2.5539(5) 2_675
Ca1 N1 2.5542(5) .
Ca1 N5 2.5615(5) .
Ca1 Ca1 4.07117(19) 2_766
O1 Ca1 2.5135(4) 2_766
B1 C3 1.5899(7) .
B1 C4 1.5912(8) .
B1 C1 1.5917(7) .
B1 C2 1.5920(7) .
N1 C1 1.1480(7) .
N2 C2 1.1477(7) .
N2 Ca1 2.5539(5) 2_675
N3 C3 1.1488(7) .
N4 C4 1.1499(8) .
B2 C6 1.5848(7) .
B2 C5 1.5850(7) .
B2 C8 1.5886(8) .
B2 C7 1.5911(8) .
N5 C5 1.1479(7) .
N6 C6 1.1480(7) .
N6 Ca1 2.5375(5) 2_666
N7 C7 1.1500(8) .
N8 C8 1.1476(9) .

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
O2 Ca1 O3 81.75(2) . .
O2 Ca1 O1 78.596(15) . .
O3 Ca1 O1 77.850(15) . .
O2 Ca1 O1 110.084(16) . 2_766
O3 Ca1 O1 143.792(16) . 2_766
O1 Ca1 O1 71.630(13) . 2_766
O2 Ca1 N6 143.250(18) . 2_666
O3 Ca1 N6 116.93(2) . 2_666
O1 Ca1 N6 133.978(16) . 2_666
O1 Ca1 N6 74.392(16) 2_766 2_666
O2 Ca1 N2 88.48(2) . 2_675
O3 Ca1 N2 71.164(18) . 2_675
O1 Ca1 N2 147.834(15) . 2_675
O1 Ca1 N2 140.423(15) 2_766 2_675
N6 Ca1 N2 70.506(19) 2_666 2_675
O2 Ca1 N1 72.886(17) . .
O3 Ca1 N1 140.370(19) . .
O1 Ca1 N1 124.335(16) . .
O1 Ca1 N1 74.865(15) 2_766 .
N6 Ca1 N1 73.447(19) 2_666 .
N2 Ca1 N1 78.101(18) 2_675 .
O2 Ca1 N5 145.383(18) . .
O3 Ca1 N5 77.62(2) . .
O1 Ca1 N5 70.114(16) . .
O1 Ca1 N5 74.057(17) 2_766 .
N6 Ca1 N5 71.360(19) 2_666 .
N2 Ca1 N5 110.30(2) 2_675 .
N1 Ca1 N5 137.916(18) . .
O2 Ca1 Ca1 95.178(13) . 2_766
O3 Ca1 Ca1 111.626(13) . 2_766
O1 Ca1 Ca1 35.868(8) . 2_766
O1 Ca1 Ca1 35.761(8) 2_766 2_766
N6 Ca1 Ca1 105.158(13) 2_666 2_766
N2 Ca1 Ca1 175.662(14) 2_675 2_766
N1 Ca1 Ca1 100.727(13) . 2_766
N5 Ca1 Ca1 67.725(15) . 2_766
Ca1 O1 Ca1 108.371(13) . 2_766
C3 B1 C4 108.93(4) . .
C3 B1 C1 111.29(4) . .
C4 B1 C1 109.44(4) . .
C3 B1 C2 108.09(4) . .
C4 B1 C2 110.73(4) . .
C1 B1 C2 108.36(4) . .
C1 N1 Ca1 167.74(5) . .
N1 C1 B1 177.52(5) . .
C2 N2 Ca1 166.18(5) . 2_675
N2 C2 B1 178.96(6) . .
N3 C3 B1 176.92(6) . .
N4 C4 B1 177.82(6) . .
C6 B2 C5 109.38(4) . .
C6 B2 C8 108.24(4) . .
C5 B2 C8 112.94(5) . .
C6 B2 C7 110.07(4) . .
C5 B2 C7 109.14(4) . .
C8 B2 C7 107.04(4) . .
C5 N5 Ca1 165.85(5) . .
N5 C5 B2 175.97(6) . .
C6 N6 Ca1 167.34(5) . 2_666
N6 C6 B2 176.90(6) . .
N7 C7 B2 175.92(7) . .
N8 C8 B2 174.37(7) . .

# eof


_database_code_depnum_ccdc_archive 'CCDC 705245'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Mg_TCB_DMF


_audit_creation_method           'ct.exe (M. Köckerling, 1996)'

_chemical_name_systematic        
;
Hexakis-dimethylformamide-magnesium(II) bis-tetracyanidoborate
;
_chemical_formula_moiety         '(Mg1 2+), 2(B C4 N4 1-), 6(C3 H7 O1 N1)'
_chemical_formula_sum            'C26 H42 B2 Mg N14 O6'
_chemical_formula_weight         692.67

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'
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.6187(4)
_cell_length_b                   11.1119(5)
_cell_length_c                   12.2149(5)
_cell_angle_alpha                66.096(2)
_cell_angle_beta                 75.570(2)
_cell_angle_gamma                76.422(2)
_cell_volume                     1023.85(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    7093
_cell_measurement_theta_min      3.79
_cell_measurement_theta_max      32.14

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.34
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             366
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9612
_exptl_absorpt_correction_T_max  0.9684
_exptl_absorpt_process_details   'Bruker-Nonius SADABS'


_diffrn_ambient_temperature      173(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  'CCD area detector, Bruker-Nonius Apex X8'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            19459
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.42
_diffrn_reflns_theta_max         32.61
_reflns_number_total             7410
_reflns_number_gt                5446
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0772P)²+0.0982P] 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_number_reflns         7410
_refine_ls_number_parameters     223
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0445
_refine_ls_wR_factor_ref         0.1401
_refine_ls_wR_factor_gt          0.1253
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        32.61
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.048

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 1.22239(16) 0.14481(12) 0.16449(11) 0.0386(2) Uani 1 1 d . . .
C1 C 1.20712(18) 0.15564(14) 0.03334(11) 0.0523(3) Uani 1 1 d . . .
N1 N 1.1934(2) 0.16504(17) -0.06023(12) 0.0795(4) Uani 1 1 d . . .
C2 C 1.35556(14) 0.22812(11) 0.15425(11) 0.0442(2) Uani 1 1 d . . .
N2 N 1.44851(15) 0.28908(13) 0.14972(13) 0.0637(3) Uani 1 1 d . . .
C3 C 1.27037(18) -0.00619(12) 0.24763(11) 0.0507(3) Uani 1 1 d . . .
N3 N 1.3062(2) -0.11380(12) 0.30851(13) 0.0771(4) Uani 1 1 d . . .
C4 C 1.05320(15) 0.20535(12) 0.22574(10) 0.0430(2) Uani 1 1 d . . .
N4 N 0.93317(15) 0.25062(15) 0.26890(11) 0.0616(3) Uani 1 1 d . . .
Mg1 Mg 1.0000 0.5000 0.5000 0.02656(10) Uani 1 2 d S . .
O1 O 0.81994(8) 0.50405(7) 0.41574(6) 0.03324(15) Uani 1 1 d . . .
C5 C 0.73238(11) 0.41857(9) 0.44256(8) 0.02994(17) Uani 1 1 d . . .
H5A H 0.7501 0.3379 0.5097 0.036 Uiso 1 1 calc R . .
N5 N 0.61652(9) 0.43293(8) 0.38360(8) 0.03289(17) Uani 1 1 d . . .
C6 C 0.52209(14) 0.32716(13) 0.41630(14) 0.0494(3) Uani 1 1 d . . .
H6A H 0.5524 0.2537 0.4896 0.074 Uiso 1 1 calc R . .
H6B H 0.5437 0.2950 0.3494 0.074 Uiso 1 1 calc R . .
H6C H 0.4065 0.3614 0.4320 0.074 Uiso 1 1 calc R . .
C7 C 0.58763(19) 0.55097(16) 0.27706(13) 0.0625(4) Uani 1 1 d . . .
H7A H 0.6581 0.6145 0.2650 0.094 Uiso 1 1 calc R . .
H7B H 0.4740 0.5920 0.2886 0.094 Uiso 1 1 calc R . .
H7C H 0.6113 0.5262 0.2055 0.094 Uiso 1 1 calc R . .
O2 O 1.14153(9) 0.56950(7) 0.33100(6) 0.03486(15) Uani 1 1 d . . .
C8 C 1.14112(11) 0.54413(10) 0.24131(9) 0.03233(18) Uani 1 1 d . . .
H8A H 1.1055 0.4637 0.2551 0.039 Uiso 1 1 calc R . .
N6 N 1.18700(11) 0.62159(9) 0.12807(8) 0.03788(19) Uani 1 1 d . . .
C9 C 1.18427(19) 0.58583(15) 0.02667(11) 0.0549(3) Uani 1 1 d . . .
H9A H 1.1495 0.4983 0.0577 0.082 Uiso 1 1 calc R . .
H9B H 1.2931 0.5825 -0.0223 0.082 Uiso 1 1 calc R . .
H9C H 1.1084 0.6525 -0.0238 0.082 Uiso 1 1 calc R . .
C10 C 1.2354(2) 0.74899(13) 0.09993(12) 0.0570(3) Uani 1 1 d . . .
H10A H 1.2323 0.7610 0.1757 0.086 Uiso 1 1 calc R . .
H10B H 1.1608 0.8208 0.0520 0.086 Uiso 1 1 calc R . .
H10C H 1.3457 0.7512 0.0531 0.086 Uiso 1 1 calc R . .
O3 O 0.91210(9) 0.69617(7) 0.48091(6) 0.03409(15) Uani 1 1 d . . .
C11 C 0.85807(12) 0.78148(9) 0.39046(9) 0.03222(18) Uani 1 1 d . . .
H11A H 0.8663 0.7578 0.3225 0.039 Uiso 1 1 calc R . .
N7 N 0.78980(11) 0.90325(8) 0.38307(8) 0.03515(18) Uani 1 1 d . . .
C12 C 0.71789(18) 0.99647(12) 0.27843(12) 0.0525(3) Uani 1 1 d . . .
H12A H 0.7370 0.9562 0.2173 0.079 Uiso 1 1 calc R . .
H12B H 0.7671 1.0780 0.2435 0.079 Uiso 1 1 calc R . .
H12C H 0.6010 1.0181 0.3039 0.079 Uiso 1 1 calc R . .
C13 C 0.7741(2) 0.94434(13) 0.48429(12) 0.0562(3) Uani 1 1 d . . .
H13A H 0.8275 0.8725 0.5482 0.084 Uiso 1 1 calc R . .
H13B H 0.6591 0.9641 0.5166 0.084 Uiso 1 1 calc R . .
H13C H 0.8251 1.0242 0.4565 0.084 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
B1 0.0465(6) 0.0390(6) 0.0317(5) -0.0128(4) -0.0089(4) -0.0072(5)
C1 0.0639(8) 0.0558(7) 0.0381(6) -0.0199(5) -0.0094(5) -0.0052(6)
N1 0.1035(11) 0.0967(11) 0.0459(6) -0.0359(7) -0.0167(7) -0.0074(9)
C2 0.0422(5) 0.0389(5) 0.0462(6) -0.0120(4) -0.0079(4) -0.0033(4)
N2 0.0517(6) 0.0600(7) 0.0796(9) -0.0212(6) -0.0120(6) -0.0167(5)
C3 0.0728(8) 0.0410(6) 0.0431(6) -0.0145(5) -0.0159(6) -0.0128(5)
N3 0.1250(13) 0.0415(6) 0.0659(8) -0.0096(6) -0.0342(8) -0.0141(7)
C4 0.0464(6) 0.0532(6) 0.0342(5) -0.0165(5) -0.0101(4) -0.0122(5)
N4 0.0493(6) 0.0875(9) 0.0545(7) -0.0361(6) -0.0062(5) -0.0073(6)
Mg1 0.0271(2) 0.0272(2) 0.0250(2) -0.00703(15) -0.00776(15) -0.00461(15)
O1 0.0332(3) 0.0342(3) 0.0337(3) -0.0083(3) -0.0128(3) -0.0078(2)
C5 0.0282(4) 0.0308(4) 0.0311(4) -0.0113(3) -0.0076(3) -0.0025(3)
N5 0.0259(3) 0.0392(4) 0.0373(4) -0.0166(3) -0.0085(3) -0.0040(3)
C6 0.0374(5) 0.0523(6) 0.0702(8) -0.0285(6) -0.0133(5) -0.0131(5)
C7 0.0603(8) 0.0700(9) 0.0531(7) 0.0016(6) -0.0346(6) -0.0200(7)
O2 0.0355(3) 0.0403(4) 0.0278(3) -0.0102(3) -0.0034(3) -0.0106(3)
C8 0.0314(4) 0.0326(4) 0.0311(4) -0.0098(3) -0.0063(3) -0.0041(3)
N6 0.0448(5) 0.0391(4) 0.0279(4) -0.0096(3) -0.0084(3) -0.0057(3)
C9 0.0725(8) 0.0632(8) 0.0335(5) -0.0193(5) -0.0162(5) -0.0082(6)
C10 0.0843(10) 0.0462(6) 0.0361(6) -0.0058(5) -0.0036(6) -0.0260(6)
O3 0.0392(4) 0.0295(3) 0.0335(3) -0.0102(3) -0.0118(3) -0.0018(3)
C11 0.0360(4) 0.0300(4) 0.0321(4) -0.0118(3) -0.0094(3) -0.0033(3)
N7 0.0426(4) 0.0296(4) 0.0342(4) -0.0114(3) -0.0140(3) 0.0000(3)
C12 0.0711(8) 0.0358(5) 0.0517(7) -0.0098(5) -0.0347(6) 0.0038(5)
C13 0.0862(10) 0.0408(6) 0.0452(6) -0.0229(5) -0.0212(6) 0.0071(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
B1 C3 1.5875(18) .
B1 C2 1.5886(17) .
B1 C1 1.5936(17) .
B1 C4 1.5944(18) .
C1 N1 1.1384(17) .
C2 N2 1.1428(16) .
C3 N3 1.1396(17) .
C4 N4 1.1401(17) .
Mg1 O1 2.0483(6) 2_766
Mg1 O1 2.0483(6) .
Mg1 O2 2.0594(7) 2_766
Mg1 O2 2.0594(7) .
Mg1 O3 2.0689(7) 2_766
Mg1 O3 2.0689(7) .
O1 C5 1.2410(11) .
C5 N5 1.3159(12) .
C5 H5A 0.9500 .
N5 C7 1.4494(15) .
N5 C6 1.4526(13) .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
O2 C8 1.2379(12) .
C8 N6 1.3164(13) .
C8 H8A 0.9500 .
N6 C10 1.4518(15) .
N6 C9 1.4527(14) .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
O3 C11 1.2396(11) .
C11 N7 1.3187(13) .
C11 H11A 0.9500 .
N7 C13 1.4494(14) .
N7 C12 1.4530(14) .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .

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
C3 B1 C2 109.08(10) . .
C3 B1 C1 110.34(10) . .
C2 B1 C1 110.74(10) . .
C3 B1 C4 109.77(10) . .
C2 B1 C4 107.79(9) . .
C1 B1 C4 109.08(10) . .
N1 C1 B1 178.64(17) . .
N2 C2 B1 177.94(13) . .
N3 C3 B1 178.70(14) . .
N4 C4 B1 178.85(13) . .
O1 Mg1 O1 180.0 2_766 .
O1 Mg1 O2 88.32(3) 2_766 2_766
O1 Mg1 O2 91.68(3) . 2_766
O1 Mg1 O2 91.68(3) 2_766 .
O1 Mg1 O2 88.32(3) . .
O2 Mg1 O2 179.999(1) 2_766 .
O1 Mg1 O3 88.88(3) 2_766 2_766
O1 Mg1 O3 91.12(3) . 2_766
O2 Mg1 O3 87.98(3) 2_766 2_766
O2 Mg1 O3 92.02(3) . 2_766
O1 Mg1 O3 91.12(3) 2_766 .
O1 Mg1 O3 88.88(3) . .
O2 Mg1 O3 92.02(3) 2_766 .
O2 Mg1 O3 87.98(3) . .
O3 Mg1 O3 180.0 2_766 .
C5 O1 Mg1 128.96(6) . .
O1 C5 N5 123.98(9) . .
O1 C5 H5A 118.0 . .
N5 C5 H5A 118.0 . .
C5 N5 C7 120.92(9) . .
C5 N5 C6 121.48(9) . .
C7 N5 C6 117.41(10) . .
N5 C6 H6A 109.5 . .
N5 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
N5 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
N5 C7 H7A 109.5 . .
N5 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
N5 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C8 O2 Mg1 126.60(6) . .
O2 C8 N6 124.10(9) . .
O2 C8 H8A 117.9 . .
N6 C8 H8A 117.9 . .
C8 N6 C10 120.98(9) . .
C8 N6 C9 121.43(10) . .
C10 N6 C9 117.54(10) . .
N6 C9 H9A 109.5 . .
N6 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
N6 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
N6 C10 H10A 109.5 . .
N6 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
N6 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C11 O3 Mg1 124.16(6) . .
O3 C11 N7 123.81(9) . .
O3 C11 H11A 118.1 . .
N7 C11 H11A 118.1 . .
C11 N7 C13 120.24(9) . .
C11 N7 C12 121.62(9) . .
C13 N7 C12 117.99(9) . .
N7 C12 H12A 109.5 . .
N7 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
N7 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
N7 C13 H13A 109.5 . .
N7 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
N7 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .


# eof


_database_code_depnum_ccdc_archive 'CCDC 884526'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_exp_1970
#TrackingRef 'web_deposit_cif_file_1_Bernhardt_1343128735.exp_1970.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H4 B2 Mg N8 O2'
_chemical_formula_sum            'C8 H4 B2 Mg N8 O2'
_chemical_formula_weight         290.12

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   I-42d
_symmetry_space_group_name_Hall  'I -4 2bw'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y+1/2, -z+1/4'
'-x, -y, z'
'-x, y+1/2, -z+1/4'
'-y+1/2, -x, z+3/4'
'-y, x, -z'
'y, -x, -z'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1, -z+3/4'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1, -z+3/4'
'-y+1, -x+1/2, z+5/4'
'-y+1/2, x+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'y+1, x+1/2, z+5/4'

_cell_length_a                   12.3683(2)
_cell_length_b                   12.3683(2)
_cell_length_c                   9.1712(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1402.96(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    3553
_cell_measurement_theta_min      5.0529
_cell_measurement_theta_max      62.3012

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.3140
_exptl_crystal_size_mid          0.2965
_exptl_crystal_size_min          0.0858
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_crystal_face_indexfrac_h
_exptl_crystal_face_indexfrac_k
_exptl_crystal_face_indexfrac_l
_exptl_crystal_face_x
_exptl_crystal_face_y
_exptl_crystal_face_z
7 -4 -1 0.0510 7.0468 -3.8653 -1.2422 0.1831 0.9969 0.1090
3 5 4 0.1767 2.9885 4.5136 4.3187 -0.7819 -0.0205 0.6059
0 2 -6 0.1479 0.0417 1.7068 -5.9082 -0.0084 0.2181 -0.9905
2 -2 6 0.1311 1.9696 -1.7055 5.9129 -0.0773 0.0106 1.0413
8 0 2 0.1371 8.0311 -0.2316 2.0103 -0.3788 0.8290 0.5259
3 0 6 0.1379 2.9750 0.2891 6.0469 -0.3528 0.0479 1.0206
-7 4 1 0.0348 -7.0468 3.8653 1.2422 -0.1831 -0.9969 -0.1090
-3 -7 -1 0.0952 -3.0092 -6.8624 -1.4633 0.9605 -0.0308 -0.0761
2 7 -2 0.1748 2.0245 7.2167 -1.5261 -0.8637 0.0448 -0.4331
-1 -7 3 0.1431 -1.0258 -7.3344 2.5241 0.8029 0.0268 0.6197
-1 2 5 0.1236 -1.0408 2.3988 5.1733 -0.3959 -0.4435 0.7116
-4 6 2 0.0937 -4.0371 5.7428 2.3765 -0.5622 -0.7736 0.0824
-4 6 -1 0.0880 -4.0162 6.0977 -0.6104 -0.5082 -0.6454 -0.4013
-7 -1 2 0.0974 -7.0533 -1.2379 1.9089 0.3803 -0.8472 0.1675
7 1 -3 0.1294 7.0602 1.3562 -2.9046 -0.3624 0.8900 -0.3288
0 6 -4 0.1456 0.0273 6.4551 -3.5879 -0.6257 -0.0599 -0.7833
3 -6 3 0.1303 2.9966 -6.3349 2.5994 0.5151 0.4456 0.6984
-2 6 4 0.1239 -2.0397 5.5075 4.3726 -0.6839 -0.6305 0.4557
3 7 2 0.1981 3.0023 6.7441 2.4589 -0.9785 -0.0119 0.2373
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             584
_exptl_absorpt_coefficient_mu    1.256
_exptl_absorpt_correction_T_min  0.748
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(1)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.2705
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4954
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0116
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         6.01
_diffrn_reflns_theta_max         62.39
_reflns_number_total             570
_reflns_number_gt                561
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro171.34.49, Oxford Diffraction'
_computing_cell_refinement       'CrysAlisPro171.34.49, Oxford Diffraction'
_computing_data_reduction        'CrysAlisPro171.34.49, Oxford Diffraction'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond, v.2.1e (Brandenburg, 2001)'
_computing_publication_material  ?

_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)+(0.0253P)²+0.2895P] where P=(Fo²+2Fc²)/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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(6)
_refine_ls_number_reflns         570
_refine_ls_number_parameters     53
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0175
_refine_ls_R_factor_gt           0.0170
_refine_ls_wR_factor_ref         0.0458
_refine_ls_wR_factor_gt          0.0454
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_restrained_S_all      1.113
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mg Mg 0.5000 0.5000 0.0000 0.01514(18) Uani 1 4 d S . .
O O 0.5000 0.5000 -0.22090(12) 0.0277(3) Uani 1 2 d S . .
H H 0.5457(14) 0.5319(16) -0.277(2) 0.060(6) Uiso 1 1 d . . .
B B 0.2500 0.21414(14) -0.1250 0.0179(4) Uani 1 2 d S . .
C1 C 0.34077(9) 0.29233(9) -0.05980(12) 0.0191(3) Uani 1 1 d . . .
N1 N 0.40239(8) 0.35461(8) -0.02013(10) 0.0203(2) Uani 1 1 d . . .
C2 C 0.19682(9) 0.14161(9) -0.00058(13) 0.0196(3) Uani 1 1 d . . .
N2 N 0.15599(9) 0.09277(9) 0.08903(11) 0.0279(3) Uani 1 1 d . . .

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
Mg 0.0156(2) 0.0156(2) 0.0143(3) 0.000 0.000 0.000
O 0.0286(7) 0.0381(7) 0.0164(5) 0.000 0.000 -0.0177(7)
B 0.0179(8) 0.0167(9) 0.0192(8) 0.000 0.0024(8) 0.000
C1 0.0201(6) 0.0194(6) 0.0177(5) 0.0033(5) 0.0052(5) 0.0037(5)
N1 0.0197(5) 0.0198(5) 0.0215(5) 0.0009(4) 0.0025(4) -0.0017(4)
C2 0.0181(5) 0.0198(5) 0.0207(5) -0.0037(6) -0.0015(5) -0.0007(4)
N2 0.0270(5) 0.0310(6) 0.0256(6) 0.0041(5) 0.0015(5) -0.0065(5)

_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
Mg O 2.0259(11) 6_655 ?
Mg O 2.0259(11) . ?
Mg N1 2.1737(10) 3_665 ?
Mg N1 2.1737(10) . ?
Mg N1 2.1737(10) 7_565 ?
Mg N1 2.1737(10) 6_655 ?
O H 0.859(19) . ?
B C2 1.5935(16) . ?
B C2 1.5935(16) 12_544 ?
B C1 1.5979(16) . ?
B C1 1.5979(16) 12_544 ?
C1 N1 1.1431(16) . ?
C2 N2 1.1381(16) . ?

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
O Mg O 180.0 6_655 . ?
O Mg N1 94.87(2) 6_655 3_665 ?
O Mg N1 85.13(2) . 3_665 ?
O Mg N1 94.87(2) 6_655 . ?
O Mg N1 85.13(2) . . ?
N1 Mg N1 170.26(5) 3_665 . ?
O Mg N1 85.13(2) 6_655 7_565 ?
O Mg N1 94.87(2) . 7_565 ?
N1 Mg N1 90.413(4) 3_665 7_565 ?
N1 Mg N1 90.413(4) . 7_565 ?
O Mg N1 85.13(2) 6_655 6_655 ?
O Mg N1 94.87(2) . 6_655 ?
N1 Mg N1 90.413(4) 3_665 6_655 ?
N1 Mg N1 90.413(4) . 6_655 ?
N1 Mg N1 170.26(5) 7_565 6_655 ?
Mg O H 126.7(12) . . ?
C2 B C2 111.48(13) . 12_544 ?
C2 B C1 111.27(6) . . ?
C2 B C1 108.58(5) 12_544 . ?
C2 B C1 108.58(5) . 12_544 ?
C2 B C1 111.27(6) 12_544 12_544 ?
C1 B C1 105.51(13) . 12_544 ?
N1 C1 B 174.52(12) . . ?
C1 N1 Mg 162.71(9) . . ?
N2 C2 B 177.42(12) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        61.40
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.075
_refine_diff_density_min         -0.103
_refine_diff_density_rms         0.022



_database_code_depnum_ccdc_archive 'CCDC 893430'
