#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:55:46 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178924 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/53/4115332.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4115332
loop_
_publ_author_name
'Christoph Janiak'
'Tobias G. Scharmann'
'Sax A. Mason'
_publ_section_title
;
 Two-Dimensional Water and Ice Layers: Neutron Diffraction Studies at 278,
 263, and 20 K
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14010
_journal_page_last               14011
_journal_paper_doi               10.1021/ja0274608
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety         'Ni[HB(C2H2N3)3]2, 6D2O'
_chemical_formula_sum            'C12 H14 B2 D12 N18 Ni O6'
_chemical_formula_weight         610.77
_chemical_name_common            NiN33.6D2O
_chemical_name_systematic
; 
bis(hydrotris(1,2,4-triazolyl)borato)nickel(II)-
hexakis(deuterium oxide) 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2bc 2a'
_symmetry_space_group_name_H-M   'P m n b'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.995(8)
_cell_angle_beta                 90.000(10)
_cell_angle_gamma                89.998(8)
_cell_formula_units_Z            4
_cell_length_a                   10.8517(17)
_cell_length_b                   20.919(3)
_cell_length_c                   11.6959(13)
_cell_measurement_temperature    263(2)
_cell_volume                     2655.0(6)
_computing_cell_refinement       'ILL program Rafd19'
_computing_data_collection       'ILL programs Hklgen and Mad'
_computing_data_reduction        'Retreat   (Wilkinson et al, 1988)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      263(2)
_diffrn_measurement_device_type  'thermal beam instrument D19 at ILL'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  germanium
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'neutron reactor'
_diffrn_radiation_type           neutrons
_diffrn_radiation_wavelength     1.31430
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            3266
_diffrn_reflns_theta_max         50.00
_diffrn_reflns_theta_min         3.60
_exptl_absorpt_coefficient_mu    2.78
_exptl_absorpt_correction_T_max  0.6931
_exptl_absorpt_correction_T_min  0.4876
_exptl_absorpt_correction_type   'crystal dimensions; D19abs'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1327
_exptl_crystal_size_max          4.10
_exptl_crystal_size_mid          3.80
_exptl_crystal_size_min          2.00
_refine_diff_density_max         0.774
_refine_diff_density_min         -0.921
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       0.00125(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.278
_refine_ls_hydrogen_treatment    full
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         2048
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.294
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0345P)²+17.2856P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1194
_reflns_number_gt                1648
_reflns_number_total             2048
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0274608-4_s1_2.cif
_cod_data_source_block           263neu
_cod_database_code               4115332
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'x+1/2, -y, -z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'-x-1/2, y, z'
'x-1/2, -y-1/2, z-1/2'
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
Ni Ni 0.2500 0.25382(9) -0.00172(19) 0.0257(5) Uani 1 2 d S
B1 B 0.2500 0.36807(18) 0.1792(3) 0.0277(10) Uani 1 2 d S
H1 H 0.2500 0.4107(3) 0.2480(6) 0.051(2) Uani 1 2 d S
N11 N 0.2500 0.30181(11) 0.2386(2) 0.0301(6) Uani 1 2 d S
N12 N 0.2500 0.24692(11) 0.1756(2) 0.0308(6) Uani 1 2 d S
C11 C 0.2500 0.20040(16) 0.2517(3) 0.0343(9) Uani 1 2 d S
H11 H 0.2500 0.1504(4) 0.2267(7) 0.057(2) Uani 1 2 d S
N13 N 0.2500 0.22158(13) 0.3609(2) 0.0410(7) Uani 1 2 d S
C12 C 0.2500 0.28510(18) 0.3490(3) 0.0350(9) Uani 1 2 d S
H12 H 0.2500 0.3185(5) 0.4177(8) 0.071(3) Uani 1 2 d S
N14 N 0.13565(19) 0.37089(7) 0.10112(14) 0.0311(5) Uani 1 1 d .
N15 N 0.11764(19) 0.32538(8) 0.01938(15) 0.0314(5) Uani 1 1 d .
C13 C 0.0146(3) 0.34309(13) -0.0328(3) 0.0402(7) Uani 1 1 d .
H13 H -0.0249(7) 0.3163(3) -0.1019(7) 0.0704(19) Uani 1 1 d .
N16 N -0.0344(2) 0.39712(10) 0.0106(2) 0.0480(6) Uani 1 1 d .
C14 C 0.0441(3) 0.41299(12) 0.0933(2) 0.0387(7) Uani 1 1 d .
H14 H 0.0373(8) 0.4551(3) 0.1467(7) 0.079(2) Uani 1 1 d .
B2 B 0.2500 0.1393(2) -0.1840(4) 0.0441(14) Uani 1 2 d S
H2 H 0.2500 0.0960(4) -0.2517(8) 0.076(3) Uani 1 2 d S
N21 N 0.2500 0.20504(12) -0.2424(2) 0.0434(8) Uani 1 2 d S
N22 N 0.2500 0.26009(12) -0.1794(2) 0.0376(7) Uani 1 2 d S
C21 C 0.2500 0.30634(17) -0.2556(3) 0.0383(9) Uani 1 2 d S
H21 H 0.2500 0.3561(4) -0.2306(7) 0.064(3) Uani 1 2 d S
N23 N 0.2500 0.28483(14) -0.3649(2) 0.0475(8) Uani 1 2 d S
C22 C 0.2500 0.22127(19) -0.3529(3) 0.0441(10) Uani 1 2 d S
H22 H 0.2500 0.1876(6) -0.4208(9) 0.085(3) Uani 1 2 d S
N24 N 0.1357(2) 0.13634(8) -0.10422(16) 0.0435(6) Uani 1 1 d .
N25 N 0.1182(2) 0.18156(8) -0.02233(16) 0.0370(5) Uani 1 1 d .
C23 C 0.0171(3) 0.16358(14) 0.0301(3) 0.0501(8) Uani 1 1 d .
H23 H -0.0226(8) 0.1903(4) 0.0997(8) 0.082(2) Uani 1 1 d .
N26 N -0.0327(3) 0.10956(11) -0.0122(3) 0.0681(8) Uani 1 1 d .
C24 C 0.0450(4) 0.09392(14) -0.0957(3) 0.0589(10) Uani 1 1 d .
H24 H 0.0396(11) 0.0520(4) -0.1509(9) 0.106(3) Uani 1 1 d .
O1 O 0.2500 -0.0325(4) -1.0121(8) 0.078(2) Uani 1 2 d SU
D11 D 0.1817(6) -0.0610(2) -1.0050(5) 0.0952(15) Uani 1 1 d U
O2 O 0.3097(15) 0.0492(5) -0.8244(13) 0.101(4) Uani 0.50 1 d PU
D21 D 0.2500 0.0224(5) -0.8805(12) 0.148(4) Uani 1 2 d SU
D22 D 0.2500 0.0383(4) -0.7494(14) 0.157(5) Uani 1 2 d SU
O3 O 0.2500 0.0366(3) -0.5694(6) 0.0559(15) Uani 1 2 d SU
D31 D 0.1791(4) 0.06124(19) -0.5444(4) 0.0720(11) Uani 1 1 d U
O4 O 0.2500 -0.0493(4) -0.3717(11) 0.103(4) Uani 1 2 d SU
D41 D 0.2500 -0.0215(4) -0.4401(8) 0.094(2) Uani 1 2 d SU
D42 D 0.165(3) -0.0406(6) -0.3252(14) 0.158(9) Uani 0.50 1 d PU
O5 O 0.457(2) -0.0390(5) -0.2431(13) 0.177(8) Uani 1 1 d U
D51 D 0.510(3) -0.0535(8) -0.237(3) 0.35(2) Uani 1 1 d U
D52 D 0.422(2) -0.0498(7) -0.1726(15) 0.262(11) Uani 1 1 d U
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
N12 Ni N22 179.63(14) . .
N12 Ni N15 86.09(10) . .
N22 Ni N15 94.18(10) . .
N12 Ni N15 86.09(10) . 7_655
N22 Ni N15 94.18(10) . 7_655
N15 Ni N15 86.86(12) . 7_655
N12 Ni N25 93.71(10) . 7_655
N22 Ni N25 86.02(10) . 7_655
N15 Ni N25 179.56(12) . 7_655
N15 Ni N25 93.52(7) 7_655 7_655
N12 Ni N25 93.71(10) . .
N22 Ni N25 86.02(10) . .
N15 Ni N25 93.52(7) . .
N15 Ni N25 179.56(13) 7_655 .
N25 Ni N25 86.10(13) 7_655 .
N14 B1 N14 107.2(3) . 7_655
N14 B1 N11 107.43(18) . .
N14 B1 N11 107.43(18) 7_655 .
N14 B1 H1 111.6(3) . .
N14 B1 H1 111.6(3) 7_655 .
N11 B1 H1 111.3(5) . .
C12 N11 N12 107.5(2) . .
C12 N11 B1 131.8(3) . .
N12 N11 B1 120.7(2) . .
C11 N12 N11 104.9(2) . .
C11 N12 Ni 136.4(2) . .
N11 N12 Ni 118.71(18) . .
N12 C11 N13 113.3(3) . .
N12 C11 H11 121.9(5) . .
N13 C11 H11 124.8(5) . .
C12 N13 C11 103.2(3) . .
N13 C12 N11 111.1(3) . .
N13 C12 H12 125.0(6) . .
N11 C12 H12 123.9(6) . .
C14 N14 N15 107.9(2) . .
C14 N14 B1 131.8(2) . .
N15 N14 B1 120.3(2) . .
C13 N15 N14 104.37(19) . .
C13 N15 Ni 136.49(17) . .
N14 N15 Ni 118.99(15) . .
N15 C13 N16 113.2(2) . .
N15 C13 H13 122.5(5) . .
N16 C13 H13 124.3(5) . .
C14 N16 C13 103.3(2) . .
N14 C14 N16 111.2(2) . .
N14 C14 H14 123.4(5) . .
N16 C14 H14 125.4(5) . .
N21 B2 N24 107.6(2) . 7_655
N21 B2 N24 107.6(2) . .
N24 B2 N24 105.9(3) 7_655 .
N21 B2 H2 112.5(6) . .
N24 B2 H2 111.5(3) 7_655 .
N24 B2 H2 111.5(3) . .
C22 N21 N22 107.9(3) . .
C22 N21 B2 131.1(3) . .
N22 N21 B2 121.0(3) . .
C21 N22 N21 104.8(3) . .
C21 N22 Ni 136.3(2) . .
N21 N22 Ni 118.99(19) . .
N22 C21 N23 113.2(3) . .
N22 C21 H21 121.7(6) . .
N23 C21 H21 125.1(6) . .
C22 N23 C21 103.4(3) . .
N21 C22 N23 110.7(3) . .
N21 C22 H22 123.7(7) . .
N23 C22 H22 125.6(7) . .
C24 N24 N25 107.9(3) . .
C24 N24 B2 131.5(3) . .
N25 N24 B2 120.5(2) . .
C23 N25 N24 104.3(2) . .
C23 N25 Ni 136.39(19) . .
N24 N25 Ni 119.20(17) . .
N25 C23 N26 113.9(3) . .
N25 C23 H23 122.6(5) . .
N26 C23 H23 123.5(5) . .
C24 N26 C23 102.8(3) . .
N24 C24 N26 111.1(3) . .
N24 C24 H24 122.1(7) . .
N26 C24 H24 126.8(7) . .
D11 O1 D11 101.9(10) 7_655 .
D21 O2 D22 91.3(14) . .
D21 O2 O2 53.1(8) . 7_655
D22 O2 O2 54.4(10) . 7_655
O2 D21 O2 73.9(16) 7_655 .
O2 D22 O2 71(2) 7_655 .
D31 O3 D31 104.7(8) . 7_655
D41 O4 D42 107.9(9) . .
D41 O4 D42 107.9(9) . 7_655
D42 O4 D42 116(2) . 7_655
D51 O5 D52 99(4) . .
O5 D51 D52 49(3) . .
O5 D52 D51 32(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni N12 2.079(3) .
Ni N22 2.082(3) .
Ni N15 2.089(2) .
Ni N15 2.089(2) 7_655
Ni N25 2.095(2) 7_655
Ni N25 2.095(2) .
B1 N14 1.542(3) .
B1 N14 1.542(3) 7_655
B1 N11 1.550(5) .
B1 H1 1.201(7) .
N11 C12 1.338(4) .
N11 N12 1.364(3) .
N12 C11 1.319(4) .
C11 N13 1.352(4) .
C11 H11 1.086(8) .
N13 C12 1.336(5) .
C12 H12 1.064(11) .
N14 C14 1.331(3) .
N14 N15 1.363(2) .
N15 C13 1.326(4) .
C13 N16 1.348(4) .
C13 H13 1.074(8) .
N16 C14 1.332(4) .
C14 H14 1.081(8) .
B2 N21 1.535(5) .
B2 N24 1.553(4) 7_655
B2 N24 1.553(4) .
B2 H2 1.203(8) .
N21 C22 1.337(5) .
N21 N22 1.367(4) .
N22 C21 1.315(5) .
C21 N23 1.355(5) .
C21 H21 1.081(8) .
N23 C22 1.337(5) .
C22 H22 1.061(12) .
N24 C24 1.330(4) .
N24 N25 1.360(3) .
N25 C23 1.313(4) .
C23 N26 1.347(4) .
C23 H23 1.078(10) .
N26 C24 1.331(5) .
C24 H24 1.090(9) .
O1 D11 0.954(6) 7_655
O1 D11 0.954(6) .
O2 D21 1.079(15) .
O2 D22 1.114(14) .
O2 O2 1.30(3) 7_655
D21 O2 1.079(15) 7_655
D22 O2 1.114(14) 7_655
O3 D31 0.971(5) .
O3 D31 0.971(5) 7_655
O4 D41 0.989(11) .
O4 D42 1.09(3) .
O4 D42 1.09(3) 7_655
O5 D51 0.66(4) .
O5 D52 0.934(19) .
D51 D52 1.22(4) .
