Two-Dimensional Water and Ice Layers: Neutron Diffraction Studies at 278, 263, and 20 K
Christoph Janiak; Tobias G. Scharmann; Sax A. Mason; Journal of the American Chemical Society 124 (2002) 14010–14011; doi:10.1021/ja0274608

data_4115332
_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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.0345P)^2^+17.2856P] where P=(Fo^2^+2Fc^2^)/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