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_4115333
_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_compound_source        'Chem. Ber. 1994, 127, 1379'
_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           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P -2bc 2a'
_symmetry_space_group_name_H-M   'P 21 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                90.000(6)
_cell_angle_beta                 90.000(6)
_cell_angle_gamma                90.000(6)
_cell_formula_units_Z            4
_cell_length_a                   10.7548(10)
_cell_length_b                   20.7363(15)
_cell_length_c                   11.587(2)
_cell_measurement_temperature    20(2)
_cell_volume                     2584.1(5)
_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-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      20(2)
_diffrn_measurement_device       '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  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4439
_diffrn_reflns_theta_max         55.76
_diffrn_reflns_theta_min         3.63
_exptl_absorpt_coefficient_mu    2.78
_exptl_absorpt_correction_T_max  0.6931
_exptl_absorpt_correction_T_min  0.4865
_exptl_absorpt_correction_type   'crystal dimensions; D19abs'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.570
_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         0.567
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.155
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_coef       0.00045(3)
_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_all   1.155
_refine_ls_hydrogen_treatment    full
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         2881
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_obs          0.0285
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0158P)^2^+24.5447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0669
_refine_ls_wR_factor_obs         0.0667
_reflns_number_observed          2861
_reflns_number_total             2881
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja0274608-4_s1_3.cif
_cod_data_source_block           20neu
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0158P)^2^+24.5447P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0158P)^2^+24.5447P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2584.0(5)
_cod_database_code               4115333