A Solid-State Spectral Effect in Eclipsed Tetracyanonickelates: X-ray Crystal Structure, Polarized Specular Reflectance Spectroscopy, and ZINDO Modeling of Sr[Ni(CN)4].5H2O, Rb2[Ni(CN)4].H2O, and Na2[Ni(CN)4].3H2O
Frank R. Fronczek; Terry J. Delord; Steven F. Watkins; Petia Gueorguieva; George G. Stanley; Annegret S. Zizza; Jeffrey B. Cornelius; Yves A. Mantz; Ronald L. Musselman; Inorganic Chemistry 42 (2003) 7026–7036; doi:10.1021/ic0345222

data_4312410
_publ_section_title
;
 A Solid-State Spectral Effect in Eclipsed Tetracyanonickelates: X-ray
 Crystal Structure, Polarized Specular Reflectance Spectroscopy, and ZINDO
 Modeling of Sr[Ni(CN)4].5H2O, Rb2[Ni(CN)4].H2O, and Na2[Ni(CN)4].3H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7026
_journal_page_last               7036
_journal_paper_doi               10.1021/ic0345222
_journal_volume                  42
_journal_year                    2003
_chemical_compound_source        'local laboratory'
_chemical_formula_moiety         '2(Na 1+), C4 N4 Ni 2-, 3(H2 O)'
_chemical_formula_sum            'C4 H6 N4 Na2 Ni O3'
_chemical_formula_weight         262.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.311(5)
_cell_angle_beta                 87.326(5)
_cell_angle_gamma                83.772(6)
_cell_formula_units_Z            4
_cell_length_a                   7.2980(10)
_cell_length_b                   8.8620(10)
_cell_length_c                   15.132(2)
_cell_measurement_reflns_used    8200
_cell_measurement_temperature    100
_cell_measurement_theta_max      35.0
_cell_measurement_theta_min      2.5
_cell_volume                     971.8(2)
_computing_cell_refinement
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius 1999)'
_computing_data_reduction
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'Direct_methods (SIR, Altomare, et al., 1994)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device       'KappaCCD (with Oxford Cryostream)'
_diffrn_measurement_method       ' \w scans with \k offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.018
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            34807
_diffrn_reflns_theta_full        35.0
_diffrn_reflns_theta_max         35.0
_diffrn_reflns_theta_min         2.6
_diffrn_standards_decay_%        <2
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.069
_exptl_absorpt_correction_T_max  0.813
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.74
_refine_diff_density_min         -0.73
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.0409(10)
_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   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         8269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.030
_refine_ls_R_factor_gt           0.024
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+0.2613P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.061
_refine_ls_wR_factor_ref         0.064
_reflns_number_gt                7223
_reflns_number_total             8269
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic0345222si20030515_022929.cif
_cod_data_source_block           NaNiCN
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4312410