Color Properties and Structural Phase Transition in Penta- And Hexacoordinate Isothiocyanato Ni(II) Compounds
T. V. Brinzari; C. Tian; G. J. Halder; J. L. Musfeldt; M.-H. Whangbo; J. A. Schlueter; Inorganic Chemistry 48 (2009) 7650–7658; doi:10.1021/ic802120n

data_4302892
_publ_contact_author_address
;
Materials Science Division
Argonne National Laboratory
Argonne, IL 60439-4831, USA
;
_publ_contact_author_email       JASchlueter@anl.gov
_publ_contact_author_fax         '(630) 252-9151'
_publ_contact_author_name        'Dr. John Schlueter'
_publ_contact_author_phone       '(630) 252-3588'
_publ_section_title
;
Color Properties and Structural Phase Transition in Penta- And
Hexacoordinate Isothiocyanato Ni(II) Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7650
_journal_page_last               7658
_journal_paper_doi               10.1021/ic802120n
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         '4(C8 H20 N 1+), C6 N6 Ni S6 4-'
_chemical_formula_sum            'C38 H80 N10 Ni S6'
_chemical_formula_weight         928.19
_chemical_melting_point          449
_chemical_name_common
; 
Tetrabutylammonium hexathiocyanato nickalate(II) 
;
_chemical_name_systematic
; 
Tetraethylammonium hexathiocyanato nickalate(II) 
;
_space_group_IT_number           64
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      64
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual editing of SHELXL-97 cif file'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   18.973(2)
_cell_length_b                   21.050(3)
_cell_length_c                   38.715(5)
_cell_measurement_reflns_used    2026
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.127
_cell_measurement_theta_min      2.860
_cell_volume                     15462(3)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Siemens, 1997-1998)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2001)'
_computing_publication_material
;
SHELXTL (Sheldrick, 2001), PLATON (Spek, 2003)
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 2001)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       'area detector \w scans'
_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  0.0582
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            40067
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.05
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  0.851
_exptl_absorpt_correction_T_min  0.754
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(Sheldrick, 2001)
;
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6024
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.00029(4)
_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   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         8167
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0668P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1472
_refine_ls_wR_factor_ref         0.1721
_reflns_number_gt                4783
_reflns_number_total             8167
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802120n_si_002_3.cif
_cod_data_source_block           TEANiNCS_RT
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               4302892