Tetraethylammonium tris(thiocyanato-κ<i>N</i>)[tris(1<i>H</i>-pyrazol-1-yl-κ<i>N</i>^2^)methane]nickelate(II)
Lyubartseva, Ganna; Parkin, Sean; Mallik, Uma Prasad; Jeon, Hee Kyung; Acta Crystallographica Section E 68 (2012) m888–; doi:10.1107/S1600536812024774

data_2235646
_publ_section_title
;
 Tetraethylammonium
 tris(thiocyanato-\k<i>N</i>)[tris(1<i>H</i>-pyrazol-1-yl-\k<i>N</i>^2^)methane]nickelate(II)
;
_journal_coeditor_code           TK5107
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m888
_journal_paper_doi               10.1107/S1600536812024774
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '(C8 H20 N) [Ni (N C S)3 (C10 H10 N6)]'
_chemical_formula_moiety         'C8 H20 N +, C13 H10 N9 Ni S3 -'
_chemical_formula_sum            'C21 H30 N10 Ni S3'
_chemical_formula_weight         577.44
_chemical_name_systematic
;
Tetraethylammonium tris(thiocyanato-\k<i>N</i>)[tris(1<i>H</i>-pyrazol-1-yl-
\k<i>N</i>^2^)methane]nickelate(II)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.592(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.7117(12)
_cell_length_b                   7.4378(3)
_cell_length_c                   24.7885(9)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      68.10
_cell_measurement_theta_min      2.98
_cell_volume                     5473.2(4)
_computing_cell_refinement       'APEX2 (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'APEX2 (Bruker, 2006)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and local procedures'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 0.847
_diffrn_measured_fraction_theta_max 0.847
_diffrn_measurement_device_type  'Bruker X8 Proteum'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'graded multilayer optics'
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_sigmaI/netI    0.0829
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            17387
_diffrn_reflns_theta_full        68.54
_diffrn_reflns_theta_max         68.54
_diffrn_reflns_theta_min         2.98
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.407
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2006)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.511
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         17387
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0544
_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^)+(0.1128P)^2^+8.5319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1818
_refine_ls_wR_factor_ref         0.1862
_reflns_number_gt                16112
_reflns_number_total             17387
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk5107.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2235646
_cod_database_fobs_code          2235646