Crystal structure of tetraaquabis(thiocyanato-κ<i>N</i>)nickel(II)–2,5-dimethylpyrazine (1/4)
Suckert, Stefan; Wriedt, Mario; Jess, Inke; Näther, Christian; Acta Crystallographica Section E 71 (2015) m18–; doi:10.1107/S2056989014026991

data_2240362
_publ_section_title
;
 Crystal structure of
 tetraaquabis(thiocyanato-\k<i>N</i>)nickel(II)--2,5-dimethylpyrazine
 (1/4)
;
_journal_coeditor_code           PK2540
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m18
_journal_paper_doi               10.1107/S2056989014026991
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Ni (N C S)2 (H2 O)4], 4C6 H8 N2'
_chemical_formula_moiety         'C2 H8 N2 Ni O4 S2, 4(C6 H8 N2)'
_chemical_formula_sum            'C26 H40 N10 Ni O4 S2'
_chemical_formula_weight         679.51
_chemical_name_systematic
;
Tetraaquabis(thiocyanato-\k<i>N</i>)nickel(II)--2,5-dimethylpyrazine (1/4)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0731(6)
_cell_length_b                   14.7989(8)
_cell_length_c                   17.3092(11)
_cell_measurement_reflns_used    21266
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      28.09
_cell_measurement_theta_min      2.82
_cell_volume                     3348.8(3)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2008)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2008)
;
_computing_data_reduction
;
X-AREA (Stoe & Cie, 2008)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Stoe IPDS-1'
_diffrn_measurement_method       '\f 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  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21266
_diffrn_reflns_theta_full        28.09
_diffrn_reflns_theta_max         28.09
_diffrn_reflns_theta_min         2.82
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.751
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(X-SHAPE and X-RED32; Stoe & Cie, 2008)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.400
_refine_ls_extinction_coef       0.0068(8)
_refine_ls_extinction_expression Fc*=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL97 (Sheldrick, 2008)
;
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         4041
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0627P)^2^+0.7837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.1001
_reflns_number_gt                3146
_reflns_number_total             4041
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pk2540sup1.cf
_cod_data_source_block           I
_cod_database_code               2240362
_cod_database_fobs_code          2240362