Crystal structures and electrochemical properties of nickel(II) complexes with <i>N</i>,<i>N</i>',<i>N</i>'',<i>S</i>-tetradentate Schiff base ligands
Hirotsu, Masakazu; Sanou, Junhei; Nakae, Toyotaka; Matsunaga, Takumi; Kinoshita, Isamu; Acta Crystallographica Section E 78 (2022) –; doi:10.1107/S2056989022003954

data_2244074
_publ_section_title
;
 Crystal structures and electrochemical properties of nickel(II) complexes
 with <i>N</i>,<i>N</i>',<i>N</i>'',<i>S</i>-tetradentate Schiff base
 ligands
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989022003954
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          '[Ni (C13 H18 N3 S)] P F6, C H2 Cl2'
_chemical_formula_moiety         'C13 H18 N3 Ni S +, F6 P -, C H2 Cl2'
_chemical_formula_sum            'C14 H20 Cl2 F6 N3 Ni P S'
_chemical_formula_weight         536.97
_chemical_name_systematic
;[2-({[2-(Piperazin-1-yl-\k^2^<i>N</i>^1^,<i>N</i>^4^)ethyl]imino-\k<i>N</i>}methyl)benzenethiolato-\k<i>S</i>]nickel(II) hexafluorophosphate
dichloromethane monosolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                98.065(4)
_cell_angle_beta                 101.274(6)
_cell_angle_gamma                96.150(5)
_cell_formula_units_Z            2
_cell_length_a                   8.725(3)
_cell_length_b                   10.507(4)
_cell_length_c                   11.316(4)
_cell_measurement_reflns_used    3095
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.4739
_cell_measurement_theta_min      3.3178
_cell_volume                     997.6(6)
_computing_cell_refinement
;
CrystalClear (Rigaku, 2008)
;
_computing_data_collection
;
CrystalClear (Rigaku, 2008)
;
_computing_data_reduction
;
CrystalClear (Rigaku, 2008)
;
_computing_molecular_graphics
;
Ortep-3 for Windows (Farrugia, 2012), Mercury (Macrae <i>et al.</i>,
2020)
;
_computing_publication_material
;
WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR97 (Altomare <i>et al.</i>,  1999)
;
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Rigaku AFC11 with Saturn 724+ CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0700
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8155
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         27.455
_diffrn_reflns_theta_min         3.318
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    1.485
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8275
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>REQAB</i>; Rigaku, 1998)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_description       Prism
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.521
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         4392
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.930
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0389P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0871
_reflns_number_gt                3240
_reflns_number_total             4392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            dj2045sup1.cif
_cod_data_source_block           2
_cod_database_code               2244074
_shelx_estimated_absorpt_t_min   0.786
_shelx_estimated_absorpt_t_max   0.890
_shelx_hkl_checksum              13507
_shelx_res_checksum              20294
_shelxl_version_number           .2013
_cod_database_fobs_code 2244074