Syntheses, Electronic Structures, and EPR/UV-Vis-NIR Spectroelectrochemistry of Nickel(II), Copper(II), and Zinc(II) Complexes with a Tetradentate Ligand Based on S-Methylisothiosemicarbazide
Vladimir B. Arion; Peter Rapta; Joshua Telser; Sergiu S. Shova; Martin Breza; Karol Lušpai; Jozef Kožišek; Inorganic Chemistry 50 (2011) 2918–2931; doi:10.1021/ic102277v

data_4324765
_publ_section_title
;
 Syntheses, Electronic Structures, and EPR/UV-Vis-NIR
 Spectroelectrochemistry of Nickel(II), Copper(II), and Zinc(II) Complexes
 with a Tetradentate Ligand Based on S-Methylisothiosemicarbazide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2918
_journal_page_last               2931
_journal_paper_doi               10.1021/ic102277v
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C23 H31 N3 Ni O3 S'
_chemical_formula_sum            'C23 H31 N3 Ni O3 S'
_chemical_formula_weight         488.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 109.426(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.3176(19)
_cell_length_b                   7.2509(3)
_cell_length_c                   21.5531(10)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.13
_cell_measurement_theta_min      2.31
_cell_volume                     4763.1(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1078
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            81756
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    0.931
_exptl_absorpt_correction_T_max  0.9637
_exptl_absorpt_correction_T_min  0.5230
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       plate
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.054
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         81929
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1160
_refine_ls_R_factor_gt           0.0669
_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^)+(0.0787P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1585
_refine_ls_wR_factor_ref         0.1792
_reflns_number_gt                52852
_reflns_number_total             81929
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102277v_si_002_2.cif
_cod_data_source_block           vlar024
_cod_database_code               4324765