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_4324764
_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 Cu N3 O3 S'
_chemical_formula_sum            'C23 H31 Cu N3 O3 S'
_chemical_formula_weight         493.11
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m 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                   31.637(6)
_cell_length_b                   6.9058(14)
_cell_length_c                   10.956(2)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.70
_cell_measurement_theta_min      2.68
_cell_volume                     2393.7(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0762
_diffrn_reflns_av_sigmaI/netI    0.0283
_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       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            57330
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    1.028
_exptl_absorpt_correction_T_max  0.8953
_exptl_absorpt_correction_T_min  0.4935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       plate
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         2546
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0383P)^2^+4.1846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0967
_reflns_number_gt                2104
_reflns_number_total             2546
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102277v_si_002_1.cif
_cod_data_source_block           VLAR023
_cod_original_cell_volume        2393.6(8)
_cod_database_code               4324764