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_4324768
_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'
_chemical_formula_sum            'C23 H31 Cu N3 O3'
_chemical_formula_weight         461.05
_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                 93.060(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   34.687(3)
_cell_length_b                   13.8621(11)
_cell_length_c                   9.5329(6)
_cell_measurement_reflns_used    2959
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.92
_cell_measurement_theta_min      2.35
_cell_volume                     4577.2(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1356
_diffrn_reflns_av_sigmaI/netI    0.0783
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            48431
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    0.982
_exptl_absorpt_correction_T_max  0.9711
_exptl_absorpt_correction_T_min  0.8129
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       plate
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.399
_refine_diff_density_min         -1.000
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4202
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1079
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0731P)^2^+27.5482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1394
_refine_ls_wR_factor_ref         0.1668
_reflns_number_gt                2761
_reflns_number_total             4202
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102277v_si_002_5.cif
_cod_data_source_block           vlar032
_cod_database_code               4324768