Novel Thiosalamo Ligand as a Remarkably Stable N2S2 Salen-Type Chelate and Synthesis of a Nickel(II) Complex
Shigehisa Akine; Tatsuya Nabeshima; Inorganic Chemistry 44 (2005) 1205–1207; doi:10.1021/ic048347g

data_4308643
_publ_contact_author_address
;
Tsukuba, Ibaraki 305-8571, Japan
;
_publ_contact_author_email       nabesima@chem.tsukuba.ac.jp
_publ_contact_author_fax         +81-29-853-4507
_publ_contact_author_name        'Tatsuya Nabeshima'
_publ_contact_author_phone       +81-29-853-4507
_publ_section_title
;
Novel Thiosalamo Ligand as a Remarkably Stable N2S2 Salen-Type Chelate and
Synthesis of a Nickel(II) Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1205
_journal_page_last               1207
_journal_paper_doi               10.1021/ic048347g
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         C42H52N4Ni3O15
_chemical_formula_sum            'C42 H52 N4 Ni3 O15'
_chemical_formula_weight         1029.01
_chemical_name_common            '[Ni3salamo2(OAc)2(EtOH)2]'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.042(6)
_cell_angle_beta                 83.680(6)
_cell_angle_gamma                78.832(3)
_cell_formula_units_Z            2
_cell_length_a                   10.7606(17)
_cell_length_b                   12.4817(18)
_cell_length_c                   16.8606(19)
_cell_measurement_reflns_used    14041
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      2.17
_cell_volume                     2208.1(5)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  ORTEP-3
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Rigaku Mercury CCD diffractometer'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_sigmaI/netI    0.0991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14041
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.340
_exptl_absorpt_correction_T_max  0.8777
_exptl_absorpt_correction_T_min  0.6163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Corp., 2000)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.012
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         7534
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0551
_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^)+(0.0552P)^2^+1.9773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1335
_reflns_number_gt                5004
_reflns_number_total             7534
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048347gsi20041122_032645_3.cif
_cod_data_source_block           salamoNi
_cod_database_code               4308643