Syntheses, Structures and Magnetic Properties of Tetranuclear Cubane-type and Heptanuclear Wheel-type Nickel(II) Complexes with 3-Methoxysalicylic Acid Derivatives
Kobayashi, Fumiya; Ohtani, Ryo; Teraoka, Saki; Kosaka, Wataru; Miyasaka, Hitoshi; Zhang, Yingjie; Lindoy, Leonard F.; Hayami, Shinya; Nakamura, Masaaki; Dalton Trans.  (2017) –; doi:10.1039/C7DT01757J

data_7043237
_publ_section_title
;
 Syntheses, Structures and Magnetic Properties of Tetranuclear Cubane-type
 and Heptanuclear Wheel-type Nickel(II) Complexes with 3-Methoxysalicylic
 Acid Derivatives
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01757J
_journal_year                    2017
_chemical_formula_moiety         'C16 H15 N3 Ni O5'
_chemical_formula_sum            'C16 H15 N3 Ni O5'
_chemical_formula_weight         388.01
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2017-06-04 deposited with the CCDC.
2017-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 95.5363(8)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   6.85643(16)
_cell_length_b                   15.3741(4)
_cell_length_c                   14.9966(4)
_cell_measurement_reflns_used    17210
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.04
_cell_volume                     1573.44(7)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0729
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25006
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.267
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             800.00
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.790
_refine_diff_density_min         -0.400
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3592
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0435P)^2^+1.8335P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0973
_reflns_number_gt                3229
_reflns_number_total             3592
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c7dt01757j2.cif
_cod_data_source_block           Ni_mononuclear
_cod_original_cell_volume        1573.43(7)
_cod_database_code               7043237