Wheel-Shaped Icosanuclear Homo- and Heterometallic Complexes of NiII, CoII, and CuII Ions Supported by Unsymmetrical Aminoalcohol Ligands
Takayuki Nakajima; Keiko Seto; Fumihiro Horikawa; Isao Shimizu; Andreas Scheurer; Bunsho Kure; Takashi Kajiwara; Tomoaki Tanase; Masahiro Mikuriya; Inorganic Chemistry 51 (2012) 12503–12510; doi:10.1021/ic3019106

data_4331096
_publ_section_title
;
 Wheel-Shaped Icosanuclear Homo- and Heterometallic Complexes of NiII,
 CoII, and CuII Ions Supported by Unsymmetrical Aminoalcohol Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12503
_journal_page_last               12510
_journal_paper_doi               10.1021/ic3019106
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C180 H282 N14 Ni20 O76'
_chemical_formula_sum            'C180 H282 N14 Ni20 O76'
_chemical_formula_weight         5032.26
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      86
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   22.6978(6)
_cell_length_b                   22.6978(6)
_cell_length_c                   22.9284(8)
_cell_measurement_reflns_used    24761
_cell_measurement_temperature    163
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.10
_cell_volume                     11812.5(6)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_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      163
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            109700
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.632
_exptl_absorpt_correction_T_max  0.721
_exptl_absorpt_correction_T_min  0.635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            lime
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       block
_exptl_crystal_F_000             5256.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_platon_squeeze_details
;
;
_refine_diff_density_max         1.430
_refine_diff_density_min         -0.660
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     660
_refine_ls_number_reflns         13418
_refine_ls_number_restraints     5
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0742P)^2^+17.4662P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1456
_reflns_number_gt                11047
_reflns_number_total             13418
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic3019106_si_002_2.cif
_cod_data_source_block           Ni20(1)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               4331096