Oligometallic Template Strategy for Synthesis of a Macrocyclic Dimer-Type Octaoxime Ligand for Its Cooperative Complexation
Shigehisa Akine; Toshio Tadokoro; Tatsuya Nabeshima; Inorganic Chemistry 51 (2012) 11478–11486; doi:10.1021/ic3012525

data_4330831
_publ_contact_author_address
;
Tsukuba, Ibaraki 305-8571, Japan
;
_publ_contact_author_email       akine@chem.tsukuba.ac.jp
_publ_contact_author_fax         +81-29-853-4527
_publ_contact_author_name        'Shigehisa Akine'
_publ_contact_author_phone       +81-29-853-4527
_publ_section_title
;
 Oligometallic Template Strategy for Synthesis of a Macrocyclic Dimer-Type
 Octaoxime Ligand for Its Cooperative Complexation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11478
_journal_page_last               11486
_journal_paper_doi               10.1021/ic3012525
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C38 H42 N4 O15 Zn3, C4 H10 O, C H Cl3'
_chemical_formula_sum            'C43 H53 Cl3 N4 O16 Zn3'
_chemical_formula_weight         1184.35
_chemical_name_common            '[LZn3(OAc)2(H2O)](CHCl3)(Et2O)'
_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                64.5631(14)
_cell_angle_beta                 68.8301(16)
_cell_angle_gamma                84.4374(18)
_cell_formula_units_Z            2
_cell_length_a                   13.6167(8)
_cell_length_b                   14.4293(8)
_cell_length_c                   14.9773(8)
_cell_measurement_reflns_used    21600
_cell_measurement_temperature    120
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      3.04
_cell_volume                     2472.2(2)
_computing_cell_refinement       'Rapid AUTO (Rigaku Corp.)'
_computing_data_collection       'Rapid AUTO (Rigaku Corp.)'
_computing_data_reduction        'Rapid AUTO (Rigaku Corp.)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  ORTEP-3
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF99 (Beurskens et al., 1999)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS Rapid'
_diffrn_measurement_method       IP
_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  0.0773
_diffrn_reflns_av_sigmaI/netI    0.1029
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21600
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.04
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.678
_exptl_absorpt_correction_T_max  0.7302
_exptl_absorpt_correction_T_min  0.6791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Rapid AUTO (Rigaku Corp.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.245
_refine_diff_density_min         -0.973
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         9688
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0615
_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^)+(0.0691P)^2^+2.8926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1690
_reflns_number_gt                6998
_reflns_number_total             9688
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3012525_si_001_2.cif
_cod_data_source_block           LZn3
_cod_database_code               4330831