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_4330833
_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 H40 Ca N4 O14 Zn2, C H4 O'
_chemical_formula_sum            'C39 H44 Ca N4 O15 Zn2'
_chemical_formula_weight         979.60
_chemical_name_common            '[LZn2Ca(OAc)2](MeOH)'
_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                61.5710(10)
_cell_angle_beta                 64.4047(14)
_cell_angle_gamma                73.0515(13)
_cell_formula_units_Z            2
_cell_length_a                   12.3350(5)
_cell_length_b                   14.4580(5)
_cell_length_c                   14.8059(6)
_cell_measurement_reflns_used    19801
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      3.06
_cell_volume                     2081.88(14)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19801
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.350
_exptl_absorpt_correction_T_max  0.8232
_exptl_absorpt_correction_T_min  0.5517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Rapid AUTO (Rigaku Corp.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         9028
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0283
_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^)+(0.0312P)^2^+1.2768P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0744
_reflns_number_gt                7961
_reflns_number_total             9028
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3012525_si_001_4.cif
_cod_data_source_block           LZn2Ca
_cod_database_code               4330833