Helical Metallohost-Guest Complexes via Site-Selective Transmetalation of Homotrinuclear Complexes
Shigehisa Akine; Takanori Taniguchi; Tatsuya Nabeshima; Journal of the American Chemical Society 128 (2006) 15765–15774; doi:10.1021/ja0646702

data_4111166
_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
;
 Helical Metallohost-Guest Complexes via Site-Selective Transmetalation of
 Homotrinuclear Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15765
_journal_page_last               15774
_journal_paper_doi               10.1021/ja0646702
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         C39H51N4O19TbZn2
_chemical_formula_sum            'C39 H51 N4 O19 Tb Zn2'
_chemical_formula_weight         1169.50
_chemical_name_common            '[LZn2Tb(OAc)3(MeOH)] (H2O)(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                73.867(19)
_cell_angle_beta                 83.20(2)
_cell_angle_gamma                86.92(2)
_cell_formula_units_Z            2
_cell_length_a                   12.948(9)
_cell_length_b                   13.222(8)
_cell_length_c                   13.435(8)
_cell_measurement_reflns_used    15937
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      3.07
_cell_volume                     2193(2)
_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    'DIRDIF99 (Beurskens et al., 1999)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.937
_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  0.0600
_diffrn_reflns_av_sigmaI/netI    0.1171
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15937
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.762
_exptl_absorpt_correction_T_max  0.6821
_exptl_absorpt_correction_T_min  0.4448
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Corp., 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.209
_refine_diff_density_min         -2.073
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         8982
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0546
_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^)+(0.0342P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1350
_refine_ls_wR_factor_ref         0.1409
_reflns_number_gt                7733
_reflns_number_total             8982
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0646702si20060630_083808.cif
_cod_data_source_block           LZn2Tb
_cod_database_code               4111166