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_4111165
_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         C37.80H48.20Cl3GdN4O19.30Zn2
_chemical_formula_sum            'C37.8 H48.2 Cl3 Gd N4 O19.3 Zn2'
_chemical_formula_weight         1261.74
_chemical_name_common            '[LZn2Gd(OAc)3] 2.8MeOH CHCl3 0.5H2O'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 121.6798(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   35.270(10)
_cell_length_b                   13.185(3)
_cell_length_c                   23.448(7)
_cell_measurement_reflns_used    30674
_cell_measurement_temperature    120
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      3.06
_cell_volume                     9279(4)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            30674
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_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    2.692
_exptl_absorpt_correction_T_max  0.7746
_exptl_absorpt_correction_T_min  0.2950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Corp., 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             5059
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.883
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     670
_refine_ls_number_reflns         8587
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0283P)^2^+27.5820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.0974
_reflns_number_gt                7372
_reflns_number_total             8587
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0646702si20060630_083733.cif
_cod_data_source_block           LZn2Gd
_cod_original_formula_sum        'C37.80 H48.20 Cl3 Gd N4 O19.30 Zn2'
_cod_database_code               4111165