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_4111173
_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         C36H46N5O20ScZn2
_chemical_formula_sum            'C36 H46 N5 O20 Sc Zn2'
_chemical_formula_weight         1044.48
_chemical_name_common            '[LZn2Sc(OAc)2](NO3)(MeOH)2(EtOH)'
_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                95.050(8)
_cell_angle_beta                 95.675(9)
_cell_angle_gamma                94.160(7)
_cell_formula_units_Z            4
_cell_length_a                   12.297(6)
_cell_length_b                   16.082(8)
_cell_length_c                   21.117(10)
_cell_measurement_reflns_used    27287
_cell_measurement_temperature    120
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      3.07
_cell_volume                     4126(3)
_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 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Rigaku Mercury CCD system'
_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  0.0525
_diffrn_reflns_av_sigmaI/netI    0.0835
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27287
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_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    1.403
_exptl_absorpt_correction_T_max  0.8171
_exptl_absorpt_correction_T_min  0.5709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Corp., 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.816
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1163
_refine_ls_number_reflns         14191
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.1159
_refine_ls_R_factor_gt           0.0778
_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^)+(0.0579P)^2^+13.4241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1546
_refine_ls_wR_factor_ref         0.1702
_reflns_number_gt                10173
_reflns_number_total             14191
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0646702si20060630_084137.cif
_cod_data_source_block           LZn2Sc
_cod_original_cell_volume        4125(4)
_cod_database_code               4111173