Ni(II)-Mediated Self-Assembly of Artificial β-Dipeptides Forming a Macrocyclic Tetranuclear Complex with Interior Spaces for In-Line Molecular Arrangement
Ryosuke Miyake; Shohei Tashiro; Motoo Shiro; Kentaro Tanaka; Mitsuhiko Shionoya; Journal of the American Chemical Society 130 (2008) 5646–5647; doi:10.1021/ja8009555

data_4107728
_publ_contact_author_address
;
Department of Chemistry
The University of Tokyo
Graduate School of Science
7-3-1, Hongo
Bunkyo-ku
Tokyo
113-0033
;
_publ_contact_author_email       ' shionoya@chem.s.u-tokyo.ac.jp '
_publ_contact_author_fax         ' 81-3-5841-8061 '
_publ_contact_author_name        ' Prof Mitsuhiko Shionoya '
_publ_contact_author_phone       ' 81-3-5841-8061 '
_publ_section_title
;
 Ni(II)-Mediated Self-Assembly of Artificial \b-Dipeptides Forming a
 Macrocyclic Tetranuclear Complex with Interior Spaces for In-Line
 Molecular Arrangement
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5646
_journal_page_last               5647
_journal_paper_doi               10.1021/ja8009555
_journal_volume                  130
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C48 H108 N28 Ni4 O12, 8(Cl O4), 10(H2 O) '
_chemical_formula_sum            'C48 H128 Cl8 N28 Ni4 O54'
_chemical_formula_weight         2480.12
_space_group_IT_number           32
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      32
_symmetry_space_group_name_Hall  'P 2 -2ab'
_symmetry_space_group_name_H-M   'P b a 2'
_audit_creation_date             2007-11-08
_audit_creation_method           'by CrystalStructure 3.8'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   21.5700(8)
_cell_length_b                   22.1013(8)
_cell_length_c                   10.0759(3)
_cell_measurement_reflns_used    27667
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      3.3
_cell_volume                     4803.4(3)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku & RAC 2007)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'CrystalStructure (Rigaku & RAC 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Burla, 1994)'
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.106
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            44803
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    1.109
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_description       block
_exptl_crystal_F_000             2584.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.06
_refine_diff_density_min         -0.89
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  5021 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_coef       0.0124(9)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     671
_refine_ls_number_reflns         10820
_refine_ls_R_factor_gt           0.0705
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1309P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2274
_reflns_number_gt                6994
_reflns_number_total             10820
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja8009555-file002.cif
_cod_data_source_block           '_071107'
_cod_original_formula_sum        'C48 H128 Cl8 N28 Ni4 O54 '
_cod_database_code               4107728