Assembly Modulation by Adjusting Countercharges of Heterobimetallic Supramolecular Polymers Composed of Tris(spiroborate) Twin Bowls
Hiroshi Danjo; Kadzuya Hirata; Masanori Noda; Susumu Uchiyama; Kiichi Fukui; Masatoshi Kawahata; Isao Azumaya; Kentaro Yamaguchi; Toshifumi Miyazawa; Journal of the American Chemical Society 132 (2010) 15556–15558; doi:10.1021/ja1084964

data_4103470
_publ_contact_author_address
;Department of Chemistry
Faculty of Science and Technology
Konan University
Okamoto Higashinada Kobe 6588501 Japan
;
_publ_contact_author_email       danjo@konan-u.ac.jp
_publ_contact_author_fax         81(78)4352539
_publ_contact_author_name        'Hiroshi Danjo'
_publ_contact_author_phone       81(78)4352502
_publ_section_title
;
 Assembly Modulation by Adjusting Countercharges of Heterobimetallic
 Supramolecular Polymers Composed of Tris(spiroborate) Twin Bowls
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15556
_journal_page_last               15558
_journal_paper_doi               10.1021/ja1084964
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C76 H74 B3 K N6 O18'
_chemical_formula_weight         1430.94
_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                83.6720(10)
_cell_angle_beta                 77.0270(10)
_cell_angle_gamma                67.0870(10)
_cell_formula_units_Z            2
_cell_length_a                   14.5849(11)
_cell_length_b                   16.2575(12)
_cell_length_c                   18.6167(14)
_cell_measurement_temperature    150
_cell_volume                     3960.9(5)
_computing_cell_refinement       'APEX II (Bruker AXS, 2006)'
_computing_data_collection       'APEX II (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.861
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measurement_device_type  'Bruker APEX II CCD Area Detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0146
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19537
_diffrn_reflns_theta_full        27.09
_diffrn_reflns_theta_max         27.09
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.136
_exptl_absorpt_correction_T_max  0.9733
_exptl_absorpt_correction_T_min  0.9603
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_crystal_colour            'pale orange'
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prsimatic
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.008
_refine_diff_density_min         -1.145
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.792
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     949
_refine_ls_number_reflns         15011
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.795
_refine_ls_R_factor_all          0.1845
_refine_ls_R_factor_gt           0.1471
_refine_ls_shift/su_max          5.081
_refine_ls_shift/su_mean         0.075
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4174
_refine_ls_wR_factor_ref         0.4483
_reflns_number_gt                10189
_reflns_number_total             15011
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1084964_si_002.cif
_cod_data_source_block           c:\xray_data\a\a0805281dan
_cod_database_code               4103470