Templating Odd Numbered Magnetic Rings: Oxovanadium Heptagons Sandwiched by β-Cyclodextrins
Norihisa Hoshino; Motohiro Nakano; Hiroyuki Nojiri; Wolfgang Wernsdorfer; Hiroki Oshio; Journal of the American Chemical Society 131 (2009) 15100–15101; doi:10.1021/ja9066496

data_4105205
_publ_contact_author_address
;
 Graduate School of Pure and Applied Sciences
 University of Tsukuba
 Tennodai 1-1-1
 Tsukuba 305-8571
 Japan
;
_publ_contact_author_email       oshio@chem.tsukuba.ac.jp
_publ_contact_author_fax         +81-29-853-4238
_publ_contact_author_name        'Prof. Hiroki Oshio'
_publ_contact_author_phone       +81-29-853-4238
_publ_section_title
;
 Templating Odd Numbered Magnetic Rings: Oxovanadium Heptagons Sandwiched
 by \b-Cyclodextrins
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15100
_journal_page_last               15101
_journal_paper_doi               10.1021/ja9066496
_journal_volume                  131
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_formula_moiety
'(C84 H126 Na14 O84 V7 7-), 7(Na +), 65(H2 O)'
_chemical_formula_sum            'C84 H256 Na14 O149 V7'
_chemical_formula_weight         4329.33
_chemical_name_systematic
; 
 Na7[(V=O)7Na7(H2O)7(b-CD)2].65H2O (1)
;
_space_group_IT_number           155
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 2"'
_symmetry_space_group_name_H-M   'R 3 2 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            9
_cell_length_a                   34.444(3)
_cell_length_b                   34.444(3)
_cell_length_c                   46.286(6)
_cell_measurement_reflns_used    978
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      18.867
_cell_measurement_theta_min      2.365
_cell_volume                     47556(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_sigmaI/netI    0.0707
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            75501
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.435
_exptl_absorpt_correction_T_max  0.9180
_exptl_absorpt_correction_T_min  0.8118
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       rod
_exptl_crystal_F_000             20403
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
 Use of the SQUEEZE subroutine of the PLATON program suite
 (PLATON Reference : Spek, A.L. (1990), Acta Cryst. A46, C-34)
 indicated the presence of a large solvent accessible void
 comprising a total volume of 25213.6 A. Calculations indicated
 the contribution of 6523.1 -e per lattice due to diffuse cation
 and solvent scattering. 630 electrons are assigned to the 63
 sodium cations, with the remaining 5850 electrons assigned to
 585 molecules of water. This equates to 7 sodium cations and
 65 water molecules per a [(V=O)7Na7(H2O)7(b-CD)2]7- ion.
;
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.10(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     823
_refine_ls_number_reflns         18547
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0709
_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^)+(0.1167P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1761
_refine_ls_wR_factor_ref         0.1912
_reflns_number_gt                11233
_reflns_number_total             18547
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9066496_si_001_1.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'R 3 2'
_cod_database_code               4105205