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_4105206
_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 +), 39(H2 O)'
_chemical_formula_sum            'C84 H204 Na14 O123 V7'
_chemical_formula_weight         3860.91
_chemical_name_systematic
; 
 Na7[(V=O)7Na7(H2O)7(b-CD)2].39H2O (2)
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 100.184(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   21.322(8)
_cell_length_b                   18.694(7)
_cell_length_c                   23.798(9)
_cell_measurement_reflns_used    973
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      18.564
_cell_measurement_theta_min      2.262
_cell_volume                     9336(6)
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0846
_diffrn_reflns_av_sigmaI/netI    0.1233
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            43616
_diffrn_reflns_theta_full        25.12
_diffrn_reflns_theta_max         25.12
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    0.474
_exptl_absorpt_correction_T_max  0.9733
_exptl_absorpt_correction_T_min  0.8685
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Bruker XPREP'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       plate
_exptl_crystal_F_000             4014
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.06
_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 large solvent accessible voids
 comprising a total volume of 4332.4 A. Calculations indicated
 the contribution of 917.3 -e per lattice due to diffuse cation
 and solvent scattering. 140 electrons are assigned to the 14
 sodium cations, with the remaining 780 electrons assigned to
 78 molecules of water. This equates to 7 sodium cations and
 39 water molecules per a [(V=O)7Na7(H2O)7(b-CD)2]7- ion.
;
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.09(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.883
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1639
_refine_ls_number_reflns         22800
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      0.891
_refine_ls_R_factor_all          0.1137
_refine_ls_R_factor_gt           0.0772
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1202P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1925
_refine_ls_wR_factor_ref         0.2067
_reflns_number_gt                12138
_reflns_number_total             22800
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9066496_si_001_2.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4105206