Redox-Switched Complexation/Decomplexation of K+ and Cs+ by Molecular Cyanometalate Boxes
Julie L. Boyer; Maya Ramesh; Haijun Yao; Thomas B. Rauchfuss; Scott R. Wilson; Journal of the American Chemical Society 129 (2007) 1931–1936; doi:10.1021/ja0646545

data_4109088
_publ_contact_author
; 
Scott R. Wilson 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_contact_author_email       srwilson@uiuc.edu
_publ_contact_author_fax         '1  217 244 8068'
_publ_contact_author_phone       '1  217 244 1708'
_publ_section_title
;
 Redox-Switched Complexation/Decomplexation of K+ and Cs+ by Molecular
 Cyanometalate Boxes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1931
_journal_page_last               1936
_journal_paper_doi               10.1021/ja0646545
_journal_volume                  129
_journal_year                    2007
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C64 H68 Co8 N12, 2(C4 H8 O), F6 P, K'
_chemical_formula_sum            'C72 H84 Co8 F6 K N12 O2 P'
_chemical_formula_weight         1805.02
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
; 
2005-06-13   text and data added, yao 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.853(4)
_cell_length_b                   12.853(4)
_cell_length_c                   23.193(14)
_cell_measurement_reflns_used    1018
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      24.4
_cell_measurement_theta_min      3.2
_cell_volume                     3831(3)
_computing_cell_refinement       'SAINT V6.22 (Bruker, 2001)'
_computing_data_collection       'SMART V5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT V6.22 (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL V6.12 (Bruker, 2001)'
_computing_publication_material  'CIFTAB (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2001)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2001)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Siemens Platform/CCD'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  p83was
_diffrn_reflns_av_R_equivalents  0.0906
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            30511
_diffrn_reflns_theta_full        25.45
_diffrn_reflns_theta_max         25.45
_diffrn_reflns_theta_min         2.85
_diffrn_standards_decay_%        0.6
_diffrn_standards_interval_time  631
_diffrn_standards_number         285
_exptl_absorpt_coefficient_mu    1.829
_exptl_absorpt_correction_T_max  0.8820
_exptl_absorpt_correction_T_min  0.7630
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Bruker, 2001)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       tabular
_exptl_crystal_F_000             1840
_exptl_crystal_id                p83was
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (??) scattering planes 
roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack (1983),  1546 Friedels'
_refine_ls_abs_structure_Flack   0.019(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3525
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0297P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0618
_refine_ls_wR_factor_ref         0.0656
_reflns_number_gt                2969
_reflns_number_total             3525
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0646545si20060630_104800.cif
_cod_data_source_block           p83was
_cod_original_cell_volume        3832(3)
_cod_original_sg_symbol_Hall     'P -4 2n '
_cod_original_sg_symbol_H-M      'P -4 21 c '
_cod_database_code               4109088