Structures and Dynamic Behavior of Large Polyhedral Coordination Cages: An Unusual Cage-to-Cage Interconversion
Andrew Stephenson; Stephen P. Argent; Thomas Riis-Johannessen; Ian S. Tidmarsh; Michael D. Ward; Journal of the American Chemical Society 133 (2011) 858–870; doi:10.1021/ja107403p

data_4105532
_publ_contact_author
; 
        Prof. Mike Ward
        Department of Chemistry
        University of Sheffield
        SHEFFIELD
        S3 7HF
;
_publ_contact_author_email       m.d.ward@sheffield.ac.uk
_publ_contact_author_fax         '0114 2229346'
_publ_section_title
;
 Structures and Dynamic Behavior of Large Polyhedral Coordination Cages:
 An Unusual Cage-to-Cage Interconversion
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              858
_journal_page_last               870
_journal_paper_doi               10.1021/ja107403p
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C216 H180 B12 Cu6 F48 N54'
_chemical_formula_weight         4955.10
_chemical_name_systematic
; 
 ? 
;
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_symmetry_cell_setting           orthorhombic
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.7261(11)
_cell_length_b                   56.9758(17)
_cell_length_c                   29.7638(9)
_cell_measurement_reflns_used    9437
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      19.08
_cell_measurement_theta_min      2.31
_cell_volume                     53802(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.1517
_diffrn_reflns_av_sigmaI/netI    0.1773
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       71
_diffrn_reflns_limit_k_min       -64
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            261120
_diffrn_reflns_theta_full        26.48
_diffrn_reflns_theta_max         26.48
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_T_max  0.9005
_exptl_absorpt_correction_T_min  0.8559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.095
_exptl_crystal_description       block
_exptl_crystal_F_000             18192
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.057
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.144(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2071
_refine_ls_number_reflns         54501
_refine_ls_number_restraints     2673
_refine_ls_restrained_S_all      0.915
_refine_ls_R_factor_all          0.2267
_refine_ls_R_factor_gt           0.1068
_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^)+(0.1750P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2721
_refine_ls_wR_factor_ref         0.3227
_reflns_number_gt                18874
_reflns_number_total             54501
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja107403p_si_001_2.cif
_cod_data_source_block           imw1390
_cod_database_code               4105532