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_4105533
_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            'C306 H294 B12 F60 N90 Ni8 O36 Si2'
_chemical_formula_weight         7603.89
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :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            6
_cell_length_a                   26.0607(3)
_cell_length_b                   26.0607(3)
_cell_length_c                   98.7782(14)
_cell_measurement_reflns_used    29485
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     58098.4(13)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Bruker-Nonius APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       128
_diffrn_reflns_limit_l_min       -128
_diffrn_reflns_number            170210
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    0.485
_exptl_absorpt_correction_T_max  0.9531
_exptl_absorpt_correction_T_min  0.9092
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       'light purple'
_exptl_crystal_F_000             23340
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.924
_refine_diff_density_min         -1.095
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.736
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         14798
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.737
_refine_ls_R_factor_all          0.1462
_refine_ls_R_factor_gt           0.1294
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3960
_refine_ls_wR_factor_ref         0.4101
_reflns_number_gt                12045
_reflns_number_total             14798
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja107403p_si_001_3.cif
_cod_data_source_block           2008src1191
_cod_original_cell_volume        58098.3(13)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4105533