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_4105531
_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            'C588 H509 B32 F128 N150 O11 Zn16'
_chemical_formula_weight         13676.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 99.950(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.117(3)
_cell_length_b                   51.828(3)
_cell_length_c                   48.797(3)
_cell_measurement_reflns_used    6462
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      84.410
_cell_measurement_theta_min      4.591
_cell_volume                     77513(10)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SHELXTL (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  'SHELXTL (Bruker, 2001)'
_computing_structure_refinement  'SHELXTL (Bruker, 2001)'
_computing_structure_solution    'SHELXTL (Bruker, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 0.915
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Frames, each covering 0.3 \% in \w'
_diffrn_radiation_monochromator  'Osmic ConFocal MaxFlux mirror optics'
_diffrn_radiation_source         '4.8 kW rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1181
_diffrn_reflns_av_sigmaI/netI    0.1129
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       63
_diffrn_reflns_limit_k_min       -63
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            302409
_diffrn_reflns_theta_full        70.55
_diffrn_reflns_theta_max         70.55
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    1.281
_exptl_absorpt_correction_T_max  0.7740
_exptl_absorpt_correction_T_min  0.7140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_description       block
_exptl_crystal_F_000             27912
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.613
_refine_diff_density_min         -2.236
_refine_diff_density_rms         0.172
_refine_ls_extinction_coef       0.0000059(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.358
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1734
_refine_ls_number_reflns         67955
_refine_ls_number_restraints     3443
_refine_ls_restrained_S_all      1.387
_refine_ls_R_factor_all          0.2594
_refine_ls_R_factor_gt           0.1882
_refine_ls_shift/su_max          0.322
_refine_ls_shift/su_mean         0.017
_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          0.4695
_refine_ls_wR_factor_ref         0.5014
_reflns_number_gt                24365
_reflns_number_total             67955
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja107403p_si_001_1.cif
_cod_data_source_block           zn16l24a
_cod_original_cell_volume        77513(9)
_cod_database_code               4105531