High-nuclearity Homoleptic and Heteroleptic Coordination Cages Based on Tetra-Capped Truncated Tetrahedral and Cuboctahedral Metal Frameworks
Stephen P. Argent; Harry Adams; Thomas Riis-Johannessen; John C. Jeffery; Lindsay P. Harding; Michael D. Ward; Journal of the American Chemical Society 128 (2006) 72–73; doi:10.1021/ja056993o

data_4110346
_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
;
 High-nuclearity Homoleptic and Heteroleptic Coordination Cages Based on
 Tetra-Capped Truncated Tetrahedral and Cuboctahedral Metal Frameworks
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              72
_journal_page_last               73
_journal_paper_doi               10.1021/ja056993o
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety
'C432 H370 Cu12 N108, 10(B F4), 20(C H3 N O2)'
_chemical_formula_sum            'C452 H430 B10 Cu12 F40 N128 O40'
_chemical_formula_weight         9925.82
_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                 102.003(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.840(7)
_cell_length_b                   50.544(13)
_cell_length_c                   48.629(12)
_cell_measurement_reflns_used    1016
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      37.267
_cell_measurement_theta_min      4.911
_cell_volume                     59719(3)
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker smart 1000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1423
_diffrn_reflns_av_sigmaI/netI    0.1860
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            173661
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.493
_exptl_absorpt_correction_T_max  0.9387
_exptl_absorpt_correction_T_min  0.7733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            GREEN
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             20464
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.812
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1430
_refine_ls_number_reflns         39038
_refine_ls_number_restraints     5183
_refine_ls_restrained_S_all      0.794
_refine_ls_R_factor_all          0.1789
_refine_ls_R_factor_gt           0.0968
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1755P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2513
_refine_ls_wR_factor_ref         0.2943
_reflns_number_gt                15302
_reflns_number_total             39038
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja056993osi20051024_054315_1.cif
_cod_data_source_block           imw289m
_cod_original_cell_volume        59720(27)
_cod_database_code               4110346