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_4110347
_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         'C576 H480 Cd16 N144, 28(Cl O4), 23(C2 H3 N)'
_chemical_formula_sum            'C622 H549 Cd16 Cl28 N167 O112'
_chemical_formula_weight         14946.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.5810(10)
_cell_angle_beta                 79.9780(10)
_cell_angle_gamma                70.1050(10)
_cell_formula_units_Z            2
_cell_length_a                   29.7224(8)
_cell_length_b                   30.1896(8)
_cell_length_c                   52.4872(13)
_cell_measurement_reflns_used    7472
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.119
_cell_measurement_theta_min      2.634
_cell_volume                     43603(2)
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 0.713
_diffrn_measured_fraction_theta_max 0.713
_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  0.0501
_diffrn_reflns_av_sigmaI/netI    0.0690
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -63
_diffrn_reflns_number            232145
_diffrn_reflns_theta_full        70.19
_diffrn_reflns_theta_max         70.19
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    4.394
_exptl_absorpt_correction_T_max  0.6677
_exptl_absorpt_correction_T_min  0.4736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             15180
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.660
_refine_diff_density_min         -1.599
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.396
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     3875
_refine_ls_number_reflns         118370
_refine_ls_number_restraints     41577
_refine_ls_restrained_S_all      1.348
_refine_ls_R_factor_all          0.1489
_refine_ls_R_factor_gt           0.1269
_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          0.3487
_refine_ls_wR_factor_ref         0.3820
_reflns_number_gt                78343
_reflns_number_total             118370
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja056993osi20051024_054315_2.cif
_cod_data_source_block           cdsdcm
_cod_database_code               4110347