Further investigations into tetrahedral M4L6 cage complexes containing guest anions: new structures and NMR spectroscopic studies
Tidmarsh, Ian S.; Taylor, Brian F.; Hardie, Michaele J.; Russo, Luca; Clegg, William; Ward, Michael D.; New Journal of Chemistry 33 (2009) 366–; doi:10.1039/b816864d

data_7051642
_publ_section_title
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 Further investigations into tetrahedral M4L6 cage complexes containing
 guest anions: new structures and NMR spectroscopic studies
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_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              366
_journal_paper_doi               10.1039/b816864d
_journal_volume                  33
_journal_year                    2009
_chemical_formula_sum            'C168 H132 F24 N36 Si4 Zn4'
_chemical_formula_weight         3484.94
_chemical_name_systematic
;
?
;
_space_group_IT_number           205
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.973(10)
_cell_length_b                   32.973(10)
_cell_length_c                   32.973(10)
_cell_measurement_reflns_used    9687
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.97
_cell_measurement_theta_min      2.19
_cell_volume                     35849(19)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEX2 CCD diffractometer'
_diffrn_measurement_method       'fine-slice \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6926
_diffrn_reflns_av_R_equivalents  0.1191
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            191194
_diffrn_reflns_theta_full        22.49
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         3.82
_exptl_absorpt_coefficient_mu    0.639
_exptl_absorpt_correction_T_max  0.9447
_exptl_absorpt_correction_T_min  0.8882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             14272
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.243
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.518
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         8337
_refine_ls_number_restraints     117
_refine_ls_restrained_S_all      1.510
_refine_ls_R_factor_all          0.2315
_refine_ls_R_factor_gt           0.1578
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4413
_refine_ls_wR_factor_ref         0.4761
_reflns_number_gt                4002
_reflns_number_total             8337
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b816864d.txt
_cod_data_source_block           ssh0399
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Cubic' changed to 'cubic' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_original_sg_symbol_H-M      Pa-3
_cod_database_code               7051642