Synthesis and Hydrogen Storage Properties of Be12(OH)12(1,3,5-benzenetribenzoate)4
Kenji Sumida; Matthew R. Hill; Satoshi Horike; Anne Dailly; Jeffrey R. Long; Journal of the American Chemical Society 131 (2009) 15120–15121; doi:10.1021/ja9072707

data_4105220
_publ_section_title
;
 Synthesis and Hydrogen Storage Properties of
 Be12(OH)12(1,3,5-benzenetribenzoate)4
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15120
_journal_page_last               15121
_journal_paper_doi               10.1021/ja9072707
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C54 H36 Be6 O18'
_chemical_formula_sum            'C54 H36 Be6 O18'
_chemical_formula_weight         1026.89
_chemical_melting_point_gt       500
_chemical_name_common            BeBTB
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           116
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 -2c'
_symmetry_space_group_name_H-M   'P -4 c 2'
_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                   24.3013(9)
_cell_length_b                   24.3013(9)
_cell_length_c                   54.570(3)
_cell_measurement_reflns_used    9824
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      107.835
_cell_measurement_theta_min      4.870
_cell_volume                     32226(2)
_computing_cell_refinement       'Bruker APEX2 v. 2009.1'
_computing_data_collection       'Bruker APEX2 v. 2009.1'
_computing_data_reduction        'Bruker APEX2 v. 2009.1'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'HELIOS multilayer mirrors'
_diffrn_radiation_source         'microfocus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0164
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            157589
_diffrn_reflns_theta_full        50.46
_diffrn_reflns_theta_max         50.46
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    0.259
_exptl_absorpt_correction_T_max  0.9451
_exptl_absorpt_correction_T_min  0.9380
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.423
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             4224
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_platon_squeeze_details
;
;
_refine_diff_density_max         0.061
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.012
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.54(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         16885
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0560P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0863
_reflns_number_gt                14199
_reflns_number_total             16885
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9072707_si_002.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_melting_point_gt' since the value was specified 'more
than' ('>') a certain temperature. The value '>500 K' was changed to
'500' - it should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        32227(2)
_cod_original_sg_symbol_Hall     'P -4 -2 c'
_cod_database_code               4105220