Determining the structure of a benzene7.2-silicalite-1 zeolite using a single-crystal X-ray method
Kamiya, Natsumi; Iwama, Wataru; Kudo, Tomokazu; Nasuno, Tomomi; Fujiyama, Shinjiro; Nishi, Koji; Yokomori, Yoshinobu; Acta Crystallographica Section B 67 (2011) 508–515; doi:10.1107/S0108768111038560

data_2104993
_publ_section_title
;
 Determining the structure of a benzene7.2-silicalite-1 zeolite using a
 single-crystal X-ray method
;
_journal_coeditor_code           DK5001
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              508
_journal_page_last               515
_journal_paper_doi               10.1107/S0108768111038560
_journal_volume                  67
_journal_year                    2011
_chemical_formula_sum            'C5.38 H5.38 O24 Si12'
_chemical_formula_weight         791.05
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   19.920(12)
_cell_length_b                   19.880(13)
_cell_length_c                   13.386(9)
_cell_measurement_temperature    296
_cell_volume                     5301(6)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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      296
_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'
_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  0.0539
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            50699
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.689
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.936
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'crystal faces of APEX 2 of Bruker Axs'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.982
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rounded-boat
_exptl_crystal_F_000             3181
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.424
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         3568
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0793P)^2^+0.0184P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1298
_reflns_number_gt                3568
_reflns_number_total             4998
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            dk5001.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               2104993
_cod_database_fobs_code          2104993