Preparation and morphology of pyramidal MFI single-crystal segments.
Schmidt, Wolfgang; Wilczok, Ursula; Weidenthaler, Claudia; Medenbach, Olaf; Goddard, Richard; Buth, Gernot; Cepak, Alexander; The journal of physical chemistry. B 111 (2007) 13538–13543; doi:10.1021/jp075934p

data_1505104
_publ_section_title
;
 Preparation and morphology of pyramidal MFI single-crystal segments.
;
_journal_issue                   48
_journal_name_full               'The journal of physical chemistry. B'
_journal_page_first              13538
_journal_page_last               13543
_journal_paper_doi               10.1021/jp075934p
_journal_volume                  111
_journal_year                    2007
_chemical_compound_source        'reaction solution'
_chemical_formula_moiety         '(O2 Si)24, C12 H28 N 1+, O H 1-'
_chemical_formula_sum            'C12 H29 N O49 Si24'
_chemical_formula_weight         1645.52
_chemical_melting_point          ?
_chemical_name_common            TPA-Silicalite-1
_chemical_name_systematic
; 
 catena-(octatetraconta-oxa-tricosa-silicon 
 tetra-n-propyl-ammonium hydroxide)
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                WUM-UA-038-02
_audit_creation_date             2007-05-15
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   20.0578(4)
_cell_length_b                   19.9466(4)
_cell_length_c                   13.4070(3)
_cell_measurement_reflns_used    4824
_cell_measurement_temperature    293
_cell_measurement_theta_max      53.13
_cell_measurement_theta_min      3.97
_cell_volume                     5363.94(19)
_computing_cell_refinement       'Proteum software (Bruker-AXS, 2005)'
_computing_data_collection       'Proteum software (Bruker-AXS, 2005)'
_computing_data_reduction        'Proteum software (Bruker-AXS, 2005)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'Bruker-AXS X8-Proteum'
_diffrn_measurement_method       'CCD \p and \w-scans'
_diffrn_radiation_monochromator  'Montel coated mirrors'
_diffrn_radiation_source         '0.2 mm focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54188
_diffrn_reflns_av_R_equivalents  0.1280
_diffrn_reflns_av_sigmaI/netI    0.0746
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            79163
_diffrn_reflns_theta_full        68.85
_diffrn_reflns_theta_max         68.85
_diffrn_reflns_theta_min         3.97
_diffrn_standards_decay_%        0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.521
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6548
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker AXS (2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.038
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             3344
_exptl_crystal_size_max          0.045
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.028
_refine_diff_density_max         0.882
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.169
_refine_ls_extinction_coef       0.00028(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         4840
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1166
_refine_ls_R_factor_gt           0.0663
_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^)+(0.1278P)^2^+11.3746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1826
_refine_ls_wR_factor_ref         0.2308
_reflns_number_gt                2811
_reflns_number_total             4840
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jp075934p_tpasilicalite1_1030.cif
_cod_data_source_block           TPA-Silicalite-1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not determined' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               1505104