In SituTransformation of TON Silica Zeolite into the Less Dense ITW: Structure-Direction Overcoming Framework Instability in the Synthesis of SiO2 Zeolites
Claudio M. Zicovich-Wilson; Felipe Gándara; Angeles Monge; Miguel A. Camblor; Journal of the American Chemical Society 132 (2010) 3461–3471; doi:10.1021/ja9094318

data_4102044
_publ_contact_author_address
;
Instituto de Ciencia de Materiales de Madrid,
 Consejo Superior de Investigaciones Cient\'ificas,
c/ Sor Juana In\'es de la Cruz, 3, 28049 Madrid, Spain.
;
_publ_contact_author_email       macamblor@icmm.cisc.es
_publ_contact_author_name        'M. A. Camblor'
_publ_section_title
;
 In SituTransformation of TON Silica Zeolite into the Less Dense ITW:
 Structure-Direction Overcoming Framework Instability in the Synthesis of
 SiO2 Zeolites
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3461
_journal_page_last               3471
_journal_paper_doi               10.1021/ja9094318
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C4.92 F0.82 N1.64 O48 Si24'
_chemical_formula_sum            'C4.92 F0.82 N1.64 O48 Si24'
_chemical_formula_weight         1549.23
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_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            1
_cell_length_a                   13.723(2)
_cell_length_b                   17.458(3)
_cell_length_c                   5.0756(8)
_cell_measurement_reflns_used    1018
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.95
_cell_measurement_theta_min      2.33
_cell_volume                     1216.0(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      295(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0543
_diffrn_reflns_av_sigmaI/netI    0.0775
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            2805
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.752
_exptl_absorpt_correction_T_max  0.9563
_exptl_absorpt_correction_T_min  0.8891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.116
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             773
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.3(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_refine_ls_number_reflns         1189
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0618
_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^)+(0.0855P)^2^+2.2255P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1490
_refine_ls_wR_factor_ref         0.1572
_reflns_number_gt                966
_reflns_number_total             1189
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9094318_si_001.cif
_cod_data_source_block           TON_template
_cod_database_code               4102044