A Study of Piperidinium Structure-Directing Agents in the Synthesis of Silica Molecular Sieves under Fluoride-Based Conditions
Stacey I. Zones; Allen W. Burton; Greg S. Lee; Marilyn M. Olmstead; Journal of the American Chemical Society 129 (2007) 9066–9079; doi:10.1021/ja0709122

data_4109680
_publ_section_title
;
 A Study of Piperidinium Structure-Directing Agents in the Synthesis of
 Silica Molecular Sieves under Fluoride-Based Conditions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9066
_journal_page_last               9079
_journal_paper_doi               10.1021/ja0709122
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'Si16 O32 F, C11 H24 N'
_chemical_formula_sum            'C11 H24 F N O32 Si16'
_chemical_formula_weight         1150.75
_chemical_name_common            SSZ-35/C11H24N
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.207(3)
_cell_angle_beta                 96.995(3)
_cell_angle_gamma                94.425(3)
_cell_formula_units_Z            1
_cell_length_a                   7.4025(12)
_cell_length_b                   11.3530(18)
_cell_length_c                   11.4856(18)
_cell_measurement_reflns_used    3768
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.3
_cell_measurement_theta_min      2.6
_cell_volume                     918.5(3)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        'SAINT and cell_now (Sheldrick, 2005)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker ApexII'
_diffrn_measurement_method       \w
_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  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0720
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17537
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.86
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.676
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Twinabs (Sheldrick, 2004)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.080
_exptl_crystal_description       needle
_exptl_crystal_F_000             586
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.583
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5049
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.584
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+13.3753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.1001
_reflns_number_gt                3629
_reflns_number_total             5057
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja0709122si20070208_095000.cif
_cod_data_source_block           twin
_cod_database_code               4109680