Facile Synthesis and Catalysis of Pure-Silica and Heteroatom LTA
Boal, Ben W.; Schmidt, Joel E.; Deimund, Mark A.; Deem, Michael W.; Henling, Lawrence M.; Brand, Stephen K.; Zones, Stacey I.; Davis, Mark E.; Chemistry of Materials 27 (2015) 7774–; doi:10.1021/acs.chemmater.5b03579

data_4003209
_publ_section_title
;
 Facile Synthesis and Catalysis of Pure-Silica and Heteroatom LTA
;
_journal_issue                   22
_journal_name_full               'Chemistry of Materials'
_journal_page_first              7774
_journal_paper_doi               10.1021/acs.chemmater.5b03579
_journal_volume                  27
_journal_year                    2015
_chemical_formula_moiety         '0.08(O24 Si12), 0.1(F1), 0.04(C4 H12 N1)'
_chemical_formula_sum            'C0.17 H0.5 F0.1 N0.04 O2 Si'
_chemical_formula_weight         65.17
_space_group_crystal_system      cubic
_space_group_IT_number           221
_space_group_name_Hall           '-P 4 2 3'
_space_group_name_H-M_alt        'P m -3 m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-31
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)),
 SHELXL-2014,
 and manual edit
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   11.824(5)
_cell_length_b                   11.824(5)
_cell_length_c                   11.824(5)
_cell_measurement_reflns_used    9063
_cell_measurement_temperature    100
_cell_measurement_theta_max      49.13
_cell_measurement_theta_min      2.44
_cell_volume                     1653.1(12)
_computing_cell_refinement       'SAINT v8.34A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 2014.11-0 (Bruker-AXS, 2007)'
_computing_data_reduction        'SAINT V8.34A (Bruker-AXS, 2007)'
_computing_molecular_graphics    'DIAMOND 3 (Crystal Impact, 1999)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement
;
SHELXL-2014/7 (Sheldrick, 2014)
PLATON-30715 SQUEEZE (Spek, 2015)  
;
_computing_structure_solution    'XT-2014/4 (Sheldrick, 2012)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CMOS Area Detector'
_diffrn_detector_area_resol_mean 10.24
_diffrn_detector_type            'Bruker PHOTON 100 CMOS'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            52351
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         51.444
_diffrn_reflns_theta_min         2.436
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_diffrn_source_current           1
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatech I\mS HB'
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.557
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0609 before and 0.0531 after correction. The Ratio of minimum to maximum transmission is 0.8917. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_description       cube
_exptl_crystal_F_000             786
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     31
_refine_ls_number_reflns         1863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+0.4532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0798
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1491
_reflns_number_total             1863
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm5b03579_si_003.cif
_cod_data_source_block           p15134
_cod_original_cell_volume        1653(2)
_cod_original_formula_sum        'C0.17 H0.50 F0.10 N0.04 O2 Si'
_cod_database_code               4003209
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.952
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C1(0.0833) H1B(0.0833) H1A(0.0833) H1C(0.0833)
3.a Everything fixed:
 H1B, H1A, H1C
;
_shelx_fab_checksum              62936
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'