Monitoring the Activation of Copper-Containing Zeotype Catalysts Prepared by Direct Synthesis Using in Situ Synchrotron Infrared Microcrystal Spectroscopy and Complementary Techniques
Eschenroeder, Eike C. V.; Turrina, Alessandro; Picone, A. Lorena; Cinque, Gianfelice; Frogley, Mark D.; Cox, Paul A.; Howe, Russell F.; Wright, Paul A.; Chemistry of Materials 26 (2014) 1434–; doi:10.1021/cm403534b

data_4001888
_publ_section_title
;
 Monitoring the Activation of Copper-Containing Zeotype Catalysts Prepared
 by Direct Synthesis Using in Situ Synchrotron Infrared Microcrystal
 Spectroscopy and Complementary Techniques
;
_journal_issue                   3
_journal_name_full               'Chemistry of Materials'
_journal_page_first              1434
_journal_paper_doi               10.1021/cm403534b
_journal_volume                  26
_journal_year                    2014
_chemical_compound_source        'Hydrothermally synthesized'
_chemical_formula_analytical
'(C10 Cu1 H24 N4)2 (C8 H 20 N1)2 Al24 Si 7.2 P16.8 O96 8.1H2O'
_chemical_formula_moiety
;
;
_chemical_formula_structural     'C36 Al24 Cu2 N10 O102.29 P16.80 Si7.20'
_chemical_formula_sum            'C18 Al12 Cu N5 O51.15 P8.4 Si3.6'
_chemical_formula_weight         1853.2145
_chemical_name_common            'Cu-SAPO STA-7'
_chemical_name_systematic        'SAPO SAV framework'
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_audit_creation_date             2013-09-28T16:38
_audit_creation_method           'from EXP file using GSAS2CIF'
_audit_update_record
' 2013-09-28T16:38  Initial CIF as created by GSAS2CIF'
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            2
_cell_length_a                   18.71193(4)
_cell_length_b                   18.71193(4)
_cell_length_c                   9.39907(4)
_cell_measurement_temperature    295
_cell_volume                     3290.956(17)
_computing_structure_refinement  GSAS
_computing_structure_solution    'GSAS software suite'
_diffrn_ambient_temperature      295
_diffrn_radiation_polarisn_ratio 0.93
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.800178
_diffrn_source                   synchrotron
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  1.00000
_exptl_absorpt_process_details
;   GSAS Absorption/surface roughness correction: function number 0
 No correction is applied.
;
_exptl_crystal_density_diffrn    1.870
_exptl_crystal_F_000             1827.2
_pd_block_id                     2013-09-28T16:38|START|y|ESRF_ID31_beamline
_pd_calc_method                  'Rietveld Refinement'
_pd_char_colour                  purple
_pd_char_particle_morphology     'tetragonal prism'
_pd_instr_location               ' ?'
_pd_meas_2theta_range_inc        0.003
_pd_meas_2theta_range_max        47.979
_pd_meas_2theta_range_min        0.003
_pd_meas_number_of_points        15993
_pd_phase_name
'from C:/gsas/PhD/Cu-STA-7_as-prep_2/CuSTA7-ap.cif'
_pd_proc_2theta_range_inc        0.003
_pd_proc_2theta_range_max        47.97879
_pd_proc_2theta_range_min        0.002792
_pd_proc_info_datetime           2013-09-28T16:38:56
_pd_proc_info_excluded_regions
; 
Regions 0.1-2.7 and 39.2-49.0 excluded due to lack of reflections
;
_pd_proc_ls_background_function
;   GSAS Background function number 1 with 34 terms.
 Shifted Chebyshev function of 1st kind
      1:    1755.58     2:   -663.920     3:    90.9130     4:    135.675    
      5:   -136.562     6:   -223.695     7:    280.681     8:   -172.829    
      9:    13.0247    10:    128.032    11:   -15.5988    12:   -24.4528    
     13:    32.8299    14:   -13.3361    15:   -3.17871    16:    45.3034    
     17:   -32.8851    18:   -18.4334    19:    37.3938    20:   -13.1017    
     21:    29.8188    22:    32.9700    23:   -16.1134    24:    46.7474    
     25:    16.9124    26:   -37.4251    27:    26.3884    28:    20.0894    
     29:   -2.13802    30:    29.0626    31:   -21.2038    32:    6.52121    
     33:   -2.41655    34:    22.3232    
;
_pd_proc_ls_peak_cutoff          0.00010
_pd_proc_ls_profile_function
;
 CW Profile function number 4 with  17 terms
 Pseudovoigt profile coefficients as parameterized in
 P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
 Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994).
 J. Appl. Cryst.,27,892-900.
 Microstrain broadening by P.W. Stephens,  (1999). J. Appl. Cryst.,32,281-289.
 Peak tails are ignored  where the intensity is below 0.0001 times the peak
   Aniso. broadening axis   0.0   0.0   1.0
;
_pd_proc_ls_prof_R_factor        0.0691
_pd_proc_ls_prof_wR_expected     0.0202
_pd_proc_ls_prof_wR_factor       0.1043
_pd_proc_number_of_points        15993
_pd_spec_mounting                ' ?'
_refine_ls_goodness_of_fit_all   5.27
_refine_ls_matrix_type           full
_refine_ls_number_parameters     37
_refine_ls_number_restraints     80
_refine_ls_R_Fsqd_factor         0.12765
_refine_ls_shift/su_max          0.04
_refine_ls_shift/su_mean         0.01
_reflns_d_resolution_high        1.193
_reflns_d_resolution_low         13.231
_reflns_limit_h_max              19
_reflns_limit_h_min              0
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              9
_reflns_limit_l_min              0
_reflns_number_total             1021
_cod_data_source_file            cm403534b_si_002.cif
_cod_data_source_block           START_publ
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'N' changed to 'n' according to
/usr/data/users/saulius/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26 (133
times).

'_geom_angle_publ_flag' value 'N' changed to 'n' according
to
/usr/data/users/saulius/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26 (49
times).

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        3290.955(16)
_cod_original_sg_symbol_Hall
;
;
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_original_formula_sum        'C18.00 Al12 Cu N5 O51.15 P8.40 Si3.60'
_cod_database_code               4001888
_gsas_exptl_extinct_corr_t_min   1.00000
_gsas_exptl_extinct_corr_t_max   1.00000