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_4001886
_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_formula_moiety         '8(Al3 O12 P3), Cu0.62 N8 O2, 2(C8 N), 8(C)'
_chemical_formula_sum            'C8 Al12 Cu0.32 N5 O48 P12'
_chemical_formula_weight         1649.8911
_chemical_name_common            'Cu-SAPO STA-7, dehydrated 250 degree C'
_chemical_name_systematic
;
Cu-SAPO STA-7, dehydrated 250 degree C
;
_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'
_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            2
_cell_length_a                   18.741(7)
_cell_length_b                   18.741(7)
_cell_length_c                   9.414(4)
_cell_measurement_reflns_used    4643
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      28.7
_cell_measurement_theta_min      2.2
_cell_volume                     3306(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector                 CCD
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device
;
AFC7: Eulerian 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Mercury (2x2 bin mode)
;
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3725
_diffrn_reflns_av_sigmaI/netI    0.2458
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            20513
_diffrn_reflns_theta_full        25.32
_diffrn_reflns_theta_max         25.32
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.670
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.980
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            PURPLE
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1624.6
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.210
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         3024
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.2442
_refine_ls_R_factor_gt           0.1357
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.028
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1985P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3290
_refine_ls_wR_factor_ref         0.3441
_reflns_number_gt                1397
_reflns_number_total             3026
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            cm403534b_si_003.cif
_cod_data_source_block           250C
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        3306.0(2)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               4001886