# Electronic Supplementary Material (ESI) for Physical Chemistry Chemical Physics
# This journal is © The Owner Societies 2011


data_global
_journal_name_full               Phys.Chem.Chem.Phys.(PCCP)

_journal_coden_Cambridge         1326

_publ_contact_author_name        'Kirschhock, Christine'
_publ_contact_author_email       christine.kirschhock@biw.kuleuven.be

_publ_section_title              
;
Zeolite Y and A Crystallization Compared by Simultaneous
UV/VIS-Raman and X-Ray Diffraction
;
loop_
_publ_author_name
A.Depla
E.Verheyen
A.Veyfeyken
E.Gobechiya
T.Hartmann
;
R.Schafer
;
J.Martens
C.Kirschhock

#Attachment 'ZeoliteA_final.cif'

data_ZeoliteA_publ
_database_code_depnum_ccdc_archive 'CCDC 831422'
#TrackingRef 'ZeoliteA_final.cif'

_pd_block_id                     2010-12-08T14:54|ZeoliteA|STOE_STADI_MP

_audit_creation_method           'from EXP file using GSAS2CIF'
_audit_creation_date             2010-12-17T15:00
_audit_author_name               ZEOLA1
_audit_update_record             
; 2010-12-17T15:00 Initial CIF as created by GSAS2CIF
;

_refine_ls_shift/su_max          16.61
_refine_ls_shift/su_mean         3.37
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     46
_refine_ls_goodness_of_fit_all   2.58
_refine_ls_number_restraints     0
_refine_ls_matrix_type           full

_pd_phase_name                   'Zeolite A'
_cell_length_a                   24.58020(20)
_cell_length_b                   24.5802
_cell_length_c                   24.5802
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_volume                     14851.0(4)
_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   'F m -3 c'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
Na NA1 0.09943(12) 0.09943(12) 0.09943(12) 1.0 Uani 0.02005 64
Na NA2 0.0 0.25 0.25 0.66666 Uiso 0.356(28) 24
Na NA3 0.25 0.1667(7) 0.1667(7) 0.1667 Uiso 0.371(31) 96
Si SI1 0.0 0.0936(5) 0.1867(5) 1.0 Uiso 0.0197(23) 96
Al AL1 0.0 0.1860(5) 0.0905(5) 1.0 Uiso 0.0372(27) 96
O O1 0.0 0.1108(4) 0.2485(12) 1.0 Uiso 0.0391(32) 96
O O2 0.0 0.1440(8) 0.1449(9) 1.0 Uiso 0.0297(29) 96
O O3 0.0539(5) 0.0576(5) 0.17155(15) 1.0 Uiso 0.0240(19) 192
O Ow1 0.0 0.2277(10) 0.3082(13) 0.33333 Uiso 0.094(19) 96
O Ow2 0.25 0.25 0.043(6) 0.175(17) Uiso 0.27(7) 48

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_22
_atom_site_aniso_U_23
_atom_site_aniso_U_33
NA1 0.0200(20) 0.0178(24) 0.0178(24) 0.0200(20) 0.0178(24) 0.0200(20)

_chemical_formula_sum            'Al3 Na3.00 O13.26 Si3'
_chemical_formula_weight         446.36
_cell_formula_units_Z            32

loop_
_atom_type_symbol
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
Na 96.003 0.000 0.000 4.76260 3.28500 3.17360 8.84220 1.26740 0.31360 1.11280
129.424 0.67600 International_Tables_Vol_C
Si 96.0 0.000 0.000 6.29150 2.43860 3.03530 32.3337 1.98910 0.67850 1.54100
81.6937 1.14070 International_Tables_Vol_C
Al 96.0 0.000 0.000 6.42020 3.03870 1.90020 0.74260 1.59360 31.5472 1.96460
85.0886 1.11510 International_Tables_Vol_C
O 424.396 0.000 0.000 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700
32.9089 0.25080 International_Tables_Vol_C
_diffrn_radiation_probe          x-ray
_diffrn_radiation_polarisn_ratio 0.0
_diffrn_radiation_wavelength     1.54056
_diffrn_radiation_type           Cu_K\a~1~
_pd_proc_ls_prof_R_factor        0.0401
_pd_proc_ls_prof_wR_factor       0.0543
_pd_proc_ls_prof_wR_expected     0.0211
_refine_ls_R_Fsqd_factor         0.26054

_pd_proc_ls_background_function  
; GSAS Background function number 1 with 12 terms.
Shifted Chebyshev function of 1st kind
1: 1599.23 2: -1117.99 3: 357.394 4: -42.1635
5: 169.019 6: -186.873 7: 44.8594 8: 100.134
9: -105.372 10: 33.6544 11: -2.08009 12: -2.17644
;

_exptl_absorpt_process_details   
; GSAS Absorption/surface roughness correction: function number 0
Debye-Scherrer absorption correction
Term (= MU.r/wave) = 1.8029
Correction is not refined.
;
_exptl_absorpt_correction_T_min  0.01862
_exptl_absorpt_correction_T_max  0.05313

_pd_proc_ls_profile_function     
;
CW Profile function number 3 with 19 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.
#1(GU) = 0.000 #2(GV) = -9.193 #3(GW) = 0.000
#4(GP) = 9.432 #5(LX) = 0.000 #6(LY) = 16.821
#7(S/L) = 0.0259 #8(H/L) = 0.0256
#9(trns) = -5.64 #10(shft)= -0.3134
#11(stec)= 0.00 #12(ptec)= 0.00 #13(sfec)= 0.00
#14(L11) = 0.012 #15(L22) = 0.000 #16(L33) = 0.034
#17(L12) = -0.004 #18(L13) = -0.004 #19(L23) = 0.004
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_peak_cutoff          0.00010
_pd_proc_info_datetime           2010-12-17T15:00:59
_pd_calc_method                  'Rietveld Refinement'

_pd_meas_2theta_range_min        3.0
_pd_meas_2theta_range_max        67.49
_pd_meas_2theta_range_inc        0.01
_pd_proc_2theta_range_min        3.00069
_pd_proc_2theta_range_max        67.49069
_pd_proc_2theta_range_inc        0.01

_pd_meas_number_of_points        6450
_pd_proc_number_of_points        6450

loop_
_refln_index_h
_refln_index_k
_refln_index_l
_refln_observed_status
_refln_F_squared_meas
_refln_F_squared_calc
_refln_phase_calc
_refln_d_spacing
_gsas_i100_meas
2 0 0 o 1501043.6 1489164.6 0.00 12.29010 100.00
2 2 0 o 930642.8 911707.3 180.00 8.69042 62.49
2 2 2 o 759919.2 749228.0 180.00 7.09569 23.03
4 0 0 o 10324.843 8057.344 0.00 6.14505 0.18
4 2 0 o 556947.3 554751.7 180.00 5.49630 30.72
4 2 2 o 29678.170 26086.391 0.00 5.01741 1.37
4 4 0 o 145306.44 133174.97 180.00 4.34521 2.57
6 0 0 o 206749.75 214269.52 0.00 4.09670 1.64
4 4 2 o 376452.4 388465.8 0.00 4.09670 11.92
5 3 1 o 13876.586 14335.107 0.00 4.15481 0.92
6 2 0 o 4.124 0.052 0.00 3.88647 0.00
6 2 2 o 923255.5 917603.3 0.00 3.70561 24.02
4 4 4 o 74499.76 52953.18 180.00 3.54785 0.59
6 4 0 o 41524.87 43352.51 180.00 3.40866 0.94
6 4 2 o 305008.03 323608.41 0.00 3.28467 12.64
7 3 1 o 106.811 68.260 180.00 3.20007 0.00
8 0 0 o 29870.822 19558.391 0.00 3.07253 0.13
8 2 0 o 541751.3 553734.8 180.00 2.98079 9.30
6 4 4 o 490603.3 501082.3 180.00 2.98079 8.40
8 2 2 o 137717.33 137632.42 180.00 2.89681 2.25
6 6 0 o 116086.54 118379.27 180.00 2.89681 0.95
7 5 1 o 2935.522 1760.053 180.00 2.83828 0.09
6 6 2 o 25848.717 23574.754 0.00 2.81954 0.41
8 4 0 o 179895.89 142073.69 180.00 2.74815 2.62
7 5 3 o 2847.457 2009.088 0.00 2.69803 0.08
8 4 2 o 54859.66 49829.58 0.00 2.68192 1.52
6 6 4 o 960761.4 949192.1 180.00 2.62026 12.72
9 3 1 o 16.278 10.391 180.00 2.57671 0.00
8 4 4 o 101949.38 116661.38 0.00 2.50871 1.27
10 0 0 o 1215207.3 1411600.4 0.00 2.45802 3.61
8 6 0 o 3297.776 3775.346 180.00 2.45802 0.04
10 2 0 o 2867.421 2992.216 180.00 2.41029 0.03
6 6 6 o 419711.8 610781.8 180.00 2.36523 1.57
8 6 2 o 2834.722 2890.720 0.00 2.41029 0.08
10 2 2 o 10033.894 14538.256 180.00 2.36523 0.12
9 5 1 o 420.548 795.754 180.00 2.37626 0.01
9 5 3 o 2.152 254.859 0.00 2.29212 0.00
10 4 0 o 35813.88 62759.48 180.00 2.28221 0.35
8 6 4 o 4247.005 8127.371 0.00 2.28222 0.10
10 4 2 o 63916.20 34855.402 0.00 2.24386 1.15
10 4 4 o 349824.34 326105.13 0.00 2.13943 2.85
11 3 1 o 2379.062 2033.783 180.00 2.14758 0.04
8 8 0 o 646554.8 561809.3 0.00 2.17260 2.70
9 7 1 o 146.109 129.068 0.00 2.14758 0.00
8 8 2 o 5714.003 5285.443 0.00 2.13943 0.04
8 6 6 o 205732.66 217034.11 0.00 2.10774 1.64
10 6 0 o 157829.77 166197.78 180.00 2.10774 1.23
9 7 3 o 1288.686 1151.473 180.00 2.08487 0.02
10 6 2 o 124688.58 119137.07 180.00 2.07741 1.88
12 0 0 o 2094023.6 2053282.3 0.00 2.04835 3.93
8 8 4 o 60030.95 59163.74 0.00 2.04835 0.46
12 2 0 o 48820.22 29449.951 0.00 2.02048 0.34
11 5 1 o 2972.478 2305.957 0.00 2.02734 0.04
10 6 4 o 5002.442 2712.573 0.00 1.99372 0.07
12 2 2 o 122.980 38.718 0.00 1.99372 0.00
11 5 3 o 8037.806 9425.934 0.00 1.97433 0.11
9 7 5 o 87.285 105.396 180.00 1.97433 0.00
12 4 0 o 30472.000 23418.947 180.00 1.94324 0.19
8 8 6 o 273580.44 288637.38 0.00 1.91939 1.74
12 4 2 o 3185.937 3356.986 0.00 1.91939 0.04
10 8 0 o 185489.00 196950.59 0.00 1.91939 1.14
10 6 6 o 2687.578 13376.047 0.00 1.87422 0.01
11 7 1 o 26.100 37.225 0.00 1.87970 0.00
10 8 2 o 202860.16 197508.03 180.00 1.89640 2.48
12 4 4 o 17147.744 5256.953 180.00 1.85280 0.09
13 3 1 o 87.025 189.435 0.00 1.83721 0.00
11 7 3 o 620.615 1319.265 180.00 1.83721 0.01
10 8 4 o 39713.74 61297.75 180.00 1.83210 0.45
12 6 0 o 2495.063 3614.234 180.00 1.83210 0.01
12 6 2 o 135.921 932.469 180.00 1.81208 0.00
8 8 8 o -96.796 352.046 0.00 1.77392 0.00
14 0 0 o 32467.998 33805.063 180.00 1.75573 0.04
13 5 1 o 805.738 1626.294 180.00 1.76023 0.01
11 7 5 o 1779.917 3455.491 180.00 1.76023 0.02
14 2 0 o 384883.4 370320.0 180.00 1.73808 1.78
10 8 6 o 21411.432 20607.160 180.00 1.73808 0.20
12 6 4 o 7338.767 7438.818 180.00 1.75573 0.07
14 2 2 o 128393.48 87777.41 180.00 1.72096 0.57
13 5 3 o 2889.035 2392.870 180.00 1.72519 0.03
10 10 0 o 2075097.5 1998949.6 0.00 1.73808 4.84
11 9 1 o 149.510 123.425 180.00 1.72519 0.00
14 4 0 o 44840.13 45471.63 180.00 1.68818 0.19
10 10 2 o 29688.471 19698.586 0.00 1.72096 0.13
12 8 0 o 3772.131 4095.334 180.00 1.70433 0.02
11 9 3 o 251.755 251.471 180.00 1.69217 0.00
14 4 2 o 34558.945 36521.79 0.00 1.67247 0.29
12 6 6 o 69611.64 73563.72 0.00 1.67247 0.28
12 8 2 o 232362.44 235517.06 180.00 1.68818 1.96
10 10 4 o 1853.971 1934.734 0.00 1.67247 0.01
13 7 1 o 2443.450 3414.944 0.00 1.66098 0.02
14 4 4 o 35230.69 35322.16 180.00 1.62786 0.12
10 8 8 o 350326.88 351740.9 180.00 1.62786 1.28
12 8 4 o 59251.28 45197.69 180.00 1.64233 0.44
11 9 5 o 76.618 96.152 180.00 1.63145 0.00
13 7 3 o 1735.197 2005.659 180.00 1.63145 0.01
15 3 1 o 169.956 158.628 180.00 1.60344 0.00
14 6 0 o 113694.91 110276.30 0.00 1.61377 0.39
10 10 6 o 5609.071 5381.448 180.00 1.60004 0.02
14 6 2 o 382252.8 365689.5 0.00 1.60004 2.60
13 7 5 o 5231.161 4557.528 0.00 1.57682 0.03
12 8 6 o 72682.83 64524.03 0.00 1.57359 0.46
14 6 4 o 483.019 605.548 180.00 1.56084 0.00
11 9 7 o 1633.574 2000.599 0.00 1.55149 0.01
15 5 1 o 213.159 263.023 180.00 1.55149 0.00
16 0 0 o 392273.2 401466.3 0.00 1.53626 0.28
12 10 2 o 8499.486 10548.781 180.00 1.56084 0.05
12 10 0 o 445556.6 394349.1 0.00 1.57359 1.43
16 2 0 o 939.315 616.435 0.00 1.52440 0.00
13 9 1 o 43.776 50.427 0.00 1.55149 0.00
15 5 3 o 249.840 193.094 0.00 1.52734 0.00
16 2 2 o 27057.344 23416.615 0.00 1.51281 0.07
10 10 8 o 96141.25 83864.96 180.00 1.51281 0.25
14 6 6 o 93.817 788.219 0.00 1.50148 0.00
13 9 3 o 6854.889 5159.182 180.00 1.52734 0.04
14 8 2 o 16.857 14.772 0.00 1.51281 0.00
14 8 0 o 100698.41 67014.18 180.00 1.52440 0.28
12 10 4 o 481.318 332.097 0.00 1.52440 0.00
16 4 0 o 5097.263 9066.788 180.00 1.49039 0.01
12 8 8 o 11145.285 20897.170 180.00 1.49039 0.03
16 4 2 o 68061.74 61519.93 0.00 1.47955 0.32
15 7 1 o 1303.239 1673.056 0.00 1.48224 0.01
13 9 5 o 6075.964 7762.876 0.00 1.48224 0.03
14 8 4 o 66706.04 59166.53 0.00 1.47955 0.32
12 10 6 o 51012.73 50457.33 0.00 1.46895 0.23
15 7 3 o -32.414 797.062 180.00 1.46114 0.00
16 4 4 o 131255.75 166043.56 180.00 1.44840 0.28
10 10 10 o 1025646.1 801159.7 0.00 1.41914 0.64
16 6 0 o 2755.488 4533.826 180.00 1.43845 0.01
17 3 1 o 786.497 686.624 0.00 1.42151 0.00
14 8 6 o 164673.70 142802.44 0.00 1.42870 0.65
16 6 2 o 65435.50 56729.42 0.00 1.42870 0.25
12 12 0 o 75231.21 86282.43 0.00 1.44840 0.08
13 9 7 o 990.965 870.183 0.00 1.42151 0.00
15 7 5 o 377.370 330.879 0.00 1.42151 0.00
13 11 1 o 512.705 1522.564 0.00 1.44092 0.00
14 10 0 o 150672.94 128886.85 180.00 1.42870 0.29
12 12 2 o 42221.42 62659.91 180.00 1.43845 0.09
12 10 8 o 16366.766 11711.298 180.00 1.40059 0.06
13 11 3 o 1396.637 1218.601 180.00 1.42151 0.01
14 10 2 o 99739.61 74675.00 180.00 1.41914 0.37
16 6 4 o 683599.5 490667.6 180.00 1.40059 2.34
12 12 4 o 29322.273 54509.71 180.00 1.40977 0.05
14 10 4 o -127.698 9607.282 0.00 1.39158 0.00
15 9 1 o 292.886 219.857 0.00 1.40287 0.00
_reflns_number_total             144
_reflns_limit_h_min              2
_reflns_limit_h_max              19
_reflns_limit_k_min              0
_reflns_limit_k_max              12
_reflns_limit_l_min              0
_reflns_limit_l_max              10
_reflns_d_resolution_high        1.392
_reflns_d_resolution_low         12.290
_chemical_name_common            'Zeolite A'
#--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--#

# Attachment 'ZeoliteX_final.cif'

data_phase_1
_database_code_depnum_ccdc_archive 'CCDC 831423'
#TrackingRef 'ZeoliteX_final.cif'

_pd_block_id                     2010-12-13T09:45|phase1|ZeoliteX||

loop_
_pd_block_diffractogram_id
2010-12-13T09:45|ZeoliteX|STOE_STADI_MP

_pd_phase_name                   'Zeolite X'
_cell_length_a                   25.13303(28)
_cell_length_b                   25.13303
_cell_length_c                   25.13303
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_volume                     15875.8(5)
_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   'F d -3'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
Na Na1 0.04929(25) 0.04929(25) 0.04929(25) 0.904(8) Uiso 0.027(5) 32
Na Na2 0.23234(24) 0.23234(24) 0.23234(24) 0.898(9) Uiso 0.010(5) 32
Na Na3 0.4187(14) 0.0840(22) 0.0694(18) 0.181(6) Uiso 0.040(19) 96
K K 0.4216(8) 0.0300(9) 0.0608(9) 0.225(3) Uiso 0.041(11) 96
Si Si -0.0562(6) 0.1241(6) 0.0360(6) 1.0 Uiso 0.005(4) 96
Al Al -0.0540(7) 0.0360(7) 0.1250(7) 1.0 Uiso 0.026(5) 96
O O1 -0.1116(9) -0.0053(10) 0.1100(8) 1.0 Uiso 0.023(4) 96
O O2 0.0033(8) -0.0023(8) 0.1443(4) 1.0 Uiso 0.015(5) 96
O O3 -0.03268(34) 0.0759(10) 0.0725(10) 1.0 Uiso 0.014(5) 96
O O4 -0.0721(4) 0.0704(10) 0.1847(9) 1.0 Uiso 0.039(5) 96

loop_
_atom_type_symbol
_atom_type_number_in_cell
Na 75.043
Si 96.0
Al 96.0
O 384.0
K 21.557

_chemical_formula_sum            'Al K0.22 Na0.78 O4 Si'
_chemical_formula_weight         145.81
_cell_formula_units_Z            96
_chemical_name_common            'Zeolite X'

data_phase_2
_database_code_depnum_ccdc_archive 'CCDC 831424'
#TrackingRef 'ZeoliteX_final.cif'

_pd_block_id                     2010-12-13T09:45|phase2|ZeoliteA||

loop_
_pd_block_diffractogram_id
2010-12-13T09:45|ZeoliteX|STOE_STADI_MP

_pd_phase_name                   ZeoliteA
_cell_length_a                   24.5228(35)
_cell_length_b                   24.5228
_cell_length_c                   24.5228
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_volume                     14747(6)
_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   'F m -3 c'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
Na NA1 0.1040(27) 0.1040(27) 0.1040(27) 1.0 Uiso 0.09(5) 64
Na NA2 0.0 0.25 0.25 0.66666 Uiso 0.17(32) 24
Na NA3 0.25 0.170(11) 0.170(11) 0.1667 Uiso 0.6(8) 96
Si SI1 0.0 0.102(4) 0.190(6) 1.0 Uiso 0.004(29) 96
Al AL1 0.0 0.186(4) 0.0775(32) 1.0 Uiso 0.012(31) 96
O O1 0.0 0.118(8) 0.256(10) 1.0 Uiso 0.07(8) 96
O O2 0.0 0.144(8) 0.149(8) 1.0 Uiso 0.05(9) 96
O O3 0.056(5) 0.054(5) 0.1707(34) 1.0 Uiso 0.01(5) 192
O Ow1 0.0 0.221(24) 0.338(17) 0.4422 Uiso 0.18(32) 96

loop_
_atom_type_symbol
_atom_type_number_in_cell
Na 96.003
Si 96.0
Al 96.0
O 426.451

_chemical_formula_sum            'Al3 Na3.00 O13.33 Si3'
_chemical_formula_weight         447.39
_cell_formula_units_Z            32
_chemical_name_common            ZeoliteA