#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/51/1505104.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1505104
loop_
_publ_author_name
'Schmidt, Wolfgang'
'Wilczok, Ursula'
'Weidenthaler, Claudia'
'Medenbach, Olaf'
'Goddard, Richard'
'Buth, Gernot'
'Cepak, Alexander'
_publ_section_title
;
 Preparation and morphology of pyramidal MFI single-crystal segments.
;
_journal_issue                   48
_journal_name_full               'The journal of physical chemistry. B'
_journal_page_first              13538
_journal_page_last               13543
_journal_paper_doi               10.1021/jp075934p
_journal_volume                  111
_journal_year                    2007
_chemical_compound_source        'reaction solution'
_chemical_formula_moiety         '(O2 Si)24, C12 H28 N 1+, O H 1-'
_chemical_formula_sum            'C12 H29 N O49 Si24'
_chemical_formula_weight         1645.52
_chemical_melting_point          ?
_chemical_name_common            TPA-Silicalite-1
_chemical_name_systematic
; 
 catena-(octatetraconta-oxa-tricosa-silicon 
 tetra-n-propyl-ammonium hydroxide)
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                WUM-UA-038-02
_audit_creation_date             2007-05-15
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   20.0578(4)
_cell_length_b                   19.9466(4)
_cell_length_c                   13.4070(3)
_cell_measurement_reflns_used    4824
_cell_measurement_temperature    293
_cell_measurement_theta_max      53.13
_cell_measurement_theta_min      3.97
_cell_volume                     5363.94(19)
_computing_cell_refinement       'Proteum software (Bruker-AXS, 2005)'
_computing_data_collection       'Proteum software (Bruker-AXS, 2005)'
_computing_data_reduction        'Proteum software (Bruker-AXS, 2005)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'Bruker-AXS X8-Proteum'
_diffrn_measurement_method       'CCD π and ω-scans'
_diffrn_radiation_monochromator  'Montel coated mirrors'
_diffrn_radiation_source         '0.2 mm focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54188
_diffrn_reflns_av_R_equivalents  0.1280
_diffrn_reflns_av_sigmaI/netI    0.0746
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            79163
_diffrn_reflns_theta_full        68.85
_diffrn_reflns_theta_max         68.85
_diffrn_reflns_theta_min         3.97
_diffrn_standards_decay_%        0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.521
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6548
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker AXS (2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.038
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             3344
_exptl_crystal_size_max          0.045
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.028
_refine_diff_density_max         0.882
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.169
_refine_ls_extinction_coef       0.00028(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         4840
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1166
_refine_ls_R_factor_gt           0.0663
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1278P)²+11.3746P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1826
_refine_ls_wR_factor_ref         0.2308
_reflns_number_gt                2811
_reflns_number_total             4840
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            jp075934p_tpasilicalite1_1030.cif
_cod_data_source_block           TPA-Silicalite-1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not determined' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               1505104
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Si1 Si 0.22569(6) -0.17386(5) 0.02797(8) 0.0311(3) Uani 1 1 d .
Si2 Si -0.07712(6) -0.05774(5) 0.33753(8) 0.0268(3) Uani 1 1 d .
Si3 Si 0.19186(6) -0.12869(5) -0.18779(8) 0.0263(3) Uani 1 1 d .
Si4 Si 0.07131(6) 0.13079(5) 0.31678(8) 0.0257(3) Uani 1 1 d .
Si5 Si -0.07674(5) 0.17251(5) 0.32743(8) 0.0254(3) Uani 1 1 d .
Si6 Si 0.22011(6) 0.06133(5) 0.02942(8) 0.0263(3) Uani 1 1 d .
Si7 Si 0.12245(6) -0.06296(5) 0.52639(8) 0.0245(3) Uani 1 1 d .
Si8 Si -0.12096(6) -0.17366(5) 0.47111(9) 0.0297(3) Uani 1 1 d .
Si9 Si 0.30731(6) -0.02927(6) 0.30770(8) 0.0280(3) Uani 1 1 d .
Si10 Si 0.18564(6) -0.06006(5) 0.16923(8) 0.0266(3) Uani 1 1 d .
Si11 Si 0.18714(6) 0.17307(5) 0.17825(8) 0.0261(3) Uani 1 1 d .
Si12 Si 0.07171(6) -0.02713(5) 0.31376(8) 0.0248(3) Uani 1 1 d .
O1 O -0.1086(2) -0.2500 0.4379(3) 0.0340(11) Uani 1 2 d S
O2 O 0.11442(14) -0.05458(14) 0.2223(2) 0.0391(8) Uani 1 1 d .
O3 O 0.19403(15) 0.12984(13) 0.0779(2) 0.0413(9) Uani 1 1 d .
O4 O 0.1902(2) 0.2500 0.1461(3) 0.0441(13) Uani 1 2 d S
O5 O 0.18741(14) -0.13034(14) 0.1130(2) 0.0382(9) Uani 1 1 d .
O6 O -0.00379(14) -0.04830(14) 0.2930(2) 0.0394(9) Uani 1 1 d .
O7 O 0.2089(2) -0.2500 0.0583(3) 0.0404(12) Uani 1 2 d S
O8 O 0.24303(16) -0.05605(15) 0.2515(2) 0.0496(10) Uani 1 1 d .
O9 O -0.00364(14) 0.15144(15) 0.2925(2) 0.0423(9) Uani 1 1 d .
O10 O 0.19242(15) -0.00022(14) 0.0907(2) 0.0471(9) Uani 1 1 d .
O11 O 0.11654(14) 0.15859(15) 0.2284(2) 0.0456(9) Uani 1 1 d .
O12 O -0.07912(16) -0.12793(14) 0.3944(2) 0.0466(10) Uani 1 1 d .
O13 O 0.30855(15) -0.05826(14) 0.4181(2) 0.0409(9) Uani 1 1 d .
O14 O -0.12830(15) -0.05805(16) 0.2464(2) 0.0526(10) Uani 1 1 d .
O15 O 0.30293(14) -0.15178(16) 0.0377(3) 0.0496(10) Uani 1 1 d .
O16 O 0.09753(17) -0.06057(14) 0.4140(2) 0.0432(9) Uani 1 1 d .
O17 O -0.09805(17) 0.13145(14) 0.4249(2) 0.0439(9) Uani 1 1 d .
O18 O 0.19339(15) -0.15151(17) -0.0749(2) 0.0461(9) Uani 1 1 d .
O19 O 0.07828(17) 0.05193(14) 0.3216(3) 0.0545(11) Uani 1 1 d .
O20 O -0.0786(2) 0.2500 0.3553(3) 0.0451(13) Uani 1 2 d S
O21 O -0.12642(15) 0.15716(16) 0.2375(2) 0.0491(10) Uani 1 1 d .
O22 O -0.09346(17) 0.00104(14) 0.4139(2) 0.0479(9) Uani 1 1 d .
O23 O 0.24476(16) 0.15518(18) 0.2533(2) 0.0581(11) Uani 1 1 d .
O24 O 0.09341(17) 0.16188(17) 0.4193(2) 0.0585(10) Uani 1 1 d .
O25 O 0.29876(15) 0.06010(19) 0.0289(3) 0.0629(13) Uani 1 1 d .
O26 O 0.3097(2) 0.04984(15) 0.3063(3) 0.0788(15) Uani 1 1 d .
O27 O 0.2825(6) -0.2232(6) -0.0693(10) 0.167(5) Uiso 0.50 1 d P
N N -0.0199(5) -0.2500 0.1107(7) 0.109(3) Uani 1 2 d S
C1 C -0.1052(15) -0.2500 0.134(2) 0.308(14) Uiso 1 2 d S
C2 C -0.1374(16) -0.2500 0.147(3) 0.329(17) Uiso 1 2 d S
C3 C -0.2080(7) -0.2500 0.1716(12) 0.153(5) Uiso 1 2 d S
C4A C 0.045(3) -0.2500 0.207(5) 0.32(3) Uiso 0.50 2 d SP
C4B C 0.001(2) -0.2500 0.230(4) 0.219(17) Uiso 0.50 2 d SP
C5 C 0.0618(11) -0.2500 0.2596(17) 0.212(9) Uiso 1 2 d S
C6 C 0.0886(7) -0.2500 0.3598(11) 0.143(5) Uiso 1 2 d S
C7 C 0.0020(7) -0.1850(8) 0.0526(12) 0.225(6) Uiso 1 1 d .
C8A C -0.0011(12) -0.1642(13) -0.025(2) 0.180(10) Uiso 0.50 1 d P
C8B C -0.0102(13) -0.1233(14) 0.043(2) 0.186(10) Uiso 0.50 1 d P
C9 C 0.0127(5) -0.0872(5) -0.0380(8) 0.142(4) Uiso 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O18 Si1 O7 113.5(2) . . y
O18 Si1 O15 112.63(18) . . y
O7 Si1 O15 116.0(2) . . y
O18 Si1 O5 105.44(17) . . y
O7 Si1 O5 103.16(18) . . y
O15 Si1 O5 104.53(17) . . y
O18 Si1 O27 78.7(4) . . y
O7 Si1 O27 79.6(4) . . y
O15 Si1 O27 68.9(4) . . y
O5 Si1 O27 173.3(4) . . y
O22 Si2 O12 109.56(17) . . y
O22 Si2 O14 111.29(18) . . y
O12 Si2 O14 110.26(18) . . y
O22 Si2 O6 110.05(17) . . y
O12 Si2 O6 107.75(17) . . y
O14 Si2 O6 107.86(17) . . y
O26 Si3 O21 108.8(2) 2_554 5 y
O26 Si3 O18 109.6(2) 2_554 . y
O21 Si3 O18 108.49(17) 5 . y
O26 Si3 O23 108.8(2) 2_554 2_554 y
O21 Si3 O23 109.64(18) 5 2_554 y
O18 Si3 O23 111.42(18) . 2_554 y
O24 Si4 O19 109.4(2) . . y
O24 Si4 O11 110.66(18) . . y
O19 Si4 O11 109.08(18) . . y
O24 Si4 O9 110.04(18) . . y
O19 Si4 O9 110.44(18) . . y
O11 Si4 O9 107.22(16) . . y
O20 Si5 O21 110.5(2) . . y
O20 Si5 O9 110.2(2) . . y
O21 Si5 O9 107.59(17) . . y
O20 Si5 O17 107.42(19) . . y
O21 Si5 O17 110.63(17) . . y
O9 Si5 O17 110.50(17) . . y
O25 Si6 O10 110.02(19) . . y
O25 Si6 O13 110.74(19) . 2_554 y
O10 Si6 O13 109.21(17) . 2_554 y
O25 Si6 O3 109.99(19) . . y
O10 Si6 O3 109.74(17) . . y
O13 Si6 O3 107.09(16) 2_554 . y
O25 Si7 O22 109.2(2) 2 5_556 y
O25 Si7 O16 109.5(2) 2 . y
O22 Si7 O16 109.95(17) 5_556 . y
O25 Si7 O17 109.24(19) 2 5_556 y
O22 Si7 O17 110.44(17) 5_556 5_556 y
O16 Si7 O17 108.55(16) . 5_556 y
O24 Si8 O15 111.22(19) 5_556 6_556 y
O24 Si8 O1 110.1(2) 5_556 . y
O15 Si8 O1 112.8(2) 6_556 . y
O24 Si8 O12 109.01(19) 5_556 . y
O15 Si8 O12 107.28(18) 6_556 . y
O1 Si8 O12 106.23(18) . . y
O26 Si9 O8 110.8(2) . . y
O26 Si9 O14 109.4(2) . 6_656 y
O8 Si9 O14 108.80(18) . 6_656 y
O26 Si9 O13 112.0(2) . . y
O8 Si9 O13 109.42(17) . . y
O14 Si9 O13 106.31(17) 6_656 . y
O5 Si10 O8 110.82(17) . . y
O5 Si10 O10 110.09(17) . . y
O8 Si10 O10 110.90(17) . . y
O5 Si10 O2 106.91(16) . . y
O8 Si10 O2 109.47(17) . . y
O10 Si10 O2 108.55(16) . . y
O23 Si11 O11 109.99(18) . . y
O23 Si11 O4 111.3(2) . . y
O11 Si11 O4 108.8(2) . . y
O23 Si11 O3 110.55(17) . . y
O11 Si11 O3 109.44(17) . . y
O4 Si11 O3 106.70(19) . . y
O19 Si12 O16 109.53(18) . . y
O19 Si12 O2 110.38(18) . . y
O16 Si12 O2 109.39(17) . . y
O19 Si12 O6 110.69(18) . . y
O16 Si12 O6 110.22(17) . . y
O2 Si12 O6 106.58(16) . . y
Si8 O1 Si8 143.0(3) 7 . y
Si12 O2 Si10 147.8(2) . . y
Si6 O3 Si11 145.8(2) . . y
Si11 O4 Si11 148.3(3) 7_565 . y
Si10 O5 Si1 144.4(2) . . y
Si12 O6 Si2 147.1(2) . . y
Si1 O7 Si1 141.6(3) . 7 y
Si9 O8 Si10 158.7(2) . . y
Si4 O9 Si5 151.2(2) . . y
Si6 O10 Si10 162.6(2) . . y
Si4 O11 Si11 152.0(2) . . y
Si2 O12 Si8 144.6(2) . . y
Si9 O13 Si6 151.3(2) . 2 y
Si9 O14 Si2 150.6(2) 6_556 . y
Si8 O15 Si1 147.0(2) 6_656 . y
Si12 O16 Si7 156.7(2) . . y
Si7 O17 Si5 148.9(2) 5_556 . y
Si3 O18 Si1 157.0(2) . . y
Si4 O19 Si12 168.4(3) . . y
Si5 O20 Si5 152.7(3) . 7_565 y
Si3 O21 Si5 155.4(2) 5 . y
Si7 O22 Si2 167.6(2) 5_556 . y
Si11 O23 Si3 169.2(3) . 2 y
Si4 O24 Si8 165.1(3) . 5_556 y
Si6 O25 Si7 176.9(3) . 2_554 y
Si3 O26 Si9 175.4(3) 2 . y
O27 O27 Si1 119.6(3) 7 . y
C7 N C7 110.8(13) 7 . y
C7 N C4B 114.0(10) 7 . y
C7 N C4B 114.0(10) . . y
C7 N C1 111.2(8) 7 . y
C7 N C1 111.2(8) . . y
C4B N C1 94.7(19) . . y
C7 N C4A 98.7(12) 7 . y
C7 N C4A 98.7(12) . . y
C4B N C4A 30(2) . . y
C1 N C4A 125(2) . . y
C2 C1 N 175(6) . . y
C1 C2 C3 177(6) . . y
C5 C4A C4B 96(8) . . y
C5 C4A N 161(7) . . y
C4B C4A N 65(5) . . y
C4A C4B C5 38(5) . . y
C4A C4B N 85(6) . . y
C5 C4B N 123(3) . . y
C4A C5 C4B 46(5) . . y
C4A C5 C6 176(6) . . y
C4B C5 C6 130(3) . . y
C8A C7 C8B 62.2(18) . . y
C8A C7 N 139(2) . . y
C8B C7 N 143.0(18) . . y
C7 C8A C8B 65(2) . . y
C7 C8A C9 117(2) . . y
C8B C8A C9 57.6(18) . . y
C8A C8B C7 53.1(18) . . y
C8A C8B C9 73(2) . . y
C7 C8B C9 121(2) . . y
C8B C9 C8A 48.9(14) . . y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 O18 1.587(3) . y
Si1 O7 1.6081(17) . y
Si1 O15 1.616(3) . y
Si1 O5 1.625(3) . y
Si1 O27 1.992(12) . y
Si2 O22 1.590(3) . y
Si2 O12 1.594(3) . y
Si2 O14 1.596(3) . y
Si2 O6 1.598(3) . y
Si3 O26 1.575(3) 2_554 y
Si3 O21 1.578(3) 5 y
Si3 O18 1.581(3) . y
Si3 O23 1.587(3) 2_554 y
Si4 O24 1.572(3) . y
Si4 O19 1.581(3) . y
Si4 O11 1.592(3) . y
Si4 O9 1.592(3) . y
Si5 O20 1.5906(14) . y
Si5 O21 1.594(3) . y
Si5 O9 1.595(3) . y
Si5 O17 1.601(3) . y
Si6 O25 1.578(3) . y
Si6 O10 1.578(3) . y
Si6 O13 1.601(3) 2_554 y
Si6 O3 1.601(3) . y
Si7 O25 1.582(3) 2 y
Si7 O22 1.583(3) 5_556 y
Si7 O16 1.588(3) . y
Si7 O17 1.591(3) 5_556 y
Si8 O24 1.587(3) 5_556 y
Si8 O15 1.592(3) 6_556 y
Si8 O1 1.6056(16) . y
Si8 O12 1.611(3) . y
Si9 O26 1.579(3) . y
Si9 O8 1.586(3) . y
Si9 O14 1.588(3) 6_656 y
Si9 O13 1.589(3) . y
Si10 O5 1.592(3) . y
Si10 O8 1.596(3) . y
Si10 O10 1.598(3) . y
Si10 O2 1.600(3) . y
Si11 O23 1.573(3) . y
Si11 O11 1.594(3) . y
Si11 O4 1.5950(15) . y
Si11 O3 1.604(3) . y
Si12 O19 1.586(3) . y
Si12 O16 1.588(3) . y
Si12 O2 1.593(3) . y
Si12 O6 1.596(3) . y
O1 Si8 1.6056(16) 7 y
O4 Si11 1.5950(15) 7_565 y
O7 Si1 1.6082(17) 7 y
O13 Si6 1.601(3) 2 y
O14 Si9 1.589(3) 6_556 y
O15 Si8 1.592(3) 6_656 y
O17 Si7 1.591(3) 5_556 y
O20 Si5 1.5906(14) 7_565 y
O21 Si3 1.578(3) 5 y
O22 Si7 1.583(3) 5_556 y
O23 Si3 1.587(3) 2 y
O24 Si8 1.587(3) 5_556 y
O25 Si7 1.582(3) 2_554 y
O26 Si3 1.575(3) 2 y
O27 O27 1.07(2) 7 y
N C7 1.575(16) 7 y
N C7 1.575(16) . y
N C4B 1.66(5) . y
N C1 1.74(3) . y
N C4A 1.83(6) . y
C1 C2 0.67(5) . y
C2 C3 1.45(3) . y
C4A C5 0.78(7) . y
C4A C4B 0.93(7) . y
C4B C5 1.27(5) . y
C5 C6 1.45(2) . y
C7 C8A 1.12(3) . y
C7 C8B 1.26(3) . y
C8A C8B 1.23(3) . y
C8A C9 1.57(3) . y
C8B C9 1.38(3) . y
