#------------------------------------------------------------------------------
#$Date: 2017-08-31 05:13:44 +0300 (Thu, 31 Aug 2017) $
#$Revision: 200009 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/69/1546913.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_1546913
loop_
_publ_author_name
'Łukaszuk, Katarzyna Anna'
'Rojo-Gama, Daniel'
'Øien-Ødegaard, Sigurd'
'Lazzarini, Andrea'
'Berlier, Gloria'
'Bordiga, Silvia'
'Lillerud, Karl Petter'
'Olsbye, Unni'
'Beato, Pablo'
'Lundegaard, Lars Fahl'
'Svelle, Stian'
_publ_section_title
;
 Zeolite morphology and catalyst performance: Conversion of methanol to
 hydrocarbons over offretite
;
_journal_name_full               'Catal. Sci. Technol.'
_journal_paper_doi               10.1039/C7CY00996H
_journal_year                    2017
_chemical_formula_moiety         'K1 O36 Si18, 2(C2.5 O0.5), 9(C), 3(O)'
_chemical_formula_sum            'C14 K O40 Si18'
_chemical_formula_weight         1352.86
_chemical_name_common            Offretite
_space_group_crystal_system      hexagonal
_space_group_IT_number           187
_space_group_name_Hall           'P -6 2'
_space_group_name_H-M_alt        'P -6 m 2'
_symmetry_space_group_name_Hall  'P -6 2'
_symmetry_space_group_name_H-M   'P -6 m 2'
_atom_sites_solution_primary     dual
_audit_creation_date             2017-05-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   13.2558(3)
_cell_length_b                   13.2558(3)
_cell_length_c                   7.5358(2)
_cell_measurement_reflns_used    2330
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      30.890
_cell_measurement_theta_min      3.244
_cell_volume                     1146.76(5)
_computing_cell_refinement       'APEX3 (Bruker AXS, 2016)'
_computing_data_collection       'APEX3 (Bruker AXS, 2016)'
_computing_data_reduction        'APEX3 (Bruker AXS, 2016)'
_computing_molecular_graphics    'Diamond v4 (Brandenburg, 2012)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      273.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 13.6986
_diffrn_detector_type            'Marmosaic 225'
_diffrn_measured_fraction_theta_full 0.859
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'MD2 microdiffractometer with MK3 mini-kappa'
_diffrn_measurement_method       'φ scans'
_diffrn_radiation_collimation    'Rh-coated Si focusing mirrors'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.750
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.859
_diffrn_reflns_Laue_measured_fraction_max 0.883
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3006
_diffrn_reflns_point_group_measured_fraction_full 0.877
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.891
_diffrn_reflns_theta_min         3.243
_diffrn_source                   synchrotron
_diffrn_source_type              'Wiggler, Station I911-3, MAX II, MAXLAB'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.817
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6502
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0859 before and 0.0729 after correction. The Ratio of minimum to maximum transmission is 0.8715. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.959
_exptl_crystal_description       prism
_exptl_crystal_F_000             675
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details
;
 Flack x determined using 428 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.24(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     77
_refine_ls_number_reflns         1065
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0871P)²+0.8372P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1322
_reflns_Friedel_coverage         0.908
_reflns_Friedel_fraction_full    0.896
_reflns_Friedel_fraction_max     0.916
_reflns_number_gt                1009
_reflns_number_total             1065
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7cy00996h5.cif
_cod_data_source_block           OFF-O-2
_cod_original_cell_volume        1146.76(6)
_cod_database_code               1546913
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.4(2)
 0.6(2)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-y, -x, -z'
'-x+y, y, -z'
'x, x-y, -z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
K001 K 0.0000 0.0000 0.5000 0.0169(6) Uani 1 12 d S T P
Si02 Si 0.23336(9) 0.23391(9) 0.78994(16) 0.0104(3) Uani 1 1 d . . .
Si03 Si 0.33161(14) 0.42469(12) 0.5000 0.0098(4) Uani 1 2 d S T P
O004 O 0.2295(3) 0.4590(6) 0.5000 0.0194(13) Uani 1 4 d S T P
O005 O 0.4590(3) 0.5410(3) 0.5000 0.0232(15) Uani 1 4 d S T P
O006 O 0.2613(4) 0.2642(4) 1.0000 0.0185(8) Uani 1 2 d S T P
O007 O 0.09790(19) 0.1958(4) 0.7416(7) 0.0167(8) Uani 1 2 d S T P
O008 O 0.2543(5) 0.1271(2) 0.7288(8) 0.0226(10) Uani 1 2 d S T P
O009 O 0.3244(3) 0.3508(3) 0.6796(5) 0.0219(7) Uani 1 1 d . . .
O00A O 0.3333 0.6667 0.0000 0.064(5) Uani 1 12 d S T P
C2 C 0.5563(11) 0.4437(11) 0.772(4) 0.112(8) Uani 1 2 d S T P
C3 C 0.502(3) 0.498(3) 1.0000 0.19(2) Uani 1 4 d S T P
C4 C 0.2632(16) 0.526(3) 0.0000 0.125(12) Uani 1 4 d S T P
C0AA C 0.3333 0.6667 0.220(12) 0.20(4) Uani 1 6 d S T P
O1 O 0.478(5) 0.239(2) 0.5000 0.25(2) Uani 1 4 d S T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2270 0.2950 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0130 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0900 0.0790 '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
O007 K001 O007 134.27(7) . 5_556
O007 K001 O007 84.60(15) 6_556 4_556
O007 K001 O007 134.27(7) 6_556 2
O007 K001 O007 134.27(7) . 6_556
O007 K001 O007 84.60(15) . 2
O007 K001 O007 84.60(15) 5_556 6_556
O007 K001 O007 84.60(15) 5_556 4_556
O007 K001 O007 84.60(15) . 3
O007 K001 O007 134.27(7) 3 4_556
O007 K001 O007 134.27(7) 5_556 3
O007 K001 O007 78.0(2) 5_556 2
O007 K001 O007 78.0(2) 6_556 3
O007 K001 O007 84.60(15) 3 2
O007 K001 O007 78.0(2) . 4_556
O007 K001 O007 134.27(7) 4_556 2
O007 K001 O008 49.11(5) 3 .
O007 K001 O008 89.17(10) 6_556 3
O007 K001 O008 49.11(5) . .
O007 K001 O008 110.43(15) 2 .
O007 K001 O008 89.17(10) 4_556 2
O007 K001 O008 49.11(5) 5_556 6_556
O007 K001 O008 89.17(10) 6_556 .
O007 K001 O008 89.17(10) 3 6_556
O007 K001 O008 171.57(13) 4_556 3
O007 K001 O008 89.17(10) 2 6_556
O007 K001 O008 49.11(5) 2 2
O007 K001 O008 110.43(15) 5_556 4_556
O007 K001 O008 171.57(13) 5_556 .
O007 K001 O008 89.17(10) 3 4_556
O007 K001 O008 110.43(15) . 3
O007 K001 O008 89.17(10) 4_556 .
O007 K001 O008 89.17(10) . 5_556
O007 K001 O008 171.57(13) . 6_556
O007 K001 O008 49.11(5) 5_556 5_556
O007 K001 O008 49.11(5) 6_556 6_556
O007 K001 O008 110.43(15) 6_556 5_556
O007 K001 O008 110.43(15) 4_556 6_556
O007 K001 O008 171.57(13) 3 5_556
O007 K001 O008 89.17(10) . 4_556
O007 K001 O008 49.11(5) 4_556 5_556
O007 K001 O008 49.11(5) 6_556 4_556
O007 K001 O008 89.17(10) 2 5_556
O007 K001 O008 49.11(5) 4_556 4_556
O007 K001 O008 49.11(5) . 2
O007 K001 O008 89.17(10) 5_556 3
O007 K001 O008 89.17(10) 5_556 2
O007 K001 O008 49.11(5) 3 3
O007 K001 O008 171.57(13) 6_556 2
O007 K001 O008 49.11(5) 2 3
O007 K001 O008 110.43(15) 3 2
O007 K001 O008 171.57(13) 2 4_556
O008 K001 O008 96.43(13) 5_556 4_556
O008 K001 O008 96.43(13) 5_556 6_556
O008 K001 O008 96.43(13) . 3
O008 K001 O008 129.00(6) 2 4_556
O008 K001 O008 129.00(5) 5_556 3
O008 K001 O008 61.14(19) . 4_556
O008 K001 O008 96.43(13) 2 .
O008 K001 O008 96.43(13) 6_556 4_556
O008 K001 O008 129.00(6) 2 6_556
O008 K001 O008 129.00(5) . 6_556
O008 K001 O008 96.43(13) 2 3
O008 K001 O008 61.14(19) 5_556 2
O008 K001 O008 129.00(5) 4_556 3
O008 K001 O008 129.00(5) 5_556 .
O008 K001 O008 61.14(19) 6_556 3
O006 Si02 K001 138.90(17) . .
O006 Si02 O007 111.7(3) . .
O006 Si02 O008 111.7(3) . .
O006 Si02 O009 106.9(2) . .
O007 Si02 K001 45.72(15) . .
O008 Si02 K001 63.4(2) . .
O008 Si02 O007 107.6(3) . .
O009 Si02 K001 113.28(14) . .
O009 Si02 O007 110.7(2) . .
O009 Si02 O008 108.2(2) . .
O004 Si03 O009 110.93(17) . .
O004 Si03 O009 110.93(17) . 4_556
O005 Si03 O004 110.5(4) . .
O005 Si03 O009 106.81(19) . 4_556
O005 Si03 O009 106.81(19) . .
O009 Si03 O009 110.7(3) . 4_556
Si03 O004 Si03 152.0(5) 8 .
Si03 O005 Si03 170.9(5) 7_665 .
Si02 O006 Si02 152.5(3) . 4_557
Si02 O007 K001 110.26(15) 8 .
Si02 O007 K001 110.26(15) . .
Si02 O007 Si02 139.5(3) . 8
Si02 O008 K001 91.0(2) . .
Si02 O008 K001 91.0(2) 9 .
Si02 O008 Si02 143.0(4) . 9
Si02 O009 Si03 141.0(2) . .
C4 O00A C4 120.000(4) 3_565 2_665
C4 O00A C4 120.000(1) . 2_665
C4 O00A C4 120.000(1) 3_565 .
C4 O00A C0AA 90.000(6) 3_565 .
C4 O00A C0AA 90.000(15) 2_665 .
C4 O00A C0AA 90.001(15) 2_665 4
C4 O00A C0AA 90.000(9) . .
C4 O00A C0AA 90.001(9) . 4
C4 O00A C0AA 89.998(6) 3_565 4
C0AA O00A C0AA 180.0 4 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K001 O007 2.892(5) .
K001 O007 2.892(5) 4_556
K001 O007 2.892(5) 3
K001 O007 2.892(5) 5_556
K001 O007 2.892(5) 6_556
K001 O007 2.892(5) 2
K001 O008 3.390(6) 2
K001 O008 3.390(6) 3
K001 O008 3.390(6) 4_556
K001 O008 3.390(6) .
K001 O008 3.390(6) 6_556
K001 O008 3.390(6) 5_556
Si02 O006 1.6296(17) .
Si02 O007 1.6448(19) .
Si02 O008 1.639(2) .
Si02 O009 1.637(3) .
Si03 O004 1.629(2) .
Si03 O005 1.6203(17) .
Si03 O009 1.645(3) 4_556
Si03 O009 1.645(3) .
O004 Si03 1.629(2) 8
O005 Si03 1.6203(17) 7_665
O006 Si02 1.6296(16) 4_557
O007 Si02 1.6448(19) 8
O008 Si02 1.639(2) 9
O00A C4 1.61(4) 3_565
O00A C4 1.61(4) 2_665
O00A C4 1.61(4) .
O00A C0AA 1.66(9) 4
O00A C0AA 1.66(9) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
K001 Si02 O006 Si02 4.8(10) . 4_557
K001 Si02 O007 Si02 179.1(7) . 8
K001 Si02 O008 Si02 -92.9(6) . 9
K001 Si02 O009 Si03 27.2(4) . .
O004 Si03 O009 Si02 55.2(5) . .
O005 Si03 O004 Si03 180.0 . 8
O005 Si03 O009 Si02 175.7(4) . .
O006 Si02 O007 K001 -138.1(2) . .
O006 Si02 O007 Si02 41.0(6) . 8
O006 Si02 O008 K001 135.0(2) . .
O006 Si02 O008 Si02 42.1(7) . 9
O006 Si02 O009 Si03 -144.1(4) . .
O007 Si02 O006 Si02 51.4(8) . 4_557
O007 Si02 O008 K001 12.1(3) . .
O007 Si02 O008 Si02 -80.8(7) . 9
O007 Si02 O009 Si03 -22.3(4) . .
O008 Si02 O006 Si02 -69.2(8) . 4_557
O008 Si02 O007 K001 -15.2(3) . .
O008 Si02 O007 Si02 164.0(5) . 8
O008 Si02 O009 Si03 95.4(4) . .
O009 Si02 O006 Si02 172.7(7) . 4_557
O009 Si02 O007 K001 102.8(2) . .
O009 Si02 O007 Si02 -78.0(5) . 8
O009 Si02 O008 K001 -107.52(18) . .
O009 Si02 O008 Si02 159.6(6) . 9
O009 Si03 O004 Si03 -61.72(16) . 8
O009 Si03 O004 Si03 61.72(16) 4_556 8
O009 Si03 O009 Si02 -68.4(5) 4_556 .
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.4(2)
2 0.6(2)
