#------------------------------------------------------------------------------
#$Date: 2017-08-31 05:13:32 +0300 (Thu, 31 Aug 2017) $
#$Revision: 200008 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/69/1546912.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_1546912
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         'K0.08 O3 Si1.5, C0.42 O0.08, C'
_chemical_formula_sum            'C0.75 K0.08 O3.52 Si1.5'
_chemical_formula_weight         110.73
_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             2017-04-28
_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            12
_cell_length_a                   13.265(3)
_cell_length_b                   13.265(3)
_cell_length_c                   7.545(2)
_cell_measurement_reflns_used    954
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      26.731
_cell_measurement_theta_min      3.241
_cell_volume                     1149.8(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    'Olex2 (Dolomanov et al., 2009)'
_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 0.817
_diffrn_measured_fraction_theta_max 0.814
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  I911-3
_diffrn_measurement_method       'ω and 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  0.0951
_diffrn_reflns_av_unetI/netI     0.0722
_diffrn_reflns_Laue_measured_fraction_full 0.817
_diffrn_reflns_Laue_measured_fraction_max 0.814
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4260
_diffrn_reflns_point_group_measured_fraction_full 0.831
_diffrn_reflns_point_group_measured_fraction_max 0.829
_diffrn_reflns_theta_full        26.744
_diffrn_reflns_theta_max         26.883
_diffrn_reflns_theta_min         1.871
_diffrn_source                   synchrotron
_diffrn_source_type              'Wiggler, Station I911-3, MAX II, MAXLAB'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.815
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1109 before and 0.0813 after correction. The Ratio of minimum to maximum transmission is 0.6622. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.919
_exptl_crystal_description       prism
_exptl_crystal_F_000             663
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details
;
 Flack x determined using 215 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.08(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     77
_refine_ls_number_reflns         694
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0569
_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)+(0.0907P)²+0.9721P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1470
_refine_ls_wR_factor_ref         0.1626
_reflns_Friedel_coverage         0.895
_reflns_Friedel_fraction_full    0.848
_reflns_Friedel_fraction_max     0.846
_reflns_number_gt                553
_reflns_number_total             694
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7cy00996h4.cif
_cod_data_source_block           OFF-O-1
_cod_original_cell_volume        1149.7(6)
_cod_original_formula_sum        'C0.75 K0.08 O3.52 Si1.50'
_cod_database_code               1546912
_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: 0.7(4)
 0.3(4)
2. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C00C) \\sim Ueq, Uanis(C0AA) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.05
;
_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 0.6667 0.3333 0.0000 0.024(2) Uani 1 12 d S T P
Si02 Si 0.5735(3) 0.6652(4) 0.0000 0.0180(13) Uani 1 2 d S T P
Si03 Si 0.6665(3) 0.5670(2) 0.2903(5) 0.0184(9) Uani 1 1 d . . .
O004 O 0.5847(13) 0.7923(6) 0.0000 0.031(6) Uani 1 4 d S T P
O005 O 0.4371(7) 0.5629(7) 0.0000 0.025(5) Uani 1 4 d S T P
O006 O 0.6627(10) 0.5937(9) 0.5000 0.023(3) Uani 1 2 d S T P
O007 O 0.6397(5) 0.6571(6) 0.1766(13) 0.029(2) Uani 1 1 d . . .
O008 O 0.5682(5) 0.4318(5) 0.244(2) 0.028(4) Uani 1 2 d S T P
O009 O 0.7939(5) 0.5878(10) 0.229(2) 0.030(4) Uani 1 2 d S T P
O00A O 0.3333 0.6667 0.5000 0.087(17) Uani 1 12 d S T P
C00B C 0.907(3) 0.814(6) 0.0000 0.15(3) Uani 1 4 d S T P
C00C C 0.404(2) 0.596(2) 0.5000 0.12(2) Uani 1 4 d S TU P
C0AA C 0.3333 0.6667 0.296(14) 0.18(4) Uani 1 6 d S TU P
C2 C 0.784(3) 0.8921(14) 0.274(5) 0.105(12) Uani 1 2 d S T P
C1 C 0.684(8) 0.842(4) 0.5000 0.21(3) Uani 1 4 d S TU P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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
O008 K001 O008 134.33(19) 5_655 3_665
O008 K001 O008 84.5(4) 6_665 4
O008 K001 O008 134.33(19) 6_665 .
O008 K001 O008 84.5(4) 5_655 6_665
O008 K001 O008 134.33(19) 5_655 .
O008 K001 O008 78.2(6) 3_665 6_665
O008 K001 O008 134.33(19) 3_665 4
O008 K001 O008 78.2(6) 5_655 2_655
O008 K001 O008 134.33(19) 2_655 4
O008 K001 O008 84.5(4) 3_665 2_655
O008 K001 O008 84.5(4) 3_665 .
O008 K001 O008 134.33(19) 6_665 2_655
O008 K001 O008 84.5(4) 2_655 .
O008 K001 O008 84.5(4) 5_655 4
O008 K001 O008 78.2(6) 4 .
O008 K001 O009 110.4(4) 2_655 .
O008 K001 O009 171.5(4) 6_665 2_655
O008 K001 O009 171.5(4) 5_655 .
O008 K001 O009 49.10(13) . .
O008 K001 O009 171.5(4) 4 3_665
O008 K001 O009 171.5(4) 3_665 5_655
O008 K001 O009 89.2(3) 6_665 .
O008 K001 O009 89.2(3) 2_655 5_655
O008 K001 O009 89.2(3) 4 2_655
O008 K001 O009 89.2(3) . 5_655
O008 K001 O009 110.4(4) . 3_665
O008 K001 O009 89.2(3) 3_665 4
O008 K001 O009 49.10(13) 3_665 .
O008 K001 O009 171.5(4) 2_655 4
O008 K001 O009 89.2(3) 5_655 2_655
O008 K001 O009 89.2(3) 4 .
O008 K001 O009 49.10(13) 5_655 6_665
O008 K001 O009 49.10(13) 5_655 5_655
O008 K001 O009 89.2(3) 3_665 6_665
O008 K001 O009 110.4(4) 6_665 5_655
O008 K001 O009 49.10(13) 6_665 6_665
O008 K001 O009 49.10(13) 4 5_655
O008 K001 O009 89.2(3) 2_655 6_665
O008 K001 O009 110.4(4) 5_655 4
O008 K001 O009 110.4(4) 4 6_665
O008 K001 O009 49.10(13) 6_665 4
O008 K001 O009 171.5(4) . 6_665
O008 K001 O009 49.10(13) 4 4
O008 K001 O009 89.2(3) 5_655 3_665
O008 K001 O009 110.4(4) 3_665 2_655
O008 K001 O009 49.10(13) 3_665 3_665
O008 K001 O009 49.10(13) 2_655 2_655
O008 K001 O009 89.2(3) 6_665 3_665
O008 K001 O009 49.10(13) . 2_655
O008 K001 O009 49.10(13) 2_655 3_665
O008 K001 O009 89.2(3) . 4
O009 K001 O009 96.4(3) 6_665 4
O009 K001 O009 96.4(3) 6_665 5_655
O009 K001 O009 96.4(3) . 2_655
O009 K001 O009 128.99(15) 3_665 4
O009 K001 O009 128.99(15) 6_665 2_655
O009 K001 O009 61.1(5) . 4
O009 K001 O009 96.4(3) 3_665 .
O009 K001 O009 96.4(3) 5_655 4
O009 K001 O009 128.99(15) 3_665 5_655
O009 K001 O009 128.99(15) . 5_655
O009 K001 O009 96.4(3) 3_665 2_655
O009 K001 O009 61.1(5) 6_665 3_665
O009 K001 O009 61.1(5) 5_655 2_655
O009 K001 O009 128.99(15) 6_665 .
O009 K001 O009 128.99(15) 4 2_655
O004 Si02 O005 110.7(8) . .
O004 Si02 O007 107.3(4) . .
O004 Si02 O007 107.3(4) . 4
O007 Si02 O005 110.8(4) 4 .
O007 Si02 O005 110.8(4) . .
O007 Si02 O007 109.8(6) . 4
O006 Si03 K001 138.7(3) . .
O006 Si03 O007 107.9(5) . .
O006 Si03 O008 110.6(7) . .
O006 Si03 O009 112.3(7) . .
O007 Si03 K001 112.3(4) . .
O008 Si03 K001 46.3(4) . .
O008 Si03 O007 109.8(5) . .
O009 Si03 K001 63.4(5) . .
O009 Si03 O007 108.0(6) . .
O009 Si03 O008 108.2(6) . .
Si02 O004 Si02 170.9(11) . 9_565
Si02 O005 Si02 152.2(11) 7_665 .
Si03 O006 Si03 152.9(7) 4_556 .
Si02 O007 Si03 142.5(5) . .
Si03 O008 K001 109.6(4) 7_665 .
Si03 O008 K001 109.6(4) . .
Si03 O008 Si03 140.8(8) . 7_665
Si03 O009 K001 91.0(4) . .
Si03 O009 K001 91.0(4) 8_655 .
Si03 O009 Si03 142.8(11) . 8_655
C00C O00A C00C 120.000(6) 2_665 .
C00C O00A C00C 120.000(4) 3_565 2_665
C00C O00A C00C 120.000(2) 3_565 .
C0AA O00A C00C 90.00(4) 4_556 3_565
C0AA O00A C00C 90.00(2) 4_556 2_665
C0AA O00A C00C 90.000(7) . .
C0AA O00A C00C 90.00(3) . 3_565
C0AA O00A C00C 90.002(11) 4_556 .
C0AA O00A C00C 90.00(2) . 2_665
C0AA O00A C0AA 180.0 4_556 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K001 O008 2.915(13) 5_655
K001 O008 2.915(13) 4
K001 O008 2.915(13) 2_655
K001 O008 2.915(13) 3_665
K001 O008 2.915(13) 6_665
K001 O008 2.915(13) .
K001 O009 3.395(13) 6_665
K001 O009 3.395(13) 2_655
K001 O009 3.395(13) 4
K001 O009 3.395(13) .
K001 O009 3.395(13) 5_655
K001 O009 3.395(13) 3_665
Si02 O004 1.618(5) .
Si02 O005 1.631(6) .
Si02 O007 1.628(8) .
Si02 O007 1.628(8) 4
Si03 O006 1.627(4) .
Si03 O007 1.648(8) .
Si03 O008 1.644(5) .
Si03 O009 1.638(6) .
O004 Si02 1.618(5) 9_565
O005 Si02 1.631(6) 7_665
O006 Si03 1.627(4) 4_556
O008 Si03 1.644(5) 7_665
O009 Si03 1.638(6) 8_655
O00A C00C 1.63(5) 2_665
O00A C00C 1.63(5) 3_565
O00A C00C 1.63(5) .
O00A C0AA 1.54(11) 4_556
O00A C0AA 1.54(11) .
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.7(4)
2 0.3(4)
