data_OFF-H-b-2
_audit_creation_date              2017-05-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number      '2014/7'
# start Validation Reply Form
_vrf_PLAT306_OFF-H-b-2      
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O00B Check
RESPONSE: Residual disordered electron density in the pores was
modelled using dummy O and C atoms.
;
# Added during the CSD deposition process: Monday 02 May 2017 02:02 PM
# end Validation Reply Form
_publ_contact_author_address      
;
inGAP Centre for Research Based Innovation
Department of Chemistry
University of Oslo
0315 Oslo
Norway
;
_publ_contact_author_email        sigurdoi@kjemi.uio.no
_publ_contact_author_name         'Sigurd Øien-Ødegaard'
_publ_contact_author_phone        '+47 90 545 313'
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Bruker-AXS (2016). APEX3. Version 2016.5-0. Madison, Wisconsin, USA.

Sheldrick, G. M. (2015a). Sheldrick, G. M., Acta Cryst. A, 2015, 71, 3-8.

Sheldrick, G. M. (2015b). Sheldrick, G. M., Acta Cryst. C, 2015, 71, 3-8.
;
_chemical_name_common             'Offretite'
_chemical_name_systematic         ?
_chemical_formula_moiety          'K1 O36 Si18, 2(C2.5 O0.5), 3(O), 9(C)'
_chemical_formula_sum             'C14 K O40 Si18'
_chemical_formula_weight          1352.86
_chemical_absolute_configuration  ?
_chemical_melting_point           ?
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' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system       'hexagonal'
_space_group_IT_number            187
_space_group_name_H-M_alt         'P -6 m 2'
_space_group_name_Hall            'P -6 2'
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'

_cell_length_a                    13.2269(16)
_cell_length_b                    13.2269(16)
_cell_length_c                    7.5381(10)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      1142.1(3)
_cell_formula_units_Z             1
_cell_measurement_reflns_used     5147
_cell_measurement_temperature     273(2)
_cell_measurement_theta_max       30.40
_cell_measurement_theta_min       3.244
_shelx_estimated_absorpt_T_max    ?
_shelx_estimated_absorpt_T_min    ?
_exptl_absorpt_coefficient_mu     0.708
_exptl_absorpt_correction_T_max   0.7461
_exptl_absorpt_correction_T_min   0.6092
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.2616 before and 0.0226 after correction. The Ratio of minimum to maximum transmission is 0.8165. The λ/2 correction factor is 0.00150.'
_exptl_absorpt_special_details    ?
_exptl_crystal_colour             'colourless'
_exptl_crystal_density_diffrn     1.967
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_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
_exptl_transmission_factor_max    ?
_exptl_transmission_factor_min    ?
_diffrn_reflns_av_R_equivalents   0.0282
_diffrn_reflns_av_unetI/netI      0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max        15
_diffrn_reflns_limit_h_min        -17
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_l_max        10
_diffrn_reflns_limit_l_min        -10
_diffrn_reflns_number             6592
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full         25.242
_diffrn_reflns_theta_max          28.711
_diffrn_reflns_theta_min          3.080
_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 0.987
_diffrn_measured_fraction_theta_max 0.991
_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            MoK\a
_diffrn_radiation_wavelength      0.71073
_diffrn_source                    synchrotron
_diffrn_source_type               'Wiggler, Station I911-3, MAX II, MAXLAB'
_diffrn_standards_number          0
_reflns_Friedel_coverage          0.878
_reflns_Friedel_fraction_full     0.992
_reflns_Friedel_fraction_max      0.995
_reflns_number_gt                 1156
_reflns_number_total              1180
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression      'I > 2σ(I)'
_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)'
_refine_diff_density_max          0.960
_refine_diff_density_min          -0.467
_refine_diff_density_rms          0.100
_refine_ls_abs_structure_details
;
 Flack x determined using 523 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack    0.02(3)
_refine_ls_extinction_coef        .
_refine_ls_extinction_method      none
_refine_ls_goodness_of_fit_ref    1.166
_refine_ls_hydrogen_treatment     undef
_refine_ls_matrix_type            full
_refine_ls_number_parameters      77
_refine_ls_number_reflns          1180
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0363
_refine_ls_R_factor_gt            0.0358
_refine_ls_restrained_S_all       1.166
_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)+(0.0568P)²+1.4053P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme       calc
_refine_ls_wR_factor_gt           0.1046
_refine_ls_wR_factor_ref          0.1050
_refine_special_details
;
 Refined as a 2-component twin.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.4(2)
 0.6(2)
;
_atom_sites_solution_hydrogens    .
_atom_sites_solution_primary      dual
_atom_sites_solution_secondary    ?
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
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 K001 K 0.6667 0.3333 0.5000 0.0159(5) Uani 1 12 d S T P . .
 Si02 Si 0.66716(10) 0.56720(8) 0.78980(12) 0.0104(3) Uani 1 1 d . . . . .
 Si03 Si 0.75984(11) 0.75814(11) 0.5000 0.0098(3) Uani 1 2 d S T P . .
 O004 O 0.6693(4) 0.5978(4) 1.0000 0.0184(7) Uani 1 2 d S T P . .
 O005 O 0.76453(18) 0.5291(4) 0.7421(5) 0.0164(7) Uani 1 2 d S T P . .
 O006 O 0.7491(6) 0.8745(3) 0.5000 0.0236(13) Uani 1 4 d S T P . .
 O007 O 0.8962(3) 0.7925(6) 0.5000 0.0200(12) Uani 1 4 d S T P . .
 O008 O 0.5395(2) 0.4605(2) 0.7290(6) 0.0230(9) Uani 1 2 d S T P . .
 O009 O 0.6931(3) 0.6839(2) 0.6789(3) 0.0221(6) Uani 1 1 d . . . . .
 O00A O 1.0000 1.0000 1.0000 0.073(5) Uani 1 12 d S T P . .
 O00B O 0.426(2) 0.574(2) 0.5000 0.31(2) Uani 1 4 d S T P . .
 C00C C 0.9268(11) 0.854(2) 1.0000 0.136(12) Uani 1 4 d S T P . .
 C1 C 1.0000 1.0000 1.176(4) 0.19(2) Uani 1 6 d S T P . .
 C0AA C 0.668(5) 0.834(2) 1.0000 0.202(19) Uani 1 4 d S T P . .
 C2 C 0.5530(19) 0.7765(10) 0.774(2) 0.115(7) Uani 1 2 d S T P . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
 K001 O005 2.891(4) 6_666 ?
 K001 O005 2.891(4) 4_556 ?
 K001 O005 2.891(4) 5_656 ?
 K001 O005 2.891(4) 3_665 ?
 K001 O005 2.891(4) . ?
 K001 O005 2.891(4) 2_655 ?
 K001 O008 3.385(5) 5_656 ?
 K001 O008 3.385(5) . ?
 K001 O008 3.385(5) 4_556 ?
 K001 O008 3.385(5) 6_666 ?
 K001 O008 3.385(5) 2_655 ?
 K001 O008 3.385(5) 3_665 ?
 Si02 O004 1.6321(13) . ?
 Si02 O005 1.6409(17) . ?
 Si02 O008 1.6338(17) . ?
 Si02 O009 1.634(3) . ?
 Si03 O006 1.6155(15) . ?
 Si03 O007 1.625(2) . ?
 Si03 O009 1.642(2) 4_556 ?
 Si03 O009 1.642(2) . ?
 O004 Si02 1.6320(13) 4_557 ?
 O005 Si02 1.6409(17) 8_655 ?
 O006 Si03 1.6155(15) 9_565 ?
 O007 Si03 1.625(2) 8_655 ?
 O008 Si02 1.6338(17) 7_665 ?
 O00A C00C 1.68(3) 2_765 ?
 O00A C00C 1.68(3) . ?
 O00A C00C 1.68(3) 3_675 ?
 O00A C1 1.33(3) 4_557 ?
 O00A C1 1.33(3) . ?

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
 O005 K001 O005 78.29(16) 6_666 3_665 ?
 O005 K001 O005 78.29(17) . 4_556 ?
 O005 K001 O005 84.39(12) . 2_655 ?
 O005 K001 O005 134.37(6) 6_666 . ?
 O005 K001 O005 134.37(6) 6_666 2_655 ?
 O005 K001 O005 84.39(12) 3_665 . ?
 O005 K001 O005 134.37(6) 3_665 4_556 ?
 O005 K001 O005 84.39(12) 6_666 5_656 ?
 O005 K001 O005 84.39(12) 5_656 4_556 ?
 O005 K001 O005 134.37(6) 3_665 5_656 ?
 O005 K001 O005 84.39(12) 3_665 2_655 ?
 O005 K001 O005 134.37(6) . 5_656 ?
 O005 K001 O005 78.29(17) 5_656 2_655 ?
 O005 K001 O005 84.39(12) 6_666 4_556 ?
 O005 K001 O005 134.37(6) 4_556 2_655 ?
 O005 K001 O008 110.20(11) 5_656 6_666 ?
 O005 K001 O008 49.04(4) . . ?
 O005 K001 O008 49.04(4) 6_666 6_666 ?
 O005 K001 O008 171.51(11) 2_655 6_666 ?
 O005 K001 O008 89.33(8) 4_556 3_665 ?
 O005 K001 O008 49.04(4) 3_665 2_655 ?
 O005 K001 O008 89.33(8) . 6_666 ?
 O005 K001 O008 89.33(8) 5_656 2_655 ?
 O005 K001 O008 89.33(8) 4_556 . ?
 O005 K001 O008 49.05(4) 2_655 2_655 ?
 O005 K001 O008 110.20(11) 2_655 3_665 ?
 O005 K001 O008 171.51(11) 3_665 4_556 ?
 O005 K001 O008 89.33(8) 3_665 6_666 ?
 O005 K001 O008 49.04(4) 5_656 4_556 ?
 O005 K001 O008 171.51(11) 6_666 . ?
 O005 K001 O008 49.05(4) 4_556 6_666 ?
 O005 K001 O008 49.04(4) 6_666 5_656 ?
 O005 K001 O008 89.33(8) 6_666 2_655 ?
 O005 K001 O008 89.33(8) 3_665 5_656 ?
 O005 K001 O008 110.20(11) . 2_655 ?
 O005 K001 O008 171.51(11) . 5_656 ?
 O005 K001 O008 171.51(11) 4_556 2_655 ?
 O005 K001 O008 49.05(4) 5_656 5_656 ?
 O005 K001 O008 110.20(11) 6_666 4_556 ?
 O005 K001 O008 110.20(11) 4_556 5_656 ?
 O005 K001 O008 89.33(8) . 4_556 ?
 O005 K001 O008 89.33(8) 2_655 5_656 ?
 O005 K001 O008 49.04(4) 4_556 4_556 ?
 O005 K001 O008 89.33(8) 6_666 3_665 ?
 O005 K001 O008 110.20(11) 3_665 . ?
 O005 K001 O008 49.04(4) 3_665 3_665 ?
 O005 K001 O008 89.33(8) 5_656 . ?
 O005 K001 O008 49.04(4) . 3_665 ?
 O005 K001 O008 49.04(4) 2_655 . ?
 O005 K001 O008 171.51(11) 5_656 3_665 ?
 O005 K001 O008 89.33(8) 2_655 4_556 ?
 O008 K001 O008 96.31(10) 5_656 4_556 ?
 O008 K001 O008 61.32(14) 5_656 2_655 ?
 O008 K001 O008 96.31(10) 2_655 . ?
 O008 K001 O008 129.05(4) 3_665 4_556 ?
 O008 K001 O008 129.05(4) 5_656 . ?
 O008 K001 O008 96.31(10) 6_666 4_556 ?
 O008 K001 O008 61.32(14) 3_665 6_666 ?
 O008 K001 O008 129.05(4) 2_655 4_556 ?
 O008 K001 O008 96.31(10) 3_665 2_655 ?
 O008 K001 O008 129.05(4) 6_666 2_655 ?
 O008 K001 O008 96.31(10) 3_665 . ?
 O008 K001 O008 129.05(4) 5_656 3_665 ?
 O008 K001 O008 61.32(14) 4_556 . ?
 O008 K001 O008 96.31(10) 5_656 6_666 ?
 O008 K001 O008 129.05(4) 6_666 . ?
 O004 Si02 K001 139.08(14) . . ?
 O004 Si02 O005 111.7(2) . . ?
 O004 Si02 O008 111.7(2) . . ?
 O004 Si02 O009 107.04(18) . . ?
 O005 Si02 K001 45.81(13) . . ?
 O008 Si02 K001 63.44(18) . . ?
 O008 Si02 O005 107.7(2) . . ?
 O008 Si02 O009 108.12(19) . . ?
 O009 Si02 K001 113.01(10) . . ?
 O009 Si02 O005 110.63(18) . . ?
 O006 Si03 O007 110.4(3) . . ?
 O006 Si03 O009 106.99(17) . . ?
 O006 Si03 O009 107.00(17) . 4_556 ?
 O007 Si03 O009 110.93(15) . . ?
 O007 Si03 O009 110.93(15) . 4_556 ?
 O009 Si03 O009 110.5(2) . 4_556 ?
 Si02 O004 Si02 152.3(3) 4_557 . ?
 Si02 O005 K001 110.18(13) 8_655 . ?
 Si02 O005 K001 110.18(13) . . ?
 Si02 O005 Si02 139.6(3) 8_655 . ?
 Si03 O006 Si03 171.2(5) . 9_565 ?
 Si03 O007 Si03 152.0(4) 8_655 . ?
 Si02 O008 K001 90.99(18) 7_665 . ?
 Si02 O008 K001 90.99(18) . . ?
 Si02 O008 Si02 143.1(3) . 7_665 ?
 Si02 O009 Si03 141.3(2) . . ?
 C00C O00A C00C 120.000(6) . 3_675 ?
 C00C O00A C00C 120.000(3) . 2_765 ?
 C00C O00A C00C 120.000(6) 2_765 3_675 ?
 C1 O00A C00C 90.00(2) . 2_765 ?
 C1 O00A C00C 90.000(16) 4_557 . ?
 C1 O00A C00C 90.000(4) . 3_675 ?
 C1 O00A C00C 90.000(16) . . ?
 C1 O00A C00C 90.000(4) 4_557 3_675 ?
 C1 O00A C00C 90.00(2) 4_557 2_765 ?
 C1 O00A C1 180.000(17) 4_557 . ?


_olex2_submission_special_instructions 'No special instructions were received'
loop_
  _twin_individual_id
  _twin_individual_mass_fraction_refined
 1 0.4(2)
 2 0.6(2)

