data_OFF-O-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_PLAT029_OFF-O-2      
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.859 Note 
RESPONSE: The diffractometer was single axis (synchrotron), and the 
crystal was weakly diffracting. Thus, low completeness was obtained.
;
_vrf_PLAT306_OFF-O-2      
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1 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), 9(C), 3(O)'
_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' 0.0040 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'

_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                    13.2558(3)
_cell_length_b                    13.2558(3)
_cell_length_c                    7.5358(2)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      1146.76(6)
_cell_formula_units_Z             1
_cell_measurement_reflns_used     2330
_cell_measurement_temperature     273(2)
_cell_measurement_theta_max       30.890
_cell_measurement_theta_min       3.244
_shelx_estimated_absorpt_T_max    ?
_shelx_estimated_absorpt_T_min    ?
_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_absorpt_special_details    ?
_exptl_crystal_colour             'colourless'
_exptl_crystal_density_diffrn     1.959
_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   0.0325
_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_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_source                    synchrotron
_diffrn_source_type               'Wiggler, Station I911-3, MAX II, MAXLAB'
_diffrn_standards_number          0
_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_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          0.763
_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_coef        .
_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_R_factor_all           0.0458
_refine_ls_R_factor_gt            0.0431
_refine_ls_restrained_S_all       1.112
_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
_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 0.0000 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 . .


_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 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_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
 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_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_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 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 . . . ?


_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)

