data_OFF-O-1
_audit_creation_date              2017-04-28
_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-1      
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.817 Note 
RESPONSE: The diffractometer was single axis (synchrotron), and the 
crystal was weakly diffracting. Thus, low completeness was obtained.
;
# 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          'K0.08 O3 Si1.5, C0.42 O0.08, C'
_chemical_formula_sum             'C0.75 K0.08 O3.52 Si1.50'
_chemical_formula_weight          110.73
_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' 0.2270 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                    13.265(3)
_cell_length_b                    13.265(3)
_cell_length_c                    7.545(2)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      1149.7(6)
_cell_formula_units_Z             12
_cell_measurement_reflns_used     954
_cell_measurement_temperature     273(2)
_cell_measurement_theta_max       26.731
_cell_measurement_theta_min       3.241
_shelx_estimated_absorpt_T_max    ?
_shelx_estimated_absorpt_T_min    ?
_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_absorpt_special_details    ?
_exptl_crystal_colour             'colourless'
_exptl_crystal_density_diffrn     1.919
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_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
_exptl_transmission_factor_max    ?
_exptl_transmission_factor_min    ?
_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_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_source                    synchrotron
_diffrn_source_type               'Wiggler, Station I911-3, MAX II, MAXLAB'
_diffrn_standards_number          0
_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_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     '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)'
_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_coef        .
_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_R_factor_all           0.0801
_refine_ls_R_factor_gt            0.0569
_refine_ls_restrained_S_all       1.145
_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
_refine_special_details
;
 Refined as a 2-component twin.
;
_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
;
_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 0.0000 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 . .


_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 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_
  _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
 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 . ?


_olex2_submission_special_instructions 'No special instructions were received'
loop_
  _twin_individual_id
  _twin_individual_mass_fraction_refined
 1 0.7(4)
 2 0.3(4)

