data_STF_e
_audit_creation_date              2016-04-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_publ_contact_author_name
;
 'Pablo J. Bereciartua'
 'Jose Luis Jorda'
;
_publ_contact_author_email          
;
 'Pablo J. Bereciartua'    'pabbepe@itq.upv.es'
 'Jose Luis Jorda'         'jjorda@itq.upv.es'
;
_publ_contact_author_address
;
        Instituto de Tecnologia Quimica CSIC-UPV
        Universidad Politecnica de Valencia
        Avenida de los naranjos s/n
        46022 Valencia
        Spain
;
_publ_contact_author_fax             '34 96 387 9448'
_publ_contact_author_phone           '34 96 387 7800'
_publ_section_references
;
Burla, M.C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G.L.,
 De Caro, L., Giacovazzo, C., Polidori, G., Siliqi, D., Spagna, R.
 (2007). J. Appl. Cryst. 40, 609-613.

Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
;
_chemical_name_common             ?
_chemical_name_systematic         ?
_chemical_formula_moiety          'O8 Si4'
_chemical_formula_sum             'O8 Si4'
_chemical_formula_weight          240.34
_chemical_melting_point           ?

_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       'monoclinic'
_space_group_IT_number            12
_space_group_name_H-M_alt         'C 1 2/m 1'
_space_group_name_Hall            '-C 2y'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y, -z'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z'
 '-x, -y, -z'
 'x, -y, z'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z'

_cell_length_a                    13.734
_cell_length_b                    17.946
_cell_length_c                    7.266
_cell_angle_alpha                 90
_cell_angle_beta                  99.50
_cell_angle_gamma                 90
_cell_volume                      1766.4
_cell_formula_units_Z             8
_cell_measurement_reflns_used     ?
_cell_measurement_temperature     293(2)
_cell_measurement_theta_max       ?
_cell_measurement_theta_min       ?
_shelx_estimated_absorpt_T_max    ?
_shelx_estimated_absorpt_T_min    ?
_exptl_absorpt_coefficient_mu     0.000
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_type    ?
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_exptl_crystal_colour             ?
_exptl_crystal_density_diffrn     1.807
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_description        ?
_exptl_crystal_F_000              313
_exptl_crystal_size_max           ?
_exptl_crystal_size_mid           ?
_exptl_crystal_size_min           ?
_exptl_transmission_factor_max    ?
_exptl_transmission_factor_min    ?
_diffrn_reflns_av_R_equivalents   0.1147
_diffrn_reflns_av_unetI/netI      0.1097
_diffrn_reflns_Laue_measured_fraction_full 0.538
_diffrn_reflns_Laue_measured_fraction_max 0.538
_diffrn_reflns_limit_h_max        14
_diffrn_reflns_limit_h_min        -14
_diffrn_reflns_limit_k_max        19
_diffrn_reflns_limit_k_min        -19
_diffrn_reflns_limit_l_max        8
_diffrn_reflns_limit_l_min        -8
_diffrn_reflns_number             1602
_diffrn_reflns_point_group_measured_fraction_full 0.538
_diffrn_reflns_point_group_measured_fraction_max 0.538
_diffrn_reflns_theta_full         0.823
_diffrn_reflns_theta_max          0.823
_diffrn_reflns_theta_min          0.067
_diffrn_ambient_temperature       293(2)
_diffrn_detector_area_resol_mean  ?
_diffrn_measured_fraction_theta_full 0.538
_diffrn_measured_fraction_theta_max 0.538
_diffrn_measurement_device        'transmission electron microscope'
_diffrn_measurement_device_type   'JEOL JEM-2100F'
_diffrn_measurement_method        '\o-scan'
_diffrn_radiation_type            electrons
_diffrn_radiation_wavelength      0.0251
_diffrn_source                    ?
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_full     .
_reflns_Friedel_fraction_max      .
_reflns_number_gt                 579
_reflns_number_total              774
_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 > 2\s(I)'
_computing_cell_refinement        ?
_computing_data_collection        ?
_computing_data_reduction         ?
_computing_molecular_graphics     'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material   'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement   'ShelXL (Sheldrick, 2008)'
_computing_structure_solution     'SIR2014 (Burla et al., 2015)'
_refine_diff_density_max          0.432
_refine_diff_density_min          -0.480
_refine_diff_density_rms          0.105
_refine_ls_extinction_coef        .
_refine_ls_extinction_method      none
_refine_ls_goodness_of_fit_ref    2.502
_refine_ls_hydrogen_treatment     undef
_refine_ls_matrix_type            full
_refine_ls_number_parameters      40
_refine_ls_number_reflns          774
_refine_ls_number_restraints      20
_refine_ls_R_factor_all           0.3161
_refine_ls_R_factor_gt            0.2882
_refine_ls_restrained_S_all       2.572
_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/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme       calc
_refine_ls_wR_factor_gt           0.6095
_refine_ls_wR_factor_ref          0.6439
_refine_special_details           ?
_olex2_refinement_description
;
1. Restrained distances
 Si1-O8_$1 = Si1-O3 = Si1-O1 = Si1-O6_$2
 1.61 with sigma of 0.02
 Si2-O1 = Si2-O5 = Si2-O6 = Si2-O7
 1.61 with sigma of 0.02
 Si3-O7 = Si3-O8 = Si3-O9 = Si3-O10_$3
 1.61 with sigma of 0.02
 Si4-O2 = Si4-O4_$4 = Si4-O10 = Si4-O10_$5
 1.61 with sigma of 0.02
 Si5-O2 = Si5-O4 = Si5-O5 = Si5-O5_$5
 1.61 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uiso(Si1) = Uiso(Si2) = Uiso(Si3) = Uiso(Si4) = Uiso(Si5)
Uiso(O1) = Uiso(O2) = Uiso(O3) = Uiso(O4) = Uiso(O5) = Uiso(O6) = Uiso(O7) =
Uiso(O8) = Uiso(O9) = Uiso(O10)
;
_atom_sites_solution_hydrogens    .
_atom_sites_solution_primary      direct
_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
 Si1 Si 0.8928(7) 0.2485(5) 0.4147(13) 0.059(3) Uiso 1 1 d D . . . .
 Si2 Si 0.7143(8) 0.1552(5) 0.3222(14) 0.059(3) Uiso 1 1 d D . . . .
 Si3 Si 0.6012(8) 0.1547(6) -0.0583(14) 0.059(3) Uiso 1 1 d D . . . .
 Si4 Si 0.4291(10) 0.0000 0.2208(18) 0.059(3) Uiso 1 2 d DS T P . .
 Si5 Si 0.6457(11) 0.0000 0.3877(18) 0.059(3) Uiso 1 2 d DS T P . .
 O1 O 0.8249(12) 0.1769(9) 0.390(3) 0.070(3) Uiso 1 1 d D . . . .
 O2 O 0.5466(13) 0.0000 0.244(3) 0.070(3) Uiso 1 2 d DS T P . .
 O3 O 1.0000 0.2219(14) 0.5000 0.070(3) Uiso 1 2 d DS T P . .
 O4 O 0.6224(18) 0.0000 0.598(2) 0.070(3) Uiso 1 2 d DS T P . .
 O5 O 0.7144(12) 0.0676(8) 0.348(2) 0.070(3) Uiso 1 1 d D . . . .
 O6 O 0.6501(12) 0.1981(9) 0.445(2) 0.070(3) Uiso 1 1 d D . . . .
 O7 O 0.6817(14) 0.1748(10) 0.111(2) 0.070(3) Uiso 1 1 d D . . . .
 O8 O 0.6167(15) 0.2031(9) -0.235(2) 0.070(3) Uiso 1 1 d D . . . .
 O9 O 0.5000 0.1737(14) 0.0000 0.070(3) Uiso 1 2 d DS T P . .
 O10 O 0.3893(13) -0.0701(7) 0.100(2) 0.070(3) Uiso 1 1 d D . . . .

_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
 Si1 O1 1.580(14) . ?
 Si1 O3 1.574(11) . ?
 Si1 O6 1.583(14) 7_656 ?
 Si1 O8 1.556(14) 7_655 ?
 Si2 O1 1.566(15) . ?
 Si2 O5 1.582(15) . ?
 Si2 O6 1.558(15) . ?
 Si2 O7 1.569(14) . ?
 Si3 O7 1.552(14) . ?
 Si3 O8 1.593(14) . ?
 Si3 O9 1.556(12) . ?
 Si3 O10 1.559(13) 5_655 ?
 Si4 O2 1.595(17) . ?
 Si4 O4 1.594(16) 2_656 ?
 Si4 O10 1.579(11) 6 ?
 Si4 O10 1.579(11) . ?
 Si5 O2 1.574(15) . ?
 Si5 O4 1.613(15) . ?
 Si5 O5 1.592(12) 6 ?
 Si5 O5 1.592(12) . ?
 O3 Si1 1.574(11) 2_756 ?
 O4 Si4 1.594(16) 5_656 ?
 O6 Si1 1.583(14) 7_656 ?
 O8 Si1 1.556(14) 7_655 ?
 O9 Si3 1.556(12) 2_655 ?
 O10 Si3 1.559(13) 5_655 ?

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
 O1 Si1 O6 107.0(13) . 7_656 ?
 O3 Si1 O1 107.2(12) . . ?
 O3 Si1 O6 110.7(9) . 7_656 ?
 O8 Si1 O1 113.0(10) 7_655 . ?
 O8 Si1 O3 116.3(11) 7_655 . ?
 O8 Si1 O6 102.3(11) 7_655 7_656 ?
 O1 Si2 O5 103.2(9) . . ?
 O1 Si2 O7 110.8(12) . . ?
 O6 Si2 O1 108.0(12) . . ?
 O6 Si2 O5 114.3(11) . . ?
 O6 Si2 O7 110.7(12) . . ?
 O7 Si2 O5 109.5(10) . . ?
 O7 Si3 O8 109.8(11) . . ?
 O7 Si3 O9 106.6(10) . . ?
 O7 Si3 O10 107.9(10) . 5_655 ?
 O9 Si3 O8 110.2(11) . . ?
 O9 Si3 O10 111.9(13) . 5_655 ?
 O10 Si3 O8 110.4(11) 5_655 . ?
 O4 Si4 O2 119.6(15) 2_656 . ?
 O10 Si4 O2 108.0(10) 6 . ?
 O10 Si4 O2 108.0(10) . . ?
 O10 Si4 O4 107.4(10) 6 2_656 ?
 O10 Si4 O4 107.4(10) . 2_656 ?
 O10 Si4 O10 105.7(13) . 6 ?
 O2 Si5 O4 110.2(16) . . ?
 O2 Si5 O5 110.7(10) . . ?
 O2 Si5 O5 110.7(10) . 6 ?
 O5 Si5 O4 112.7(9) 6 . ?
 O5 Si5 O4 112.7(9) . . ?
 O5 Si5 O5 99.3(16) . 6 ?
 Si2 O1 Si1 139.7(14) . . ?
 Si5 O2 Si4 144.9(19) . . ?
 Si1 O3 Si1 144.7(19) 2_756 . ?
 Si4 O4 Si5 165.3(18) 5_656 . ?
 Si2 O5 Si5 142.1(13) . . ?
 Si2 O6 Si1 167.1(14) . 7_656 ?
 Si3 O7 Si2 140.7(14) . . ?
 Si1 O8 Si3 167.6(15) 7_655 . ?
 Si3 O9 Si3 154.7(19) 2_655 . ?
 Si3 O10 Si4 148.5(12) 5_655 . ?

_shelx_SHELXL_version_number      '2014/7'
_olex2_submission_special_instructions 'No special instructions were received'