# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_COE-3_RED

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            COE-3
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15.19 O76 Si37.59'
_chemical_formula_weight         2454.12

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Cmcm
_symmetry_space_group_name_Hall  '-C 2c 2'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   7.19(10)
_cell_length_b                   21.79(10)
_cell_length_c                   13.62(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2134(35)
_cell_formula_units_Z            1
_cell_measurement_temperature    ?
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.910
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             407
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      ?
_diffrn_radiation_wavelength     0.02510
_diffrn_radiation_type           Electrons
_diffrn_radiation_source         '200 kV accerelating voltage'
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       'Rotation Electron Diffraction'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            418
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0177
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         0.07
_diffrn_reflns_theta_max         0.65
_reflns_number_total             418
_reflns_number_gt                227
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       683(78)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         418
_refine_ls_number_parameters     38
_refine_ls_number_restraints     50
_refine_ls_R_factor_all          0.4496
_refine_ls_R_factor_gt           0.3754
_refine_ls_wR_factor_ref         0.7956
_refine_ls_wR_factor_gt          0.7646
_refine_ls_goodness_of_fit_ref   4.147
_refine_ls_restrained_S_all      4.161
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.002

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.0000 0.322(2) 0.2500 0.159(11) Uiso 1 4 d SD . .
Si2 Si 0.212(5) 0.2727(16) 0.7500 0.159(11) Uiso 1 2 d SD . .
Si3 Si 0.293(4) 0.3128(11) 0.5453(19) 0.159(11) Uiso 1 1 d D . .
Si4 Si 0.0000 0.3862(16) 0.451(3) 0.159(11) Uiso 1 2 d SD . .
Si5 Si 0.144(13) 0.5000 0.5000 0.159(11) Uiso 0.22(6) 2 d SPD . .
O1 O 0.279(7) 0.317(2) 0.656(2) 0.241(14) Uiso 1 1 d D . .
O2 O 0.0000 0.369(3) 0.342(3) 0.241(14) Uiso 1 2 d SD . .
O3 O 0.0000 0.283(4) 0.7500 0.241(14) Uiso 1 4 d SD . .
O4 O 0.190(5) 0.368(2) 0.499(3) 0.241(14) Uiso 1 1 d D . .
O5 O 0.185(6) 0.284(2) 0.2500 0.241(14) Uiso 1 2 d SD . .
C1 C -0.269(12) 0.541(5) 0.428(7) 0.4(3) Uiso 0.22(6) 1 d P . .
O8 O 1.0000 0.543(2) 0.560(5) 0.241(14) Uiso 1 2 d S . .
O7 O 0.5000 0.337(3) 0.531(6) 0.241(14) Uiso 1 2 d SD . .
O6 O 0.7500 0.7500 0.5000 0.241(14) Uiso 1 2 d S . .
GC1 C -0.5000 0.600(9) 0.2500 0.36(9) Uiso 1 4 d S . .
GC2 C -0.5000 0.449(6) 0.406(11) 0.33(6) Uiso 1 2 d S . .

_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 O5 1.56(4) 3 ?
Si1 O5 1.56(4) . ?
Si1 O2 1.61(4) . ?
Si1 O2 1.61(4) 10_556 ?
Si2 O5 1.45(5) 13_556 ?
Si2 O3 1.54(4) . ?
Si2 O1 1.67(4) 10_557 ?
Si2 O1 1.67(4) . ?
Si3 O4 1.55(4) . ?
Si3 O1 1.52(4) . ?
Si3 O6 1.53(3) 5_445 ?
Si3 O7 1.59(4) . ?
Si4 O8 1.56(5) 9_666 ?
Si4 O2 1.53(5) . ?
Si4 O4 1.57(4) . ?
Si4 O4 1.57(4) 12 ?
Si5 C1 1.61(5) 9_566 ?
Si5 C1 1.61(5) 12 ?
Si5 O8 1.61(6) 9_666 ?
Si5 O8 1.61(6) 1_455 ?
Si5 Si5 2.07(19) 9_566 ?
O3 Si2 1.54(4) 3_556 ?
O5 Si2 1.45(5) 13_556 ?
C1 Si5 1.61(5) 9_566 ?
O8 Si4 1.56(5) 9_666 ?
O8 Si5 1.61(6) 9_666 ?
O8 Si5 1.61(6) 1_655 ?
O7 Si3 1.59(4) 12_655 ?
O6 Si3 1.53(3) 9_666 ?
O6 Si3 1.53(3) 5 ?

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
O5 Si1 O5 116(5) 3 . ?
O5 Si1 O2 109.4(14) 3 . ?
O5 Si1 O2 109.4(14) . . ?
O5 Si1 O2 109.4(14) 3 10_556 ?
O5 Si1 O2 109.4(14) . 10_556 ?
O2 Si1 O2 102(5) . 10_556 ?
O5 Si2 O3 129(5) 13_556 . ?
O5 Si2 O1 111(3) 13_556 10_557 ?
O3 Si2 O1 102(3) . 10_557 ?
O5 Si2 O1 111(3) 13_556 . ?
O3 Si2 O1 102(3) . . ?
O1 Si2 O1 100(4) 10_557 . ?
O4 Si3 O1 109(3) . . ?
O4 Si3 O6 116(3) . 5_445 ?
O1 Si3 O6 116(2) . 5_445 ?
O4 Si3 O7 98(3) . . ?
O1 Si3 O7 100(4) . . ?
O6 Si3 O7 116(3) 5_445 . ?
O8 Si4 O2 99(4) 9_666 . ?
O8 Si4 O4 107(3) 9_666 . ?
O2 Si4 O4 110(2) . . ?
O8 Si4 O4 107(2) 9_666 12 ?
O2 Si4 O4 110(2) . 12 ?
O4 Si4 O4 122(4) . 12 ?
C1 Si5 C1 112(8) 9_566 12 ?
C1 Si5 O8 110(4) 9_566 9_666 ?
C1 Si5 O8 112(4) 12 9_666 ?
C1 Si5 O8 112(4) 9_566 1_455 ?
C1 Si5 O8 110(4) 12 1_455 ?
O8 Si5 O8 100(6) 9_666 1_455 ?
C1 Si5 Si5 124(4) 9_566 9_566 ?
C1 Si5 Si5 124(4) 12 9_566 ?
O8 Si5 Si5 50(3) 9_666 9_566 ?
O8 Si5 Si5 50(3) 1_455 9_566 ?
Si3 O1 Si2 138(3) . . ?
Si4 O2 Si1 155(4) . . ?
Si2 O3 Si2 164(8) 3_556 . ?
Si3 O4 Si4 142(4) . . ?
Si2 O5 Si1 153(5) 13_556 . ?
Si4 O8 Si5 122(4) 9_666 9_666 ?
Si4 O8 Si5 122(4) 9_666 1_655 ?
Si5 O8 Si5 80(6) 9_666 1_655 ?
Si3 O7 Si3 139(5) . 12_655 ?
Si3 O6 Si3 180.0(8) 9_666 5 ?

_diffrn_measured_fraction_theta_max 0.844
_diffrn_reflns_theta_full        0.65
_diffrn_measured_fraction_theta_full 0.844
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.128



# start Validation Reply Form



_vrf_ATOM007_COE-3_RED           
;
PROBLEM: _atom_site_aniso_label is missing
RESPONSE: 
For one thing, the data quality of rotation electron diffraction (RED) data 
is not as good as single crystal X-ray diffraction data, due to the multiple
scattering, absorption problem and irradiation damage. The intensity is not 
good enough for the anisotropic atomic displacement refinement. For another, 
the COE-3 sample is very beam sensitive. We need to use very weak beam and 
short exposure time for data collection. The intensities for the reflections 
were relative weak and the resolution was also low. The number of unique and 
observed reflections was low, which also indicated that the data was not 
suitable for the anisotropic atomic displacements refinement.
;

_vrf_RADNT01_COE-3_RED           
;
PROBLEM: The radiation type should contain one of the following
RESPONSE: The radiation is electron with 200 kV accelerated voltage and 
the filament is LaB6. 
;




_vrf_RFACG01_COE-3_RED           
;
PROBLEM: The value of the R factor is > 0.20
RESPONSE:Due to the multiple scattering, absorption problem and irradiation 
damage of RED data, the intensity was not as accurate as SXRD data,
which may lead to the high R factor. Besides, due to the porosities in COE-3,
the intensity quality and resolution of the diffraction data were rather poor
as indicated by the low I/sigma and high Rint.These also resulted in 
relatively high R-values in the final refinements.
;




_vrf_RFACR01_COE-3_RED           
;
PROBLEM: The value of the weighted R factor is > 0.45
RESPONSE:Due to the multiple scattering, absorption problem and irradiation 
damage of RED data, the intensity was not as accurate as SXRD data,
which may lead to the high R factor. Besides, due to the porosities in COE-3,
the intensity quality and resolution of the diffraction data were rather poor
as indicated by the low I/sigma and high Rint.These also resulted in 
relatively high R-values in the final refinements.
;



_vrf_PLAT029_COE-3_RED           
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.844 Note  
RESPONSE: Rotation Electron Diffraction (RED) is a new method for automated
collection and processing of 3D electron diffraction data. Due to the limition 
of the TEM ginometer design, it can not rotate as much as you want so that 
the completeness of the dataset is low.
;


_vrf_PLAT082_COE-3_RED           
;
PROBLEM: High R1 Value ..................................       0.38 Why ? 
RESPONSE:Due to the multiple scattering, absorption problem and irradiation 
damage of RED data, the intensity was not as accurate as SXRD data,
which may lead to the high R factor. Besides, due to the porosities in COE-3,
the intensity quality and resolution of the diffraction data were rather poor
as indicated by the low I/sigma and high Rint.These also resulted in 
relatively high R-values in the final refinements.
;



_vrf_PLAT084_COE-3_RED           
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.80 Why ? 
RESPONSE: Due to the multiple scattering, absorption problem and irradiation 
damage of RED data, the intensity was not as accurate as SXRD data,
which may lead to the high R factor. Besides, due to the porosities in COE-3,
the intensity quality and resolution of the diffraction data were rather poor
as indicated by the low I/sigma and high Rint.These also resulted in 
relatively high R-values in the final refinements.
;





_vrf_PLAT197_COE-3_RED           
;
PROBLEM: Missing            _cell_measurement_temperature     Please Do ! 
RESPONSE: The sample was measured in the TEM colume, it is high vacuum and the 
electrons interact with the sample, generating some heat. So it is hard to 
mearsure the temperature.
;




_vrf_PLAT198_COE-3_RED           
;
PROBLEM: Missing              _diffrn_ambient_temperature     Please Do ! 
RESPONSE: The sample was measured in the TEM colume, it is high vacuum and the 
electrons interact with the sample, generating some heat. So it is hard to 
mearsure the temperature.
;


_vrf_THETM01_COE-3_RED           
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: COE-3 is a kind of microporous material and during the data collection 
, it will be damaged by the eletron beam. So the resolution is lower. 
;





_database_code_depnum_ccdc_archive 'CCDC 986730'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_coe4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            COE-4
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'O88.80 Si38.40'
_chemical_formula_weight         2499.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Cmcm
_symmetry_space_group_name_Hall  '-C 2c 2'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   7.29(10)
_cell_length_b                   23.02(10)
_cell_length_c                   14.02(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2353(38)
_cell_formula_units_Z            1
_cell_measurement_temperature    ?
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             399
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      ?
_diffrn_radiation_wavelength     0.02510
_diffrn_radiation_type           Electrons
_diffrn_radiation_source         '200 kV accerelating voltage'
_diffrn_radiation_monochromator  ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       'Rotation Electron Diffraction'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            513
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0084
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         0.08
_diffrn_reflns_theta_max         0.72
_reflns_number_total             513
_reflns_number_gt                359
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         513
_refine_ls_number_parameters     34
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.4431
_refine_ls_R_factor_gt           0.3878
_refine_ls_wR_factor_ref         0.8078
_refine_ls_wR_factor_gt          0.7750
_refine_ls_goodness_of_fit_ref   4.673
_refine_ls_restrained_S_all      4.552
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.0000 0.3277(18) 0.2500 0.114(8) Uiso 1 4 d SD . .
Si2 Si 0.211(4) 0.2694(12) 0.7500 0.114(8) Uiso 1 2 d SD . .
Si3 Si 0.303(3) 0.3115(9) 0.5444(14) 0.114(8) Uiso 1 1 d D . .
Si4 Si 0.0000 0.3853(13) 0.451(2) 0.114(8) Uiso 1 2 d SD . .
Si5 Si 0.135(13) 0.5000 0.5000 0.114(8) Uiso 0.12(5) 2 d SPD . .
O1 O 0.247(5) 0.3075(16) 0.6570(19) 0.149(9) Uiso 1 1 d D . .
O2 O 0.0000 0.371(2) 0.339(2) 0.149(9) Uiso 1 2 d SD . .
O3 O 0.0000 0.249(3) 0.7500 0.149(9) Uiso 1 4 d SD . .
O4 O 0.183(4) 0.3601(15) 0.493(2) 0.149(9) Uiso 1 1 d D . .
O5 O 0.183(5) 0.2889(18) 0.2500 0.149(9) Uiso 1 2 d SD . .
O6 O 0.7500 0.7500 0.5000 0.149(9) Uiso 1 2 d S . .
O7 O 0.5000 0.335(2) 0.546(4) 0.149(9) Uiso 1 2 d SD . .
O8 O 1.0000 0.5469(16) 0.550(3) 0.149(9) Uiso 1 2 d S . .
O9 O -0.260(11) 0.533(4) 0.422(5) 0.149(9) Uiso 0.12(5) 1 d P . .
OW1 O -0.5000 0.518(6) 0.346(10) 0.29(5) Uiso 1 2 d S . .

_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 O2 1.60(4) . ?
Si1 O2 1.60(4) 10_556 ?
Si1 O5 1.60(4) 3 ?
Si1 O5 1.60(4) . ?
Si2 O5 1.55(4) 13_556 ?
Si2 O1 1.59(3) 10_557 ?
Si2 O1 1.59(3) . ?
Si2 O3 1.61(4) . ?
Si3 O7 1.53(3) . ?
Si3 O4 1.59(3) . ?
Si3 O6 1.59(2) 5_445 ?
Si3 O1 1.63(3) . ?
Si4 O8 1.56(4) 9_666 ?
Si4 O4 1.57(3) 12 ?
Si4 O4 1.57(3) . ?
Si4 O2 1.61(4) . ?
Si5 O9 1.61(5) 9_566 ?
Si5 O9 1.61(5) 12 ?
Si5 O8 1.62(5) 9_666 ?
Si5 O8 1.62(5) 1_455 ?
Si5 Si5 1.97(19) 9_566 ?
O3 Si2 1.61(4) 3_556 ?
O5 Si2 1.55(4) 13_556 ?
O6 Si3 1.59(2) 9_666 ?
O6 Si3 1.59(2) 5 ?
O7 Si3 1.53(3) 12_655 ?
O8 Si4 1.56(4) 9_666 ?
O8 Si5 1.62(5) 9_666 ?
O8 Si5 1.62(5) 1_655 ?
O9 Si5 1.61(5) 9_566 ?

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
O2 Si1 O2 103(5) . 10_556 ?
O2 Si1 O5 110.4(11) . 3 ?
O2 Si1 O5 110.4(11) 10_556 3 ?
O2 Si1 O5 110.4(11) . . ?
O2 Si1 O5 110.4(11) 10_556 . ?
O5 Si1 O5 112(4) 3 . ?
O5 Si2 O1 113(2) 13_556 10_557 ?
O5 Si2 O1 113(2) 13_556 . ?
O1 Si2 O1 110(4) 10_557 . ?
O5 Si2 O3 103(3) 13_556 . ?
O1 Si2 O3 108(2) 10_557 . ?
O1 Si2 O3 108(2) . . ?
O7 Si3 O4 106(2) . . ?
O7 Si3 O6 123(2) . 5_445 ?
O4 Si3 O6 108.4(18) . 5_445 ?
O7 Si3 O1 104(3) . . ?
O4 Si3 O1 110(2) . . ?
O6 Si3 O1 105.5(16) 5_445 . ?
O8 Si4 O4 112.1(18) 9_666 12 ?
O8 Si4 O4 112.1(18) 9_666 . ?
O4 Si4 O4 116(3) 12 . ?
O8 Si4 O2 101(3) 9_666 . ?
O4 Si4 O2 107.0(18) 12 . ?
O4 Si4 O2 107.0(18) . . ?
O9 Si5 O9 112(7) 9_566 12 ?
O9 Si5 O8 109(3) 9_566 9_666 ?
O9 Si5 O8 111(3) 12 9_666 ?
O9 Si5 O8 111(3) 9_566 1_455 ?
O9 Si5 O8 109(3) 12 1_455 ?
O8 Si5 O8 105(6) 9_666 1_455 ?
O9 Si5 Si5 124(4) 9_566 9_566 ?
O9 Si5 Si5 124(4) 12 9_566 ?
O8 Si5 Si5 53(3) 9_666 9_566 ?
O8 Si5 Si5 53(3) 1_455 9_566 ?
Si2 O1 Si3 150(3) . . ?
Si1 O2 Si4 153(4) . . ?
Si2 O3 Si2 146(5) . 3_556 ?
Si4 O4 Si3 154(3) . . ?
Si2 O5 Si1 154(4) 13_556 . ?
Si3 O6 Si3 180.0(7) 9_666 5 ?
Si3 O7 Si3 139(4) 12_655 . ?
Si4 O8 Si5 131(3) 9_666 9_666 ?
Si4 O8 Si5 131(3) 9_666 1_655 ?
Si5 O8 Si5 75(6) 9_666 1_655 ?

_diffrn_measured_fraction_theta_max 0.707
_diffrn_reflns_theta_full        0.72
_diffrn_measured_fraction_theta_full 0.707
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.116







_vrf_ATOM007_coe4                
;
PROBLEM: _atom_site_aniso_label is missing
RESPONSE: For one thing, the data quality of rotation electron diffraction (RED)
data is not as good as single crystal X-ray diffraction data, due to the multiple
scattering, absorption problem and irradiation damage. The intensity is not 
good enough for the anisotropic atomic displacement refinement. For another, 
the COE-4 sample is very beam sensitive. We need to use very weak beam and 
short exposure time for data collection. The intensities for the reflections 
were relative weak and the resolution was also low. The number of unique and 
observed reflections was low, which also indicated that the data was not 
suitable for the anisotropic atomic displacements refinement.
;





_vrf_RADNT01_coe4                
;
PROBLEM: The radiation type should contain one of the following
RESPONSE: The radiation is electron with 200 kV accelerated voltage and 
the filament is LaB6. 
;







_vrf_RFACG01_coe4                
;
PROBLEM: The value of the R factor is > 0.20
RESPONSE: Due to the multiple scattering, absorption problem and irradiation 
damage of RED data, the intensity was not as accurate as SXRD data,
which may lead to the high R factor. Besides, due to the porosities in COE-4,
the intensity quality and resolution of the diffraction data were rather poor
as indicated by the low I/sigma and high Rint.These also resulted in 
relatively high R-values in the final refinements.
;




_vrf_RFACR01_coe4                
;
PROBLEM: The value of the weighted R factor is > 0.45
RESPONSE: Due to the multiple scattering, absorption problem and irradiation 
damage of RED data, the intensity was not as accurate as SXRD data,
which may lead to the high R factor. Besides, due to the porosities in COE-4,
the intensity quality and resolution of the diffraction data were rather poor
as indicated by the low I/sigma and high Rint.These also resulted in 
relatively high R-values in the final refinements.
;





_vrf_THETM01_coe4                
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: COE-4 is a kind of microporous material and during the data collection 
, it will be damaged by the eletron beam. So the resolution is lower. 
;






_vrf_PLAT029_coe4                
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.707 Note  
RESPONSE:  Rotation Electron Diffraction (RED) is a new method for automated
collection and processing of 3D electron diffraction data. Due to the limition 
of the TEM ginometer design, it can not rotate as much as you want so that 
the completeness of the dataset is low.
;




_vrf_PLAT082_coe4                
;
PROBLEM: High R1 Value ..................................       0.39 Why ? 
RESPONSE:Due to the multiple scattering, absorption problem and irradiation 
damage of RED data, the intensity was not as accurate as SXRD data,
which may lead to the high R factor. Besides, due to the porosities in COE-4,
the intensity quality and resolution of the diffraction data were rather poor
as indicated by the low I/sigma and high Rint.These also resulted in 
relatively high R-values in the final refinements.
;




_vrf_PLAT084_coe4                
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.81 Why ? 
RESPONSE: Due to the multiple scattering, absorption problem and irradiation 
damage of RED data, the intensity was not as accurate as SXRD data,
which may lead to the high R factor. Besides, due to the porosities in COE-4,
the intensity quality and resolution of the diffraction data were rather poor
as indicated by the low I/sigma and high Rint.These also resulted in 
relatively high R-values in the final refinements.
;






_vrf_PLAT198_coe4                
;
PROBLEM: Missing              _diffrn_ambient_temperature     Please Do ! 
RESPONSE: The sample was measured in the TEM colume, it is high vacuum and the 
electrons interact with the sample, generating some heat. So it is hard to 
mearsure the temperature.
;

_vrf_PLAT197_coe4                
;
PROBLEM: Missing            _cell_measurement_temperature     Please Do ! 
RESPONSE: The sample was measured in the TEM colume, it is high vacuum and the 
electrons interact with the sample, generating some heat. So it is hard to 
mearsure the temperature.
;




# end Validation Reply Form
_database_code_depnum_ccdc_archive 'CCDC 986731'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_COE-3_PXRD
_chemical_name_mineral           ?hkl_Phase?

_chemical_name_common            COE-3
_chemical_formula_moiety         'C6.67 O76 Si39.34, 12.45C'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C19.12 O76 Si39.34'
_chemical_formula_weight         2550.63





_cell_length_a                   7.40027(35)
_cell_length_b                   23.4265(17)
_cell_length_c                   14.00808(66)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2428.48(24)
_cell_formula_units_Z            1
_cell_measurement_temperature    298
_symmetry_space_group_name_H-M   Cmcm
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,z+1/2
-x,y,-z+1/2
' x,-y,-z'
-x,-y,-z
x,y,-z+1/2
x,-y,z+1/2
-x,y,z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,z+1/2
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,-z
-x+1/2,-y+1/2,-z
x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2
-x+1/2,y+1/2,z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Si1 Si 4 0 0.32626(33) 0.25 1 1.78(34)
Si2 Si 8 0.21312(73) 0.27129(23) 0.75 1 1.78(34)
Si3 Si 16 0.29952(39) 0.31085(13) 0.54711(24) 1 1.78(34)
Si4 Si 8 0 0.38204(18) 0.45110(27) 1 1.78(34)
Si5 Si 8 0.1379(10) 0.5 0.5 0.4173(93) 1.78(34)
O1 O 16 0.27214(86) 0.30972(24) 0.65975(18) 1 2.11(39)
O2 O 8 0 0.36754(32) 0.33975(22) 1 2.11(39)
O3 O 4 0 0.25799(68) 0.75 1 2.11(39)
O4 O 16 0.18102(38) 0.35958(15) 0.49778(28) 1 2.11(39)
O5 O 8 0.18252(66) 0.28935(24) 0.25 1 2.11(39)
C1 C 16 -0.2788(14) 0.51771(40) 0.41096(48) 0.4173(93) 4.3(13)
O8 O 8 1 0.54924(13) 0.54546(35) 1 2.11(39)
O7 O 8 0.5 0.33171(30) 0.52543(56) 1 2.11(39)
O6 O 8 0.75 0.75 0.5 1 2.11(39)
EXTRA_C1 C 8 0 0.4752(31) 0.6608(60) 0.390(29) 4.3(13)
EXTRA_C2 C 8 0.6219(64) 0.3721(23) 0.25 0.473(23) 4.3(13)
EXTRA_C3 C 8 0.7730(94) 0.5286(25) 0.25 0.499(32) 4.3(13)
EXTRA_C4 C 8 0.50(31) 0.4813(23) 0.25 0.389(23) 4.3(13)

_diffrn_ambient_temperature      298
_diffrn_source                   ?
_diffrn_source_target            'Cu K\a'
_diffrn_source_type              Cu
_diffrn_radiation_type           ?
_diffrn_measurement_device_type  'PANalytical XPert Pro'
_diffrn_radiation_wavelength     1.540596
_diffrn_radiation_monochromator  'Ge 1 1 1'

_pd_meas_number_of_points        5000
_pd_meas_2theta_range_min        5.004
_pd_meas_2theta_range_max        90.004
_pd_meas_2theta_range_inc        0.017

_pd_proc_ls_prof_R_factor        3.347
_pd_proc_ls_prof_wR_factor       4.330
_pd_proc_ls_prof_wR_expected     1.750
_refine_ls_R_I_factor            0.016
_refine_ls_R_Fsqd_factor         ?
_refine_ls_R_factor_all          ?
_refine_ls_goodness_of_fit_all   2.5










loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Si1 O2 . . 1.586(7) ?
Si1 O2 . 3_555 1.586(7) ?
Si1 O5 . . 1.604(7) ?
Si1 O5 . 3_555 1.604(7) ?
Si2 O1 . . 1.612(5) ?
Si2 O1 . 6_556 1.612(5) ?
Si2 O3 . . 1.608(6) ?
Si2 O5 . 10_555 1.617(8) ?
Si3 O1 . . 1.591(4) ?
Si3 O4 . . 1.597(5) ?
Si3 O7 . . 1.591(4) ?
Si3 O6 . 9_445 1.613(3) ?
Si4 O2 . . 1.596(5) ?
Si4 O4 . . 1.581(4) ?
Si4 O4 . 8_555 1.581(4) ?
Si4 O8 . 4_466 1.611(5) ?
Si5 Si5 . 5_566 2.041(10) ?
Si5 C1 . 5_566 1.678(10) ?
Si5 C1 . 8_555 1.678(10) ?
Si5 O8 . 1_455 1.667(5) ?
Si5 O8 . 4_466 1.667(5) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 Si1 O2 . . 3_555 104.9(5) ?
O2 Si1 O5 . . . 109.19(15) ?
O2 Si1 O5 . . 3_555 109.19(15) ?
O2 Si1 O5 3_555 . . 109.19(15) ?
O2 Si1 O5 3_555 . 3_555 109.19(15) ?
O5 Si1 O5 . . 3_555 114.7(5) ?
O1 Si2 O1 . . 6_556 103.3(4) ?
O1 Si2 O3 . . . 112.0(4) ?
O1 Si2 O5 . . 10_555 111.2(3) ?
O1 Si2 O3 6_556 . . 112.0(4) ?
O1 Si2 O5 6_556 . 10_555 111.2(3) ?
O3 Si2 O5 . . 10_555 107.4(7) ?
O1 Si3 O4 . . . 111.8(3) ?
O1 Si3 O7 . . . 108.2(4) ?
O1 Si3 O6 . . 9_445 111.2(3) ?
O4 Si3 O7 . . . 102.1(3) ?
O4 Si3 O6 . . 9_445 109.3(2) ?
O7 Si3 O6 . . 9_445 113.9(3) ?
O2 Si4 O4 . . . 109.5(2) ?
O2 Si4 O4 . . 8_555 109.5(2) ?
O2 Si4 O8 . . 4_466 104.0(4) ?
O4 Si4 O4 . . 8_555 115.9(3) ?
O4 Si4 O8 . . 4_466 108.7(2) ?
O4 Si4 O8 8_555 . 4_466 108.7(2) ?
Si5 Si5 C1 5_566 . 5_566 128.4(4) ?
Si5 Si5 C1 5_566 . 8_555 128.4(4) ?
Si5 Si5 O8 5_566 . 1_455 52.2(2) ?
Si5 Si5 O8 5_566 . 4_466 52.2(2) ?
C1 Si5 C1 5_566 . 8_555 103.2(6) ?
C1 Si5 O8 5_566 . 1_455 105.5(3) ?
C1 Si5 O8 5_566 . 4_466 119.6(3) ?
C1 Si5 O8 8_555 . 1_455 119.6(3) ?
C1 Si5 O8 8_555 . 4_466 105.5(3) ?
O8 Si5 O8 1_455 . 4_466 104.5(4) ?
Si2 O1 Si3 . . . 145.2(4) ?
Si1 O2 Si4 . . . 154.7(6) ?
Si2 O3 Si2 . . 3_556 157.6(11) ?
Si3 O4 Si4 . . . 151.9(3) ?
Si1 O5 Si2 . . 10_554 151.2(5) ?
Si4 O8 Si5 4_666 . 1_655 134.7(2) ?
Si4 O8 Si5 4_666 . 5_666 134.7(2) ?
Si5 O8 Si5 1_655 . 5_666 75.5(3) ?
Si3 O7 Si3 . . 8_655 137.6(5) ?
Si3 O6 Si3 9_555 . 5_666 180.0(5) ?
_database_code_depnum_ccdc_archive 'CCDC 986835'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_COE-4_PXRD





_chemical_name_common            COE-4
_chemical_formula_moiety         'O81.42 Si38.71, 0.23 O8, 0.37 O8, 17.89 O'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'O104.14 Si38.71'
_chemical_formula_weight         2753.72






_cell_length_a                   7.39833(53)
_cell_length_b                   23.2909(23)
_cell_length_c                   13.99523(78)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_measurement_temperature    298
_cell_volume                     2411.57(32)
_symmetry_space_group_name_H-M   Cmcm



loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,z+1/2
3 -x,y,-z+1/2
4 x,-y,-z
5 -x,-y,-z
6 x,y,-z+1/2
7 x,-y,z+1/2
8 -x,y,z
9 x+1/2,y+1/2,z
10 -x+1/2,-y+1/2,z+1/2
11 -x+1/2,y+1/2,-z+1/2
12 x+1/2,-y+1/2,-z
13 -x+1/2,-y+1/2,-z
14 x+1/2,y+1/2,-z+1/2
15 x+1/2,-y+1/2,z+1/2
16 -x+1/2,y+1/2,z


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Si1 Si 4 0 0.32429(33) 0.25 1 2.57(35)
Si2 Si 8 0.20767(66) 0.27202(22) 0.75 1 2.57(35)
Si3 Si 16 0.29459(38) 0.31190(13) 0.54491(25) 1 2.57(35)
Si4 Si 8 0 0.38657(18) 0.45184(27) 1 2.57(35)
Si5 Si 8 0.13802(88) 0.5 0.5 0.339(11) 2.57(35)
O1 O 16 0.25736(86) 0.30939(22) 0.65735(17) 1 2.92(39)
O2 O 8 0 0.36286(28) 0.34430(17) 1 2.92(39)
O3 O 4 0 0.25278(63) 0.75 1 2.92(39)
O4 O 16 0.17928(26) 0.36403(16) 0.50241(34) 1 2.92(39)
O5 O 8 0.18044(56) 0.28718(21) 0.25 1 2.92(39)
O9 O 16 -0.26791(88) 0.52704(35) 0.41681(35) 0.339(11) 2.92(39)
O8 O 8 1 0.54448(15) 0.55427(40) 1 2.92(39)
O7 O 8 0.5 0.32951(23) 0.52320(49) 1 2.92(39)
O6 O 8 0.75 0.75 0.5 1 2.92(39)
EXTRA_O1 O 4 0 0.5416(26) 0.25 0.990(64) 15.0(22)
EXTRA_O2 O 8 0.784(17) 0.9619(63) 0.75 0.430(80) 15.0(22)
EXTRA_O3 O 8 0.910(41) 0 0.25 0.23(12) 15.0(22)
EXTRA_O4 O 8 0.5 0.4981(17) 0.8878(26) 0.835(55) 15.0(22)
EXTRA_O5 O 8 0.31418 0.6447(40) 0.75 0.476(34) 15.0(22)
EXTRA_O6 O 8 0.417(15) 0.4465(71) 0.25 0.374(53) 15.0(22)



_diffrn_ambient_temperature      298
_diffrn_source                   ?
_diffrn_source_target            'Cu K\a'
_diffrn_source_type              Cu
_diffrn_radiation_type           ?
_diffrn_measurement_device_type  'PANalytical XPert Pro'
_diffrn_radiation_wavelength     1.540596
_diffrn_radiation_monochromator  'Ge 1 1 1'

_pd_meas_number_of_points        5000
_pd_meas_2theta_range_min        5.008
_pd_meas_2theta_range_max        90.008
_pd_meas_2theta_range_inc        0.017

_pd_proc_ls_prof_R_factor        3.806
_pd_proc_ls_prof_wR_factor       4.755
_pd_proc_ls_prof_wR_expected     2.391
_refine_ls_R_I_factor            0.015
_refine_ls_R_Fsqd_factor         ?
_refine_ls_R_factor_all          ?
_refine_ls_goodness_of_fit_all   2



loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Si1 O2 . . 1.596(6) ?
Si1 O2 . 3_555 1.596(6) ?
Si1 O5 . . 1.590(6) ?
Si1 O5 . 3_555 1.590(6) ?
Si2 O1 . . 1.604(5) ?
Si2 O1 . 6_556 1.604(5) ?
Si2 O3 . . 1.600(6) ?
Si2 O5 . 10_555 1.608(7) ?
Si3 O1 . . 1.599(4) ?
Si3 O4 . . 1.599(5) ?
Si3 O7 . . 1.603(3) ?
Si3 O6 . 9_445 1.607(3) ?
Si4 O2 . . 1.603(5) ?
Si4 O4 . . 1.592(4) ?
Si4 O4 . 8_555 1.592(4) ?
Si4 O8 . 4_466 1.608(5) ?
Si5 Si5 . 5_566 2.042(9) ?
Si5 O9 . 5_566 1.636(7) ?
Si5 O9 . 8_555 1.636(7) ?
Si5 O8 . 1_455 1.641(5) ?
Si5 O8 . 4_466 1.641(5) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 Si1 O2 . . 3_555 111.5(5) ?
O2 Si1 O5 . . . 107.81(13) ?
O2 Si1 O5 . . 3_555 107.81(13) ?
O2 Si1 O5 3_555 . . 107.81(13) ?
O2 Si1 O5 3_555 . 3_555 107.81(13) ?
O5 Si1 O5 . . 3_555 114.2(5) ?
O1 Si2 O1 . . 6_556 107.8(4) ?
O1 Si2 O3 . . . 111.8(4) ?
O1 Si2 O5 . . 10_555 110.3(3) ?
O1 Si2 O3 6_556 . . 111.8(4) ?
O1 Si2 O5 6_556 . 10_555 110.3(3) ?
O3 Si2 O5 . . 10_555 104.7(6) ?
O1 Si3 O4 . . . 107.6(3) ?
O1 Si3 O7 . . . 111.1(4) ?
O1 Si3 O6 . . 9_445 108.5(3) ?
O4 Si3 O7 . . . 103.9(3) ?
O4 Si3 O6 . . 9_445 115.2(2) ?
O7 Si3 O6 . . 9_445 110.5(3) ?
O2 Si4 O4 . . . 107.7(3) ?
O2 Si4 O4 . . 8_555 107.7(3) ?
O2 Si4 O8 . . 4_466 107.1(4) ?
O4 Si4 O4 . . 8_555 112.8(3) ?
O4 Si4 O8 . . 4_466 110.7(2) ?
O4 Si4 O8 8_555 . 4_466 110.7(2) ?
Si5 Si5 O9 5_566 . 5_566 126.0(3) ?
Si5 Si5 O9 5_566 . 8_555 126.0(3) ?
Si5 Si5 O8 5_566 . 1_455 51.5(2) ?
Si5 Si5 O8 5_566 . 4_466 51.5(2) ?
O9 Si5 O9 5_566 . 8_555 108.0(5) ?
O9 Si5 O8 5_566 . 1_455 106.2(3) ?
O9 Si5 O8 5_566 . 4_466 116.9(3) ?
O9 Si5 O8 8_555 . 1_455 116.9(3) ?
O9 Si5 O8 8_555 . 4_466 106.2(3) ?
O8 Si5 O8 1_455 . 4_466 103.0(4) ?
Si2 O1 Si3 . . . 148.7(4) ?
Si1 O2 Si4 . . . 165.9(5) ?
Si2 O3 Si2 . . 3_556 147.5(10) ?
Si3 O4 Si4 . . . 149.3(3) ?
Si1 O5 Si2 . . 10_554 153.9(4) ?
Si4 O8 Si5 4_666 . 1_655 127.3(3) ?
Si4 O8 Si5 4_666 . 5_666 127.3(3) ?
Si5 O8 Si5 1_655 . 5_666 77.0(3) ?
Si3 O7 Si3 . . 8_655 142.9(4) ?
Si3 O6 Si3 9_555 . 5_666 180.0(5) ?





_database_code_depnum_ccdc_archive 'CCDC 986836'
