 
data_ECNU-45_treated_for_6h
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'O1.64 Si0.75' 
_chemical_formula_weight          47.46

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'
 
_space_group_crystal_system       hexagonal
_space_group_IT_number            190
_space_group_name_H-M_alt         'P -6 2 c'
_space_group_name_Hall            'P -6c -2c'
 
_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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-y, x-y, z'
 '-x+y, -x, z'
 'x, y, -z+1/2'
 '-y, x-y, -z+1/2'
 '-x+y, -x, -z+1/2'
 'y, x, -z'
 'x-y, -y, -z'
 '-x, -x+y, -z'
 'y, x, z+1/2'
 'x-y, -y, z+1/2'
 '-x, -x+y, z+1/2'
 
_cell_length_a                    19.816(3)
_cell_length_b                    19.816(3)
_cell_length_c                    13.917(3)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      4732.7(17)
_cell_formula_units_Z             83
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     5598
_cell_measurement_theta_min       0.042
_cell_measurement_theta_max       0.719
 
_exptl_crystal_description        hexagonal
_exptl_crystal_colour             ?
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.382          
_exptl_crystal_F_000              634
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           ?
_exptl_crystal_size_mid           ?
_exptl_crystal_size_min           ?
_exptl_absorpt_coefficient_mu     0.000
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.0251
_diffrn_radiation_type            electron
_diffrn_source                    electron
_diffrn_measurement_device_type   'JEOL TEM 2100 lab6 200kV'
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             5598
_diffrn_reflns_av_unetI/netI      0.1224
_diffrn_reflns_av_R_equivalents   0.1200
_diffrn_reflns_limit_h_min        -17
_diffrn_reflns_limit_h_max        17
_diffrn_reflns_limit_k_min        -19
_diffrn_reflns_limit_k_max        19
_diffrn_reflns_limit_l_min        -13
_diffrn_reflns_limit_l_max        13
_diffrn_reflns_theta_min          0.042
_diffrn_reflns_theta_max          0.719
_diffrn_reflns_theta_full         0.719
_diffrn_measured_fraction_theta_max   0.996
_diffrn_measured_fraction_theta_full  0.996
_diffrn_reflns_Laue_measured_fraction_max    0.996
_diffrn_reflns_Laue_measured_fraction_full   0.996
_diffrn_reflns_point_group_measured_fraction_max   0.991
_diffrn_reflns_point_group_measured_fraction_full  0.991
_reflns_number_total              1729
_reflns_number_gt                 1216
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.790
_reflns_Friedel_fraction_max      0.985
_reflns_Friedel_fraction_full     0.985
 
_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.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    .
_refine_ls_hydrogen_treatment     undef
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_abs_structure_details
;
 All f" are zero, so absolute structure could not be determined
;
_refine_ls_abs_structure_Flack    ?
_chemical_absolute_configuration  ?
_refine_ls_number_reflns          1729
_refine_ls_number_parameters      220
_refine_ls_number_restraints      159
_refine_ls_R_factor_all           0.1888
_refine_ls_R_factor_gt            0.1723
_refine_ls_wR_factor_ref          0.3743
_refine_ls_wR_factor_gt           0.3602
_refine_ls_goodness_of_fit_ref    1.333
_refine_ls_restrained_S_all       1.397
_refine_ls_shift/su_max           0.001
_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_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 0.4892(7) 0.0733(7) 0.2500 0.046(4) Uani 1 2 d DS T P . .
Si2 Si 0.4220(10) 0.1851(10) 0.2500 0.083(6) Uani 1 2 d DS T P . .
Si3 Si 0.4960(6) 0.2801(6) 0.0697(6) 0.050(3) Uani 1 1 d D . . . .
Si4 Si 0.6667 0.3333 0.1360(11) 0.046(4) Uani 1 3 d DS T P . .
Si5 Si 0.5237(5) 0.4426(5) 0.0455(5) 0.043(3) Uani 1 1 d . . . . .
Si6 Si 0.0769(9) 0.4016(11) 0.2500 0.094(6) Uani 1 2 d DS T P . .
Si7 Si 0.1327(12) 0.4458(13) 0.0471(12) 0.087(7) Uani 0.62(2) 1 d D U P . .
Si8 Si 0.0000 0.280(2) 0.5000 0.10(2) Uani 0.23(4) 2 d DS TU P . .
Si9 Si -0.0360(18) 0.229(2) 0.286(3) 0.15(2) Uani 0.20(3) 1 d D U P . .
Si10 Si 0.1810(14) 0.5078(15) 0.0795(16) 0.101(9) Uani 0.38(2) 1 d D U P . .
Si12 Si 0.3333 0.6667 0.152(3) 0.16(3) Uani 0.19(5) 3 d DS TU P . .
O1 O 0.4122(12) -0.0085(14) 0.2500 0.119(10) Uani 1 2 d DS TU P . .
O2 O 0.5387(15) 0.0744(16) 0.1603(14) 0.120(8) Uani 1 1 d . . . . .
O3 O 0.4739(18) 0.1440(17) 0.2500 0.107(10) Uani 1 2 d DS T P . .
O4 O 0.3317(13) 0.1208(17) 0.2500 0.121(11) Uani 1 2 d DS T P . .
O5 O 0.4375(13) 0.2348(15) 0.1563(14) 0.108(7) Uani 1 1 d . . . . .
O6 O 0.5826(10) 0.3093(15) 0.100(2) 0.127(8) Uani 1 1 d D . . . .
O7 O 0.4880(13) 0.3522(12) 0.0311(15) 0.096(7) Uani 1 1 d . U . . .
O8 O 0.6667 0.3333 0.2500 0.15(3) Uani 1 6 d S T P . .
O9 O 0.4647(12) 0.4647(12) 0.0000 0.081(7) Uani 1 2 d S T P . .
O10 O 0.3665(19) 0.0757(14) 0.004(2) 0.147(17) Uani 0.62(2) 1 d . U P . .
O11 O 0.038(2) 0.3112(12) 0.2500 0.192(17) Uani 1 2 d DS TU P . .
O12 O 0.1326(10) 0.4451(10) 0.1584(8) 0.138(8) Uani 1 1 d D U . . .
O13 O 0.1201(12) 0.5154(11) 0.0148(17) 0.110(7) Uani 1 1 d D . . . .
O14 O 0.2208(10) 0.4688(13) 0.0157(12) 0.103(6) Uani 1 1 d D U . . .
O15 O 0.001(5) 0.233(4) 0.405(2) 0.14(2) Uani 0.23(4) 1 d D U P . .
O16 O -0.038(4) 0.228(4) 0.402(3) 0.14(2) Uani 0.20(3) 1 d D U P . .
O17 O -0.021(5) 0.160(3) 0.2500 0.14(2) Uani 0.41(5) 2 d DS TU P . .
O18 O 0.2497(13) 0.5886(13) 0.121(2) 0.186(19) Uani 0.38(2) 1 d D U P . .
O21 O 0.3333 0.6667 0.270(3) 0.17(3) Uani 0.19(5) 3 d DS 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
Si1 O1 1.575(13) . ?
Si1 O3 1.58(3) . ?
Si1 O2 1.58(2) 4 ?
Si1 O2 1.58(2) . ?
Si2 O5 1.57(2) 4 ?
Si2 O5 1.57(2) . ?
Si2 O4 1.60(2) . ?
Si2 O3 1.60(2) . ?
Si3 O14 1.564(16) 7 ?
Si3 O6 1.570(17) . ?
Si3 O5 1.60(2) . ?
Si3 O7 1.61(2) . ?
Si4 O6 1.568(16) 2_655 ?
Si4 O6 1.568(16) 3_665 ?
Si4 O6 1.568(16) . ?
Si4 O8 1.586(15) . ?
Si5 O9 1.572(10) . ?
Si5 O7 1.58(2) . ?
Si5 O13 1.623(18) 8_665 ?
Si5 O2 1.63(2) 3_665 ?
Si6 O11 1.56(2) . ?
Si6 O1 1.579(13) 2 ?
Si6 O12 1.624(15) 4 ?
Si6 O12 1.624(15) . ?
Si7 Si10 1.20(3) . ?
Si7 O12 1.549(17) . ?
Si7 O10 1.57(2) 7 ?
Si7 O13 1.58(2) . ?
Si7 O14 1.63(2) . ?
Si8 O15 1.61(2) . ?
Si8 O15 1.61(2) 9_556 ?
Si8 O10 1.62(2) 10 ?
Si8 O10 1.62(2) 5 ?
Si8 O16 1.64(6) . ?
Si8 O16 1.64(6) 9_556 ?
Si9 Si9 1.00(9) 4 ?
Si9 O16 1.61(3) . ?
Si9 O4 1.61(3) 2 ?
Si9 O17 1.62(3) . ?
Si9 O11 1.63(3) . ?
Si9 O15 1.80(6) . ?
Si10 O13 1.57(2) . ?
Si10 O12 1.57(2) . ?
Si10 O18 1.61(2) . ?
Si10 O14 1.62(2) . ?
Si12 O21 1.08(7) 4 ?
Si12 O21 1.64(2) . ?
Si12 O18 1.661(10) 3_565 ?
Si12 O18 1.661(10) . ?
Si12 O18 1.661(10) 2_665 ?
O1 Si6 1.579(13) 3 ?
O2 Si5 1.63(2) 2_655 ?
O4 Si9 1.61(3) 6 ?
O4 Si9 1.61(3) 3 ?
O8 Si4 1.586(15) 4 ?
O9 Si5 1.572(10) 7 ?
O10 Si7 1.57(2) 7 ?
O10 Si8 1.62(2) 6 ?
O11 Si9 1.63(3) 4 ?
O13 Si5 1.623(18) 8_565 ?
O14 Si3 1.564(16) 7 ?
O15 O16 0.73(10) . ?
O17 Si9 1.62(3) 4 ?
O21 O21 0.57(7) 4 ?
O21 Si12 1.08(7) 4 ?
 
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 O3 113(2) . . ?
O1 Si1 O2 106.8(13) . 4 ?
O3 Si1 O2 112.4(13) . 4 ?
O1 Si1 O2 106.8(13) . . ?
O3 Si1 O2 112.4(13) . . ?
O2 Si1 O2 104.4(19) 4 . ?
O5 Si2 O5 112(2) 4 . ?
O5 Si2 O4 106.9(12) 4 . ?
O5 Si2 O4 106.9(12) . . ?
O5 Si2 O3 110.3(11) 4 . ?
O5 Si2 O3 110.3(11) . . ?
O4 Si2 O3 110(2) . . ?
O14 Si3 O6 112.7(15) 7 . ?
O14 Si3 O5 105.7(13) 7 . ?
O6 Si3 O5 110.7(13) . . ?
O14 Si3 O7 105.3(11) 7 . ?
O6 Si3 O7 109.8(13) . . ?
O5 Si3 O7 112.6(12) . . ?
O6 Si4 O6 110.4(12) 2_655 3_665 ?
O6 Si4 O6 110.4(12) 2_655 . ?
O6 Si4 O6 110.4(12) 3_665 . ?
O6 Si4 O8 108.5(12) 2_655 . ?
O6 Si4 O8 108.5(12) 3_665 . ?
O6 Si4 O8 108.5(12) . . ?
O9 Si5 O7 106.9(12) . . ?
O9 Si5 O13 109.4(11) . 8_665 ?
O7 Si5 O13 106.5(13) . 8_665 ?
O9 Si5 O2 112.0(11) . 3_665 ?
O7 Si5 O2 108.3(13) . 3_665 ?
O13 Si5 O2 113.3(13) 8_665 3_665 ?
O11 Si6 O1 107(3) . 2 ?
O11 Si6 O12 115.2(11) . 4 ?
O1 Si6 O12 108.1(12) 2 4 ?
O11 Si6 O12 115.2(11) . . ?
O1 Si6 O12 108.1(12) 2 . ?
O12 Si6 O12 103.5(14) 4 . ?
Si10 Si7 O12 68.3(14) . . ?
Si10 Si7 O10 174(2) . 7 ?
O12 Si7 O10 116.6(17) . 7 ?
Si10 Si7 O13 67.0(15) . . ?
O12 Si7 O13 106.9(15) . . ?
O10 Si7 O13 113(2) 7 . ?
Si10 Si7 O14 67.8(15) . . ?
O12 Si7 O14 105.5(13) . . ?
O10 Si7 O14 106.9(16) 7 . ?
O13 Si7 O14 107.1(15) . . ?
O15 Si8 O15 110(4) . 9_556 ?
O15 Si8 O10 111(3) . 10 ?
O15 Si8 O10 109(3) 9_556 10 ?
O15 Si8 O10 109(3) . 5 ?
O15 Si8 O10 111(3) 9_556 5 ?
O10 Si8 O10 107(3) 10 5 ?
O15 Si8 O16 26(4) . . ?
O15 Si8 O16 117(4) 9_556 . ?
O10 Si8 O16 125(3) 10 . ?
O10 Si8 O16 84(3) 5 . ?
O15 Si8 O16 117(4) . 9_556 ?
O15 Si8 O16 26(4) 9_556 9_556 ?
O10 Si8 O16 84(3) 10 9_556 ?
O10 Si8 O16 125(3) 5 9_556 ?
O16 Si8 O16 134(6) . 9_556 ?
Si9 Si9 O16 179(3) 4 . ?
Si9 Si9 O4 71.9(17) 4 2 ?
O16 Si9 O4 107(3) . 2 ?
Si9 Si9 O17 72.0(17) 4 . ?
O16 Si9 O17 108(3) . . ?
O4 Si9 O17 109(4) 2 . ?
Si9 Si9 O11 72.1(16) 4 . ?
O16 Si9 O11 109(3) . . ?
O4 Si9 O11 116(3) 2 . ?
O17 Si9 O11 107(3) . . ?
Si9 Si9 O15 157(2) 4 . ?
O16 Si9 O15 24(3) . . ?
O4 Si9 O15 131(3) 2 . ?
O17 Si9 O15 95(2) . . ?
O11 Si9 O15 95(3) . . ?
Si7 Si10 O13 68.1(14) . . ?
Si7 Si10 O12 66.3(14) . . ?
O13 Si10 O12 106.4(17) . . ?
Si7 Si10 O18 176(2) . . ?
O13 Si10 O18 114.9(17) . . ?
O12 Si10 O18 114.4(15) . . ?
Si7 Si10 O14 68.7(16) . . ?
O13 Si10 O14 108.2(17) . . ?
O12 Si10 O14 104.9(16) . . ?
O18 Si10 O14 107.6(19) . . ?
O21 Si12 O21 0.005(3) 4 . ?
O21 Si12 O18 104.9(11) 4 3_565 ?
O21 Si12 O18 104.9(11) . 3_565 ?
O21 Si12 O18 104.9(11) 4 . ?
O21 Si12 O18 104.9(11) . . ?
O18 Si12 O18 113.6(9) 3_565 . ?
O21 Si12 O18 104.9(11) 4 2_665 ?
O21 Si12 O18 104.9(11) . 2_665 ?
O18 Si12 O18 113.6(9) 3_565 2_665 ?
O18 Si12 O18 113.6(9) . 2_665 ?
Si1 O1 Si6 165(3) . 3 ?
Si1 O2 Si5 152.8(18) . 2_655 ?
Si1 O3 Si2 156(2) . . ?
Si2 O4 Si9 147(3) . 6 ?
Si2 O4 Si9 147(3) . 3 ?
Si9 O4 Si9 36(3) 6 3 ?
Si2 O5 Si3 146.8(14) . . ?
Si4 O6 Si3 175.8(19) . . ?
Si5 O7 Si3 141.3(13) . . ?
Si4 O8 Si4 180.0 . 4 ?
Si5 O9 Si5 153.1(18) 7 . ?
Si7 O10 Si8 150(2) 7 6 ?
Si6 O11 Si9 146(3) . . ?
Si6 O11 Si9 146(3) . 4 ?
Si9 O11 Si9 36(3) . 4 ?
Si7 O12 Si10 45.4(11) . . ?
Si7 O12 Si6 141.9(14) . . ?
Si10 O12 Si6 162.0(17) . . ?
Si10 O13 Si7 44.9(11) . . ?
Si10 O13 Si5 158.4(17) . 8_565 ?
Si7 O13 Si5 156.2(17) . 8_565 ?
Si3 O14 Si10 135.5(16) 7 . ?
Si3 O14 Si7 144.6(14) 7 . ?
Si10 O14 Si7 43.6(11) . . ?
O16 O15 Si8 80(5) . . ?
O16 O15 Si9 64(4) . . ?
Si8 O15 Si9 131(4) . . ?
O15 O16 Si9 93(5) . . ?
O15 O16 Si8 75(5) . . ?
Si9 O16 Si8 146(5) . . ?
Si9 O17 Si9 36(3) . 4 ?
Si10 O18 Si12 167(3) . . ?
O21 O21 Si12 179.985(9) 4 4 ?
O21 O21 Si12 0.010(6) 4 . ?
Si12 O21 Si12 179.995(16) 4 . ?
 
_refine_diff_density_max    0.247
_refine_diff_density_min   -0.282
_refine_diff_density_rms    0.092



# start Validation Reply Form

_vrf_PLAT082_ECNU-45_treated_for_6h
;
PROBLEM: High R1 Value ..................................       0.17 Report
RESPONSE: This is mainly the result of multiple scattering of electrons in the crystal
;
_vrf_PLAT084_ECNU-45_treated_for_6h
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.37 Report
RESPONSE: This is mainly the result of multiple scattering of electrons in the crystal
;
_vrf_THETM01_ECNU-45_treated_for_6h
;
PROBLEM:  The value of sine(theta_max)/wavelength is less than 0.550  Calculated sin(theta_max)/wavelength =    0.4999
RESPONSE: The radiation source is electron, the wavelength is 0.0251 Å. The calculated sin(theta_max)/wavelength) is 28.6
;
_vrf_PLAT602_ECNU-45_treated_for_6h
;
PROBLEM:  Solvent Accessible VOID(S) in Structure ........    
RESPONSE: This is a porous zeolite structure.
;