 
data_ECNU-45_treated_for_8h
 
_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
 'O1.61 Si0.76' 
_chemical_formula_weight          47.05

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                    19.772(3)
_cell_length_b                    19.772(3)
_cell_length_c                    14.088(3)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      4769.7(17)
_cell_formula_units_Z             83
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     4840
_cell_measurement_theta_min       0.042
_cell_measurement_theta_max       0.747
 
_exptl_crystal_description        hexagonal
_exptl_crystal_colour             ?
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.359          
_exptl_crystal_F_000              631
_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             4840
_diffrn_reflns_av_unetI/netI      0.1275
_diffrn_reflns_av_R_equivalents   0.1054
_diffrn_reflns_limit_h_min        -19
_diffrn_reflns_limit_h_max        20
_diffrn_reflns_limit_k_min        -20
_diffrn_reflns_limit_k_max        19
_diffrn_reflns_limit_l_min        -14
_diffrn_reflns_limit_l_max        14
_diffrn_reflns_theta_min          0.042
_diffrn_reflns_theta_max          0.747
_diffrn_reflns_theta_full         0.747
_diffrn_measured_fraction_theta_max   0.987
_diffrn_measured_fraction_theta_full  0.986
_diffrn_reflns_Laue_measured_fraction_max    0.987
_diffrn_reflns_Laue_measured_fraction_full   0.986
_diffrn_reflns_point_group_measured_fraction_max   0.938
_diffrn_reflns_point_group_measured_fraction_full  0.937
_reflns_number_total              1860
_reflns_number_gt                 1027
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.714
_reflns_Friedel_fraction_max      0.876
_reflns_Friedel_fraction_full     0.876
 
_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          1860
_refine_ls_number_parameters      222
_refine_ls_number_restraints      159
_refine_ls_R_factor_all           0.1877
_refine_ls_R_factor_gt            0.1454
_refine_ls_wR_factor_ref          0.3579
_refine_ls_wR_factor_gt           0.3294
_refine_ls_goodness_of_fit_ref    1.119
_refine_ls_restrained_S_all       1.124
_refine_ls_shift/su_max           0.003
_refine_ls_shift/su_mean          0.001
 
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 0.4774(8) 0.0644(7) 0.2500 0.070(4) Uani 1 2 d DS T P . .
Si2 Si 0.4117(9) 0.1777(9) 0.2500 0.095(6) Uani 1 2 d DS TU P . .
Si3 Si 0.4931(6) 0.2811(6) 0.0755(6) 0.072(3) Uani 1 1 d D . . . .
Si4 Si 0.6667 0.3333 0.1395(12) 0.067(4) Uani 1 3 d DS TU P . .
Si5 Si 0.5277(6) 0.4472(6) 0.0507(5) 0.066(3) Uani 1 1 d . U . . .
Si6 Si 0.0903(10) 0.4058(11) 0.2500 0.113(6) Uani 1 2 d DS TU P . .
Si7 Si 0.1386(18) 0.447(2) 0.0479(19) 0.084(12) Uani 0.24(2) 1 d D U P . .
Si8 Si 0.0000 0.284(5) 0.5000 0.18(4) Uani 0.13(4) 2 d DS TU P . .
Si9 Si -0.024(2) 0.234(3) 0.295(5) 0.19(3) Uani 0.10(3) 1 d D U P . .
Si10 Si 0.1828(8) 0.5079(9) 0.0741(7) 0.078(5) Uani 0.76(2) 1 d D U P . .
Si12 Si 0.3333 0.6667 0.1390(11) 0.071(9) Uani 0.72(5) 3 d DS TU P . .
O1 O 0.4030(12) -0.0196(12) 0.2500 0.152(12) Uani 1 2 d DS T P . .
O2 O 0.5225(15) 0.0663(12) 0.1579(10) 0.135(8) Uani 1 1 d . . . . .
O3 O 0.4612(19) 0.1338(18) 0.2500 0.139(12) Uani 1 2 d DS T P . .
O4 O 0.3206(15) 0.1070(19) 0.2500 0.23(2) Uani 1 2 d DS TU P . .
O5 O 0.4342(12) 0.2322(13) 0.1556(14) 0.131(7) Uani 1 1 d D . . . .
O6 O 0.5813(12) 0.3071(14) 0.1061(18) 0.151(8) Uani 1 1 d D . . . .
O7 O 0.4864(14) 0.3559(14) 0.0511(14) 0.128(7) Uani 1 1 d . . . . .
O8 O 0.6667 0.3333 0.2500 0.188(19) Uani 1 6 d S TU P . .
O9 O 0.4686(14) 0.4686(14) 0.0000 0.098(7) Uani 1 2 d S TU P . .
O10 O 0.368(5) 0.0775(17) 0.002(6) 0.26(8) Uani 0.24(2) 1 d . U P . .
O11 O 0.050(2) 0.3114(12) 0.2500 0.252(19) Uani 1 2 d DS TU P . .
O12 O 0.1401(12) 0.4481(13) 0.1597(13) 0.143(7) Uani 1 1 d D U . . .
O13 O 0.1235(11) 0.5146(13) 0.0060(10) 0.110(6) Uani 1 1 d D . . . .
O14 O 0.2250(12) 0.4706(13) 0.0138(14) 0.127(7) Uani 1 1 d D . . . .
O15 O 0.004(9) 0.240(9) 0.406(2) 0.20(3) Uani 0.13(4) 1 d D U P . .
O16 O -0.027(5) 0.248(10) 0.408(3) 0.20(3) Uani 0.10(3) 1 d D U P . .
O17 O -0.011(5) 0.161(4) 0.278(14) 0.20(4) Uani 0.10(3) 1 d D U P . .
O18 O 0.2469(16) 0.5963(16) 0.1028(18) 0.129(8) Uani 0.76(2) 1 d D U P . .
O21 O 0.3333 0.6667 0.2500 0.095(13) Uani 0.73(5) 6 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 O2 1.56(2) . ?
Si1 O2 1.56(2) 4 ?
Si1 O3 1.56(3) . ?
Si1 O1 1.574(13) . ?
Si2 O3 1.60(2) . ?
Si2 O5 1.628(19) . ?
Si2 O5 1.628(19) 4 ?
Si2 O4 1.64(2) . ?
Si3 O5 1.562(17) . ?
Si3 O7 1.59(3) . ?
Si3 O14 1.587(19) 7 ?
Si3 O6 1.61(2) . ?
Si4 O8 1.557(16) . ?
Si4 O6 1.57(2) 2_655 ?
Si4 O6 1.57(2) . ?
Si4 O6 1.57(2) 3_665 ?
Si5 O7 1.57(2) . ?
Si5 O2 1.597(18) 3_665 ?
Si5 O9 1.597(10) . ?
Si5 O13 1.604(18) 8_665 ?
Si6 O12 1.569(19) 4 ?
Si6 O12 1.569(19) . ?
Si6 O1 1.591(19) 2 ?
Si6 O11 1.621(13) . ?
Si7 Si10 1.13(3) . ?
Si7 O12 1.58(2) . ?
Si7 O10 1.58(3) 7 ?
Si7 O14 1.60(2) . ?
Si7 O13 1.61(3) . ?
Si8 O16 1.45(9) 9_556 ?
Si8 O16 1.45(9) . ?
Si8 O10 1.60(3) 10 ?
Si8 O10 1.60(3) 5 ?
Si8 O15 1.61(3) . ?
Si8 O15 1.61(3) 9_556 ?
Si9 Si9 1.28(13) 4 ?
Si9 O16 1.61(3) . ?
Si9 O4 1.61(3) 2 ?
Si9 O17 1.61(3) . ?
Si9 O11 1.62(3) . ?
Si9 O15 1.64(8) . ?
Si9 O17 1.90(16) 4 ?
Si10 O13 1.571(17) . ?
Si10 O12 1.60(2) . ?
Si10 O14 1.61(2) . ?
Si10 O18 1.62(3) . ?
Si12 O21 1.564(16) . ?
Si12 O18 1.66(3) 3_565 ?
Si12 O18 1.66(3) 2_665 ?
Si12 O18 1.66(3) . ?
O1 Si6 1.591(19) 3 ?
O2 Si5 1.597(18) 2_655 ?
O4 Si9 1.61(3) 6 ?
O4 Si9 1.61(3) 3 ?
O8 Si4 1.557(16) 4 ?
O9 Si5 1.597(10) 7 ?
O10 Si7 1.58(3) 7 ?
O10 Si8 1.60(3) 6 ?
O11 Si9 1.62(3) 4 ?
O13 Si5 1.604(18) 8_565 ?
O14 Si3 1.587(19) 7 ?
O15 O16 0.70(18) . ?
O17 O17 0.8(4) 4 ?
O17 Si9 1.90(16) 4 ?
O21 Si12 1.564(16) 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
O2 Si1 O2 112.2(19) . 4 ?
O2 Si1 O3 110.1(11) . . ?
O2 Si1 O3 110.1(11) 4 . ?
O2 Si1 O1 104.3(11) . . ?
O2 Si1 O1 104.3(11) 4 . ?
O3 Si1 O1 116(2) . . ?
O3 Si2 O5 108.7(11) . . ?
O3 Si2 O5 108.7(11) . 4 ?
O5 Si2 O5 109.6(19) . 4 ?
O3 Si2 O4 104.4(19) . . ?
O5 Si2 O4 112.6(11) . . ?
O5 Si2 O4 112.6(11) 4 . ?
O5 Si3 O7 110.5(13) . . ?
O5 Si3 O14 106.1(13) . 7 ?
O7 Si3 O14 110.8(13) . 7 ?
O5 Si3 O6 110.9(13) . . ?
O7 Si3 O6 110.0(14) . . ?
O14 Si3 O6 108.4(14) 7 . ?
O8 Si4 O6 107.4(11) . 2_655 ?
O8 Si4 O6 107.4(11) . . ?
O6 Si4 O6 111.4(10) 2_655 . ?
O8 Si4 O6 107.4(11) . 3_665 ?
O6 Si4 O6 111.4(10) 2_655 3_665 ?
O6 Si4 O6 111.4(10) . 3_665 ?
O7 Si5 O2 108.7(13) . 3_665 ?
O7 Si5 O9 106.1(14) . . ?
O2 Si5 O9 111.0(10) 3_665 . ?
O7 Si5 O13 111.5(12) . 8_665 ?
O2 Si5 O13 109.2(12) 3_665 8_665 ?
O9 Si5 O13 110.2(10) . 8_665 ?
O12 Si6 O12 108.3(17) 4 . ?
O12 Si6 O1 105.7(12) 4 2 ?
O12 Si6 O1 105.7(12) . 2 ?
O12 Si6 O11 115.5(11) 4 . ?
O12 Si6 O11 115.5(11) . . ?
O1 Si6 O11 105.3(16) 2 . ?
Si10 Si7 O12 70.4(18) . . ?
Si10 Si7 O10 172(4) . 7 ?
O12 Si7 O10 117(4) . 7 ?
Si10 Si7 O14 69.4(18) . . ?
O12 Si7 O14 106.6(19) . . ?
O10 Si7 O14 109(2) 7 . ?
Si10 Si7 O13 67.1(16) . . ?
O12 Si7 O13 112(2) . . ?
O10 Si7 O13 107(5) 7 . ?
O14 Si7 O13 105(2) . . ?
O16 Si8 O16 143(10) 9_556 . ?
O16 Si8 O10 84(6) 9_556 10 ?
O16 Si8 O10 117(6) . 10 ?
O16 Si8 O10 117(6) 9_556 5 ?
O16 Si8 O10 84(6) . 5 ?
O10 Si8 O10 112(5) 10 5 ?
O16 Si8 O15 123(9) 9_556 . ?
O16 Si8 O15 26(7) . . ?
O10 Si8 O15 107(5) 10 . ?
O10 Si8 O15 110(4) 5 . ?
O16 Si8 O15 26(7) 9_556 9_556 ?
O16 Si8 O15 123(9) . 9_556 ?
O10 Si8 O15 110(4) 10 9_556 ?
O10 Si8 O15 107(5) 5 9_556 ?
O15 Si8 O15 111(5) . 9_556 ?
Si9 Si9 O16 169(6) 4 . ?
Si9 Si9 O4 67(2) 4 2 ?
O16 Si9 O4 109(3) . 2 ?
Si9 Si9 O17 81(6) 4 . ?
O16 Si9 O17 109(4) . . ?
O4 Si9 O17 108(3) 2 . ?
Si9 Si9 O11 67(2) 4 . ?
O16 Si9 O11 109(3) . . ?
O4 Si9 O11 114(2) 2 . ?
O17 Si9 O11 108(3) . . ?
Si9 Si9 O15 162(4) 4 . ?
O16 Si9 O15 25(7) . . ?
O4 Si9 O15 131(6) 2 . ?
O17 Si9 O15 90(8) . . ?
O11 Si9 O15 101(6) . . ?
Si9 Si9 O17 57(6) 4 4 ?
O16 Si9 O17 134(10) . 4 ?
O4 Si9 O17 96(6) 2 4 ?
O17 Si9 O17 24(10) . 4 ?
O11 Si9 O17 96(6) . 4 ?
O15 Si9 O17 114(5) . 4 ?
Si7 Si10 O13 71.2(14) . . ?
Si7 Si10 O12 67.8(14) . . ?
O13 Si10 O12 112.5(13) . . ?
Si7 Si10 O14 69.3(15) . . ?
O13 Si10 O14 107.2(12) . . ?
O12 Si10 O14 105.3(14) . . ?
Si7 Si10 O18 175.5(19) . . ?
O13 Si10 O18 106.0(16) . . ?
O12 Si10 O18 116.6(13) . . ?
O14 Si10 O18 108.9(15) . . ?
O21 Si12 O18 107.9(10) . 3_565 ?
O21 Si12 O18 107.9(10) . 2_665 ?
O18 Si12 O18 111.0(10) 3_565 2_665 ?
O21 Si12 O18 107.9(10) . . ?
O18 Si12 O18 111.0(10) 3_565 . ?
O18 Si12 O18 111.0(10) 2_665 . ?
Si1 O1 Si6 164(2) . 3 ?
Si1 O2 Si5 161.5(18) . 2_655 ?
Si1 O3 Si2 158(2) . . ?
Si9 O4 Si9 47(5) 6 3 ?
Si9 O4 Si2 145(4) 6 . ?
Si9 O4 Si2 145(4) 3 . ?
Si3 O5 Si2 150.8(16) . . ?
Si4 O6 Si3 178(2) . . ?
Si5 O7 Si3 146.8(17) . . ?
Si4 O8 Si4 180.0 4 . ?
Si5 O9 Si5 153(2) 7 . ?
Si7 O10 Si8 152(5) 7 6 ?
Si6 O11 Si9 141(3) . 4 ?
Si6 O11 Si9 141(3) . . ?
Si9 O11 Si9 46(5) 4 . ?
Si6 O12 Si7 143.3(18) . . ?
Si6 O12 Si10 164.2(19) . . ?
Si7 O12 Si10 41.8(13) . . ?
Si10 O13 Si5 159.6(16) . 8_565 ?
Si10 O13 Si7 41.7(12) . . ?
Si5 O13 Si7 158.5(18) 8_565 . ?
Si3 O14 Si7 144.4(19) 7 . ?
Si3 O14 Si10 137.9(16) 7 . ?
Si7 O14 Si10 41.4(13) . . ?
O16 O15 Si8 64(8) . . ?
O16 O15 Si9 75(6) . . ?
Si8 O15 Si9 135(5) . . ?
O15 O16 Si8 90(7) . . ?
O15 O16 Si9 80(8) . . ?
Si8 O16 Si9 158(6) . . ?
O17 O17 Si9 99(6) 4 . ?
O17 O17 Si9 57(6) 4 4 ?
Si9 O17 Si9 42(3) . 4 ?
Si10 O18 Si12 155(2) . . ?
Si12 O21 Si12 180.0 . 4 ?
 
_refine_diff_density_max    0.236
_refine_diff_density_min   -0.238
_refine_diff_density_rms    0.086



# start Validation Reply Form

_vrf_PLAT084_ECNU-45_treated_for_8h
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.36 Report
RESPONSE: This is mainly the result of multiple scattering of electrons in the crystal.
;
_vrf_THETM01_ECNU-45_treated_for_8h
;
PROBLEM:  The value of sine(theta_max)/wavelength is less than 0.550  Calculated sin(theta_max)/wavelength =    0.5194
RESPONSE: The radiation source is electron, the wavelength is 0.0251 Å. The calculated sin(theta_max)/wavelength) is 29.8
;
_vrf_PLAT602_ECNU-45_treated_for_8h
;
PROBLEM:  Solvent Accessible VOID(S) in Structure ........    
RESPONSE: This is a porous zeolite structure.
;