 
data_ECNU-45_treated_for_10h
 
_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
 'O1.56 Si0.74' 
_chemical_formula_weight          45.65

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                    19.807(3)
_cell_length_b                    19.807(3)
_cell_length_c                    14.118(3)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      4796.8(17)
_cell_formula_units_Z             83
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     7605
_cell_measurement_theta_min       0.066
_cell_measurement_theta_max       0.717
 
_exptl_crystal_description        hexagonal
_exptl_crystal_colour             ?
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.312          
_exptl_crystal_F_000              612
_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             7605
_diffrn_reflns_av_unetI/netI      0.2023
_diffrn_reflns_av_R_equivalents   0.2476
_diffrn_reflns_limit_h_min        -19
_diffrn_reflns_limit_h_max        19
_diffrn_reflns_limit_k_min        -19
_diffrn_reflns_limit_k_max        19
_diffrn_reflns_limit_l_min        -14
_diffrn_reflns_limit_l_max        14
_diffrn_reflns_theta_min          0.066
_diffrn_reflns_theta_max          0.717
_diffrn_reflns_theta_full         0.717
_diffrn_measured_fraction_theta_max   0.995
_diffrn_measured_fraction_theta_full  0.995
_diffrn_reflns_Laue_measured_fraction_max    0.995
_diffrn_reflns_Laue_measured_fraction_full   0.995
_diffrn_reflns_point_group_measured_fraction_max   0.993
_diffrn_reflns_point_group_measured_fraction_full  0.993
_reflns_number_total              1750
_reflns_number_gt                 1002
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.795
_reflns_Friedel_fraction_max      0.991
_reflns_Friedel_fraction_full     0.991
 
_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)+(0.1712P)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          1750
_refine_ls_number_parameters      178
_refine_ls_number_restraints      74
_refine_ls_R_factor_all           0.1671
_refine_ls_R_factor_gt            0.1378
_refine_ls_wR_factor_ref          0.3367
_refine_ls_wR_factor_gt           0.3146
_refine_ls_goodness_of_fit_ref    1.011
_refine_ls_restrained_S_all       1.016
_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 0.4799(8) 0.0636(7) 0.2500 0.058(4) Uani 1 2 d DS T P . .
Si2 Si 0.4158(10) 0.1775(10) 0.2500 0.088(6) Uani 1 2 d S T P . .
Si3 Si 0.4951(6) 0.2805(6) 0.0757(8) 0.062(3) Uani 1 1 d . . . . .
Si4 Si 0.6667 0.3333 0.1386(11) 0.064(5) Uani 1 3 d DS T P . .
Si5 Si 0.5242(6) 0.4436(6) 0.0508(5) 0.053(3) Uani 1 1 d D . . . .
Si6 Si 0.0929(9) 0.4141(10) 0.2500 0.088(6) Uani 1 2 d DS TU P . .
Si7 Si 0.139(4) 0.453(3) 0.048(2) 0.05(2) Uani 0.17(3) 1 d D U P . .
Si10 Si 0.1826(8) 0.5124(9) 0.0695(7) 0.066(5) Uani 0.83(3) 1 d D U P . .
Si12 Si 0.3333 0.6667 0.1395(17) 0.064(10) Uani 0.78(6) 3 d S TU P . .
O1 O 0.4004(14) -0.0140(15) 0.2500 0.146(13) Uani 1 2 d DS T P . .
O2 O 0.5256(14) 0.0647(13) 0.1573(12) 0.118(8) Uani 1 1 d . . . . .
O3 O 0.471(2) 0.1390(19) 0.2500 0.114(11) Uani 1 2 d S T P . .
O4 O 0.325(2) 0.118(2) 0.2500 0.139(12) Uani 1 2 d S TU P . .
O5 O 0.4373(12) 0.2323(13) 0.1567(14) 0.114(7) Uani 1 1 d . . . . .
O6 O 0.5844(10) 0.3133(13) 0.1017(16) 0.111(7) Uani 1 1 d D . . . .
O7 O 0.4831(14) 0.3521(11) 0.0502(16) 0.119(8) Uani 1 1 d D . . . .
O8 O 0.6667 0.3333 0.2500 0.225(17) Uani 1 6 d DS TU P . .
O9 O 0.4608(15) 0.4608(15) 0.0000 0.096(8) Uani 1 2 d S T P . .
O10 O 0.367(3) 0.075(4) -0.011(6) 0.21(2) Uani 0.17(3) 1 d . U P . .
O11 O 0.072(4) 0.324(2) 0.2500 0.24(2) Uani 1 2 d DS TU P . .
O12 O 0.1436(14) 0.4553(17) 0.1597(16) 0.134(8) Uani 1 1 d D U . . .
O13 O 0.1220(10) 0.5185(10) 0.0042(12) 0.085(5) Uani 1 1 d D . . . .
O14 O 0.2240(13) 0.4733(13) 0.0121(14) 0.106(7) Uani 1 1 d D . . . .
O18 O 0.2487(16) 0.5974(14) 0.1068(19) 0.127(10) Uani 0.83(3) 1 d D U P . .
O21 O 0.3333 0.6667 0.2500 0.111(19) Uani 0.78(6) 6 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
Si1 O1 1.556(17) . ?
Si1 O2 1.58(2) . ?
Si1 O2 1.58(2) 4 ?
Si1 O3 1.59(3) . ?
Si2 O4 1.58(4) . ?
Si2 O3 1.61(3) . ?
Si2 O5 1.62(2) 4 ?
Si2 O5 1.62(2) . ?
Si3 O5 1.56(2) . ?
Si3 O14 1.58(2) 7 ?
Si3 O6 1.592(18) . ?
Si3 O7 1.59(2) . ?
Si4 O6 1.562(15) 2_655 ?
Si4 O6 1.562(15) 3_665 ?
Si4 O6 1.562(15) . ?
Si4 O8 1.572(15) . ?
Si5 O13 1.565(18) 8_665 ?
Si5 O7 1.572(19) . ?
Si5 O2 1.595(18) 3_665 ?
Si5 O9 1.624(12) . ?
Si6 O1 1.567(17) 2 ?
Si6 O12 1.57(2) 4 ?
Si6 O12 1.57(2) . ?
Si6 O11 1.62(3) . ?
Si7 Si10 1.09(5) . ?
Si7 O12 1.58(3) . ?
Si7 O14 1.61(6) . ?
Si7 O13 1.61(3) . ?
Si7 O10 1.62(7) 7 ?
Si10 O13 1.565(18) . ?
Si10 O14 1.60(3) . ?
Si10 O18 1.62(2) . ?
Si10 O12 1.62(3) . ?
Si12 O21 1.56(2) . ?
Si12 O18 1.61(3) 2_665 ?
Si12 O18 1.61(3) . ?
Si12 O18 1.61(3) 3_565 ?
O1 Si6 1.567(17) 3 ?
O2 Si5 1.595(18) 2_655 ?
O8 Si4 1.572(15) 4 ?
O9 Si5 1.624(12) 7 ?
O10 Si7 1.62(7) 7 ?
O13 Si5 1.565(18) 8_565 ?
O14 Si3 1.58(2) 7 ?
O21 Si12 1.56(2) 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 O2 107.6(12) . . ?
O1 Si1 O2 107.6(12) . 4 ?
O2 Si1 O2 111(2) . 4 ?
O1 Si1 O3 113(2) . . ?
O2 Si1 O3 108.6(12) . . ?
O2 Si1 O3 108.6(12) 4 . ?
O4 Si2 O3 116(2) . . ?
O4 Si2 O5 108.6(13) . 4 ?
O3 Si2 O5 107.6(12) . 4 ?
O4 Si2 O5 108.6(13) . . ?
O3 Si2 O5 107.6(12) . . ?
O5 Si2 O5 108.5(18) 4 . ?
O5 Si3 O14 106.6(13) . 7 ?
O5 Si3 O6 114.0(13) . . ?
O14 Si3 O6 108.9(13) 7 . ?
O5 Si3 O7 108.7(13) . . ?
O14 Si3 O7 110.1(13) 7 . ?
O6 Si3 O7 108.5(13) . . ?
O6 Si4 O6 109.4(10) 2_655 3_665 ?
O6 Si4 O6 109.4(10) 2_655 . ?
O6 Si4 O6 109.4(10) 3_665 . ?
O6 Si4 O8 109.5(10) 2_655 . ?
O6 Si4 O8 109.5(10) 3_665 . ?
O6 Si4 O8 109.5(10) . . ?
O13 Si5 O7 111.6(11) 8_665 . ?
O13 Si5 O2 109.6(12) 8_665 3_665 ?
O7 Si5 O2 109.6(13) . 3_665 ?
O13 Si5 O9 112.1(11) 8_665 . ?
O7 Si5 O9 103.3(13) . . ?
O2 Si5 O9 110.5(10) 3_665 . ?
O1 Si6 O12 112.1(13) 2 4 ?
O1 Si6 O12 112.1(13) 2 . ?
O12 Si6 O12 108(2) 4 . ?
O1 Si6 O11 108(3) 2 . ?
O12 Si6 O11 108.5(17) 4 . ?
O12 Si6 O11 108.5(17) . . ?
Si10 Si7 O12 72(2) . . ?
Si10 Si7 O14 70(3) . . ?
O12 Si7 O14 106(3) . . ?
Si10 Si7 O13 67.5(19) . . ?
O12 Si7 O13 113(3) . . ?
O14 Si7 O13 107(3) . . ?
Si10 Si7 O10 177(4) . 7 ?
O12 Si7 O10 111(4) . 7 ?
O14 Si7 O10 109(4) . 7 ?
O13 Si7 O10 111(4) . 7 ?
Si7 Si10 O13 72.2(17) . . ?
Si7 Si10 O14 70(3) . . ?
O13 Si10 O14 109.8(12) . . ?
Si7 Si10 O18 176(2) . . ?
O13 Si10 O18 111.4(16) . . ?
O14 Si10 O18 108.9(16) . . ?
Si7 Si10 O12 67.9(18) . . ?
O13 Si10 O12 113.6(13) . . ?
O14 Si10 O12 103.9(14) . . ?
O18 Si10 O12 109.0(15) . . ?
O21 Si12 O18 106.6(13) . 2_665 ?
O21 Si12 O18 106.6(13) . . ?
O18 Si12 O18 112.2(12) 2_665 . ?
O21 Si12 O18 106.6(13) . 3_565 ?
O18 Si12 O18 112.2(12) 2_665 3_565 ?
O18 Si12 O18 112.2(12) . 3_565 ?
Si1 O1 Si6 179(3) . 3 ?
Si1 O2 Si5 160.2(18) . 2_655 ?
Si1 O3 Si2 150(3) . . ?
Si3 O5 Si2 150.6(17) . . ?
Si4 O6 Si3 170.3(16) . . ?
Si5 O7 Si3 143.5(16) . . ?
Si4 O8 Si4 180.0 . 4 ?
Si5 O9 Si5 147(2) 7 . ?
Si6 O12 Si7 141(3) . . ?
Si6 O12 Si10 163(2) . . ?
Si7 O12 Si10 40(2) . . ?
Si5 O13 Si10 159.1(14) 8_565 . ?
Si5 O13 Si7 161(2) 8_565 . ?
Si10 O13 Si7 40(2) . . ?
Si3 O14 Si10 136.8(16) 7 . ?
Si3 O14 Si7 145.8(19) 7 . ?
Si10 O14 Si7 39.9(17) . . ?
Si12 O18 Si10 159(2) . . ?
Si12 O21 Si12 180.0 4 . ?
 
_refine_diff_density_max    0.147
_refine_diff_density_min   -0.152
_refine_diff_density_rms    0.041



# start Validation Reply Form

_vrf_PLAT020_ECNU-45_treated_for_10h
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.248 Report
RESPONSE: This is mainly the result of multiple scattering of electrons in the crystal.
;
_vrf_THETM01_ECNU-45_treated_for_10h
;
PROBLEM:  The value of sine(theta_max)/wavelength is less than 0.550  Calculated sin(theta_max)/wavelength =    0.4986
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_10h
;
PROBLEM:  Solvent Accessible VOID(S) in Structure ........    
RESPONSE: This is a porous zeolite structure.
;