 
data_ECNU-45_treated_for_4h
 
_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
 'O1.67 Si0.76' 
_chemical_formula_weight          48.04

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                    19.895(3)
_cell_length_b                    19.895(3)
_cell_length_c                    13.699(3)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      4695.8(17)
_cell_formula_units_Z             83
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     6226
_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     1.410          
_exptl_crystal_F_000              642
_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             6226
_diffrn_reflns_av_unetI/netI      0.1401
_diffrn_reflns_av_R_equivalents   0.1516
_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        -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   0.960
_diffrn_measured_fraction_theta_full  0.960
_diffrn_reflns_Laue_measured_fraction_max    0.960
_diffrn_reflns_Laue_measured_fraction_full   0.960
_diffrn_reflns_point_group_measured_fraction_max   0.964
_diffrn_reflns_point_group_measured_fraction_full  0.964
_reflns_number_total              1665
_reflns_number_gt                 1099
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.806
_reflns_Friedel_fraction_max      0.969
_reflns_Friedel_fraction_full     0.969
 
_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          1665
_refine_ls_number_parameters      232
_refine_ls_number_restraints      134
_refine_ls_R_factor_all           0.1805
_refine_ls_R_factor_gt            0.1591
_refine_ls_wR_factor_ref          0.3606
_refine_ls_wR_factor_gt           0.3414
_refine_ls_goodness_of_fit_ref    1.219
_refine_ls_restrained_S_all       1.209
_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_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) 0.0727(7) 0.2500 0.042(4) Uani 1 2 d DS T P . .
Si2 Si 0.4203(9) 0.1842(9) 0.2500 0.067(5) Uani 1 2 d S T P . .
Si3 Si 0.4969(6) 0.2801(6) 0.0676(8) 0.052(3) Uani 1 1 d . . . . .
Si4 Si 0.6667 0.3333 0.1359(13) 0.053(5) Uani 1 3 d DS T P . .
Si5 Si 0.5239(5) 0.4422(5) 0.0450(8) 0.049(3) Uani 1 1 d . . . . .
Si6 Si 0.0707(9) 0.3939(11) 0.2500 0.089(6) Uani 1 2 d DS T P . .
Si7 Si 0.1300(11) 0.4420(13) 0.0413(17) 0.081(7) Uani 0.61(3) 1 d D U P . .
Si8 Si 0.0000 0.277(3) 0.5000 0.12(2) Uani 0.23(4) 2 d DS TU P . .
Si9 Si -0.041(2) 0.223(2) 0.291(3) 0.119(19) Uani 0.23(3) 1 d D U P . .
Si10 Si 0.1726(16) 0.5016(18) 0.0843(19) 0.103(11) Uani 0.39(3) 1 d D U P . .
Si11 Si 0.223(6) 0.616(5) 0.2500 0.15(3) Uani 0.14(4) 2 d DS TU P . .
O1 O 0.4115(11) -0.0054(17) 0.2500 0.121(11) Uani 1 2 d DS T P . .
O2 O 0.5362(14) 0.0757(13) 0.1562(18) 0.106(7) Uani 1 1 d . . . . .
O3 O 0.4758(18) 0.1452(18) 0.2500 0.097(10) Uani 1 2 d S T P . .
O4 O 0.3315(17) 0.1213(18) 0.2500 0.138(15) Uani 1 2 d S T P . .
O5 O 0.4376(12) 0.2372(14) 0.1570(19) 0.106(7) Uani 1 1 d . . . . .
O6 O 0.5836(11) 0.3101(13) 0.098(2) 0.116(8) Uani 1 1 d D . . . .
O7 O 0.4859(13) 0.3493(12) 0.0297(18) 0.101(8) Uani 1 1 d . . . . .
O8 O 0.6667 0.3333 0.2500 0.17(3) Uani 1 6 d DS T P . .
O9 O 0.4618(11) 0.4618(11) 0.0000 0.074(7) Uani 1 2 d S T P . .
O10 O 0.3635(16) 0.0748(14) 0.016(3) 0.118(14) Uani 0.61(3) 1 d . U P . .
O11 O 0.033(3) 0.2998(17) 0.2500 0.166(15) Uani 1 2 d DS TU P . .
O12 O 0.1234(14) 0.4281(16) 0.1573(16) 0.138(8) Uani 1 1 d D U . . .
O13 O 0.1123(13) 0.5107(11) 0.0151(18) 0.102(7) Uani 1 1 d D . . . .
O14 O 0.2211(9) 0.4725(12) 0.0181(14) 0.092(7) Uani 1 1 d D . . . .
O15 O 0.010(4) 0.235(4) 0.405(2) 0.14(2) Uani 0.23(4) 1 d D U P . .
O16 O -0.040(4) 0.224(4) 0.408(3) 0.13(2) Uani 0.23(3) 1 d D U P . .
O17 O -0.029(5) 0.153(4) 0.2500 0.14(2) Uani 0.47(6) 2 d DS TU P . .
O18 O 0.229(4) 0.575(2) 0.151(2) 0.18(3) Uani 0.39(3) 1 d D U P . .
O19 O 0.291(12) 0.705(4) 0.2500 0.17(4) Uani 0.14(4) 2 d DS TU P . .
O20 O 0.140(10) 0.612(13) 0.2500 0.17(4) Uani 0.14(4) 2 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 1.550(19) . ?
Si1 O2 1.57(2) . ?
Si1 O2 1.57(2) 4 ?
Si1 O3 1.59(3) . ?
Si2 O4 1.57(3) . ?
Si2 O5 1.58(3) 4 ?
Si2 O5 1.58(3) . ?
Si2 O3 1.64(3) . ?
Si3 O14 1.557(18) 7 ?
Si3 O6 1.57(2) . ?
Si3 O7 1.58(2) . ?
Si3 O5 1.62(3) . ?
Si4 O8 1.563(18) . ?
Si4 O6 1.565(18) 2_655 ?
Si4 O6 1.565(18) 3_665 ?
Si4 O6 1.565(18) . ?
Si5 O2 1.57(2) 3_665 ?
Si5 O13 1.58(2) 8_665 ?
Si5 O9 1.594(10) . ?
Si5 O7 1.62(2) . ?
Si6 O12 1.569(13) 4 ?
Si6 O12 1.569(13) . ?
Si6 O1 1.577(14) 2 ?
Si6 O11 1.63(3) . ?
Si7 Si10 1.21(3) . ?
Si7 O10 1.596(15) 7 ?
Si7 O12 1.61(3) . ?
Si7 O13 1.61(3) . ?
Si7 O14 1.63(2) . ?
Si8 O16 1.57(6) 9_556 ?
Si8 O16 1.57(6) . ?
Si8 O15 1.61(3) . ?
Si8 O15 1.61(3) 9_556 ?
Si8 O10 1.64(4) 10 ?
Si8 O10 1.64(4) 5 ?
Si9 Si9 1.11(8) 4 ?
Si9 O4 1.59(3) 2 ?
Si9 O11 1.60(3) . ?
Si9 O17 1.61(3) . ?
Si9 O16 1.61(3) . ?
Si9 O15 1.81(6) . ?
Si10 O13 1.61(3) . ?
Si10 O18 1.61(3) . ?
Si10 O14 1.63(2) . ?
Si10 O12 1.63(2) . ?
Si11 O19 1.61(3) . ?
Si11 O18 1.61(2) . ?
Si11 O18 1.61(2) 4 ?
Si11 O20 1.61(3) . ?
Si11 O19 1.8(2) 2_665 ?
O1 Si6 1.577(14) 3 ?
O2 Si5 1.57(2) 2_655 ?
O4 Si9 1.59(3) 6 ?
O4 Si9 1.59(3) 3 ?
O8 Si4 1.563(18) 4 ?
O9 Si5 1.594(10) 7 ?
O10 Si7 1.596(15) 7 ?
O10 Si8 1.64(4) 6 ?
O11 Si9 1.60(3) 4 ?
O13 Si5 1.58(2) 8_565 ?
O14 Si3 1.557(18) 7 ?
O15 O16 0.90(9) . ?
O17 Si9 1.61(3) 4 ?
O18 O19 1.82(9) 2_665 ?
O19 Si11 1.8(2) 3_565 ?
O19 O18 1.82(9) 6_565 ?
O19 O18 1.82(9) 3_565 ?
 
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 108.3(13) . . ?
O1 Si1 O2 108.3(13) . 4 ?
O2 Si1 O2 110(2) . 4 ?
O1 Si1 O3 112(2) . . ?
O2 Si1 O3 109.3(12) . . ?
O2 Si1 O3 109.3(12) 4 . ?
O4 Si2 O5 108.3(12) . 4 ?
O4 Si2 O5 108.3(12) . . ?
O5 Si2 O5 108(2) 4 . ?
O4 Si2 O3 112(2) . . ?
O5 Si2 O3 110.1(11) 4 . ?
O5 Si2 O3 110.1(11) . . ?
O14 Si3 O6 110.8(15) 7 . ?
O14 Si3 O7 106.4(12) 7 . ?
O6 Si3 O7 111.0(13) . . ?
O14 Si3 O5 107.6(14) 7 . ?
O6 Si3 O5 111.8(15) . . ?
O7 Si3 O5 109.0(12) . . ?
O8 Si4 O6 109.3(13) . 2_655 ?
O8 Si4 O6 109.3(13) . 3_665 ?
O6 Si4 O6 109.7(13) 2_655 3_665 ?
O8 Si4 O6 109.3(13) . . ?
O6 Si4 O6 109.7(13) 2_655 . ?
O6 Si4 O6 109.7(13) 3_665 . ?
O2 Si5 O13 110.0(13) 3_665 8_665 ?
O2 Si5 O9 112.3(10) 3_665 . ?
O13 Si5 O9 107.6(12) 8_665 . ?
O2 Si5 O7 110.6(14) 3_665 . ?
O13 Si5 O7 111.6(14) 8_665 . ?
O9 Si5 O7 104.6(11) . . ?
O12 Si6 O12 108(3) 4 . ?
O12 Si6 O1 110.1(14) 4 2 ?
O12 Si6 O1 110.1(14) . 2 ?
O12 Si6 O11 108.7(15) 4 . ?
O12 Si6 O11 108.7(15) . . ?
O1 Si6 O11 111(2) 2 . ?
Si10 Si7 O10 179(2) . 7 ?
Si10 Si7 O12 69.1(17) . . ?
O10 Si7 O12 111(2) 7 . ?
Si10 Si7 O13 67.7(16) . . ?
O10 Si7 O13 113(2) 7 . ?
O12 Si7 O13 109.4(16) . . ?
Si10 Si7 O14 68.1(15) . . ?
O10 Si7 O14 111.2(16) 7 . ?
O12 Si7 O14 103.7(14) . . ?
O13 Si7 O14 108.3(16) . . ?
O16 Si8 O16 131(7) 9_556 . ?
O16 Si8 O15 111(4) 9_556 . ?
O16 Si8 O15 33(3) . . ?
O16 Si8 O15 33(3) 9_556 9_556 ?
O16 Si8 O15 111(4) . 9_556 ?
O15 Si8 O15 110(4) . 9_556 ?
O16 Si8 O10 78(3) 9_556 10 ?
O16 Si8 O10 135(3) . 10 ?
O15 Si8 O10 112(3) . 10 ?
O15 Si8 O10 109(2) 9_556 10 ?
O16 Si8 O10 135(3) 9_556 5 ?
O16 Si8 O10 78(3) . 5 ?
O15 Si8 O10 109(2) . 5 ?
O15 Si8 O10 112(3) 9_556 5 ?
O10 Si8 O10 106(4) 10 5 ?
Si9 Si9 O4 69.6(15) 4 2 ?
Si9 Si9 O11 69.7(15) 4 . ?
O4 Si9 O11 113(3) 2 . ?
Si9 Si9 O17 69.8(15) 4 . ?
O4 Si9 O17 108(3) 2 . ?
O11 Si9 O17 104(4) . . ?
Si9 Si9 O16 179(3) 4 . ?
O4 Si9 O16 111(3) 2 . ?
O11 Si9 O16 109(3) . . ?
O17 Si9 O16 111(3) . . ?
Si9 Si9 O15 150(2) 4 . ?
O4 Si9 O15 140(3) 2 . ?
O11 Si9 O15 89(3) . . ?
O17 Si9 O15 96(3) . . ?
O16 Si9 O15 30(3) . . ?
Si7 Si10 O13 68.1(17) . . ?
Si7 Si10 O18 174(3) . . ?
O13 Si10 O18 117(3) . . ?
Si7 Si10 O14 68.3(16) . . ?
O13 Si10 O14 108.6(18) . . ?
O18 Si10 O14 112(3) . . ?
Si7 Si10 O12 67.0(18) . . ?
O13 Si10 O12 108.3(19) . . ?
O18 Si10 O12 107(2) . . ?
O14 Si10 O12 102.7(16) . . ?
O19 Si11 O18 108(3) . . ?
O19 Si11 O18 108(3) . 4 ?
O18 Si11 O18 114(4) . 4 ?
O19 Si11 O20 110(4) . . ?
O18 Si11 O20 108(3) . . ?
O18 Si11 O20 108(3) 4 . ?
O19 Si11 O19 88(10) . 2_665 ?
O18 Si11 O19 64(4) . 2_665 ?
O18 Si11 O19 64(4) 4 2_665 ?
O20 Si11 O19 162(10) . 2_665 ?
Si1 O1 Si6 165(3) . 3 ?
Si5 O2 Si1 158.4(19) 2_655 . ?
Si1 O3 Si2 153(2) . . ?
Si2 O4 Si9 148(2) . 6 ?
Si2 O4 Si9 148(2) . 3 ?
Si9 O4 Si9 41(3) 6 3 ?
Si2 O5 Si3 145.3(14) . . ?
Si4 O6 Si3 174(2) . . ?
Si3 O7 Si5 139.3(15) . . ?
Si4 O8 Si4 180.0 4 . ?
Si5 O9 Si5 149.2(16) 7 . ?
Si7 O10 Si8 142(3) 7 6 ?
Si9 O11 Si9 41(3) 4 . ?
Si9 O11 Si6 141(3) 4 . ?
Si9 O11 Si6 141(3) . . ?
Si6 O12 Si7 149(2) . . ?
Si6 O12 Si10 149(2) . . ?
Si7 O12 Si10 43.9(12) . . ?
Si5 O13 Si10 154.7(18) 8_565 . ?
Si5 O13 Si7 158.5(19) 8_565 . ?
Si10 O13 Si7 44.2(12) . . ?
Si3 O14 Si10 143.0(17) 7 . ?
Si3 O14 Si7 142.1(16) 7 . ?
Si10 O14 Si7 43.7(12) . . ?
O16 O15 Si8 71(4) . . ?
O16 O15 Si9 63(3) . . ?
Si8 O15 Si9 125(3) . . ?
O15 O16 Si8 76(4) . . ?
O15 O16 Si9 87(4) . . ?
Si8 O16 Si9 144(5) . . ?
Si9 O17 Si9 40(3) . 4 ?
Si11 O18 Si10 138(5) . . ?
Si11 O18 O19 63(8) . 2_665 ?
Si10 O18 O19 132(9) . 2_665 ?
Si11 O19 Si11 152(10) . 3_565 ?
Si11 O19 O18 132(3) . 6_565 ?
Si11 O19 O18 53(5) 3_565 6_565 ?
Si11 O19 O18 132(3) . 3_565 ?
Si11 O19 O18 53(5) 3_565 3_565 ?
O18 O19 O18 96(6) 6_565 3_565 ?
 
_refine_diff_density_max    0.203
_refine_diff_density_min   -0.280
_refine_diff_density_rms    0.081



# start Validation Reply Form

_vrf_PLAT082_ECNU-45_treated_for_4h
;
PROBLEM: High R1 Value ..................................       0.16 Report
RESPONSE: This is mainly the result of multiple scattering of electrons in the crystal and to some extent the missing guest molecules that could not be located from the ED data.
;
_vrf_PLAT084_ECNU-45_treated_for_4h
;
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 and to some extent the missing guest molecules that could not be located from the ED data.
;
_vrf_THETM01_ECNU-45_treated_for_4h
;
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_4h
;
PROBLEM:  Solvent Accessible VOID(S) in Structure ........    
RESPONSE: This is a porous zeolite structure.
;
