#------------------------------------------------------------------------------
#$Date: 2020-08-22 08:18:32 +0300 (Sat, 22 Aug 2020) $
#$Revision: 255586 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/30/06/2300668.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2300668
loop_
_publ_author_name
'Roslova, Maria'
'Smeets, Stef'
'Wang, Bin'
'Thersleff, Thomas'
'Xu, Hongyi'
'Zou, Xiaodong'
_publ_section_title
;
InsteaDMatic: towards cross-platform automated continuous rotation
electron diffraction
;
_journal_coeditor_code TE5059SUP1
_journal_issue 5
_journal_name_full 'Journal of Applied Crystallography'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S1600576720009590
_journal_volume 53
_journal_year 2020
_chemical_formula_moiety 'O24 Si12'
_chemical_formula_sum 'O24 Si12'
_chemical_formula_weight 721.01
_space_group_crystal_system orthorhombic
_space_group_IT_number 62
_space_group_name_Hall '-P 2ac 2n'
_space_group_name_H-M_alt 'P n m a'
_audit_creation_date 2020-04-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 20.022(4)
_cell_length_b 19.899(4)
_cell_length_c 13.383(3)
_cell_measurement_temperature 293(2)
_cell_volume 5332.0(19)
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type 'Themis Z'
_diffrn_measurement_method cRED
_diffrn_radiation_type '300 kV electrons'
_diffrn_radiation_wavelength 0.019
_diffrn_reflns_av_R_equivalents 0.3082
_diffrn_reflns_av_unetI/netI 0.1708
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max 24
_diffrn_reflns_limit_h_min -24
_diffrn_reflns_limit_k_max 24
_diffrn_reflns_limit_k_min -24
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 61596
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full 0.653
_diffrn_reflns_theta_max 0.678
_diffrn_reflns_theta_min 0.049
_diffrn_source XFEG
_exptl_absorpt_coefficient_mu 0.000
_exptl_crystal_density_diffrn 1.796
_exptl_crystal_description 'merged dataset'
_exptl_crystal_F_000 939
_refine_diff_density_max 0.304
_refine_diff_density_min -0.200
_refine_diff_density_rms 0.061
_refine_ls_extinction_coef 838(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref 1.583
_refine_ls_hydrogen_treatment undef
_refine_ls_matrix_type full
_refine_ls_number_parameters 332
_refine_ls_number_reflns 5159
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.584
_refine_ls_R_factor_all 0.2612
_refine_ls_R_factor_gt 0.1992
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.5092
_refine_ls_wR_factor_ref 0.5465
_reflns_Friedel_coverage 0.000
_reflns_number_gt 2854
_reflns_number_total 5159
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file te5059sup1.cif
_cod_data_source_block zsm5_cluster_3_saed
_cod_database_code 2300668
_shelx_shelxl_version_number 2018/3
_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.
;
_olex2_refinement_description
;
1. Restrained distances
Si11-O10
1.6 with sigma of 0.02
Si6-O18
1.6 with sigma of 0.02
;
_shelx_res_file
;
TITL zsm-5_cluster_3_SAED
zsm5_cluster_3_saed.res
created by SHELXL-2018/3 at 13:08:37 on 16-Apr-2020
CELL 0.019 20.022 19.899 13.383 90 90 90
ZERR 8 0.004 0.004 0.003 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM 0.5+X,0.5-Y,0.5-Z
SYMM -X,0.5+Y,-Z
SFAC O 0.455 23.78 0.917 7.622 0.472 2.144 0.138 0.296 0 0 0 0 0.73 15.999
SFAC SI 2.129 57.775 2.533 16.476 0.835 2.88 0.322 0.386 0 0 0 0 1.11 28.086
UNIT 192 96
DFIX 1.6 Si11 O10
DFIX 1.6 Si6 O18
L.S. 5
PLAN 25
LIST 4
fmap 2
acta
SHEL 20 0.8
REM
REM
REM
WGHT 0.200000
EXTI 838.070801
FVAR 9.11617
SI1 2 0.422911 0.058476 -0.339305 11.00000 0.05308 0.07542 =
0.06779 0.00143 0.00611 0.01186
SI2 2 0.307196 0.029631 -0.193427 11.00000 0.07364 0.07705 =
0.07276 -0.00131 0.01298 -0.00237
SI3 2 0.280424 0.062941 0.030432 11.00000 0.06034 0.06833 =
0.06318 -0.00863 -0.00788 0.00780
SI4 2 0.121865 0.063721 0.025656 11.00000 0.05693 0.07282 =
0.05709 -0.00715 0.00798 -0.00150
SI5 2 0.071430 0.028383 -0.185741 11.00000 0.04564 0.06150 =
0.06084 -0.00391 0.00894 0.00231
SI6 2 0.185360 0.058787 -0.332326 11.00000 0.05713 0.06655 =
0.06504 0.00868 0.01155 -0.00246
SI7 2 0.421945 -0.171919 -0.329977 11.00000 0.06135 0.06947 =
0.07780 -0.00220 0.00162 -0.00249
SI8 2 0.307253 -0.129272 -0.188749 11.00000 0.07537 0.06999 =
0.05629 -0.00683 0.00450 -0.00295
SI9 2 0.275844 -0.173624 0.027422 11.00000 0.06645 0.05683 =
0.06482 0.00098 -0.00934 -0.00304
SI10 2 0.120411 -0.173912 0.026229 11.00000 0.07092 0.05820 =
0.08505 0.00566 -0.00064 0.00146
SI11 2 0.068328 -0.130057 -0.184689 11.00000 0.05475 0.06340 =
0.06366 0.00332 0.00962 0.00391
SI12 2 0.186273 -0.172726 -0.322553 11.00000 0.06064 0.06750 =
0.07643 0.00227 0.01024 -0.00913
O1 1 0.372873 0.056504 -0.245618 11.00000 0.08810 0.12331 =
0.09387 -0.00868 0.03955 -0.01861
O2 1 0.305698 0.058839 -0.085488 11.00000 0.11117 0.11226 =
0.05251 -0.01587 0.00804 -0.00155
O3 1 0.200027 0.058825 0.030001 11.00000 0.06477 0.16922 =
0.12296 0.00009 -0.00863 0.00033
O4 1 0.099805 0.060918 -0.087118 11.00000 0.13417 0.10150 =
0.07480 -0.00893 -0.03346 -0.01598
O5 1 0.113721 0.053951 -0.277807 11.00000 0.06681 0.11879 =
0.09851 0.01446 0.03462 0.00344
O6 1 0.243165 0.056130 -0.250066 11.00000 0.12334 0.10199 =
0.09854 0.01132 0.00354 0.00879
O7 1 0.374952 -0.152483 -0.235083 11.00000 0.09715 0.12874 =
0.08936 0.00538 0.02074 0.01673
O8 1 0.308127 -0.155099 -0.077193 11.00000 0.11027 0.14281 =
0.07503 0.02861 0.00946 0.00363
O9 1 0.198641 -0.156969 0.025908 11.00000 0.05416 0.09468 =
0.19859 -0.01192 0.01004 0.00048
O10 1 0.088564 -0.159430 -0.082671 11.00000 0.18184 0.13440 =
0.10241 0.02770 -0.04430 -0.01898
O11 1 0.116457 -0.157022 -0.270572 11.00000 0.10905 0.10560 =
0.12737 -0.03952 0.01679 0.01612
O12 1 0.242465 -0.153874 -0.243809 11.00000 0.10513 0.14527 =
0.10589 0.00761 -0.00978 -0.05379
O13 1 0.308387 -0.051044 -0.188015 11.00000 0.29012 0.09835 =
0.15187 -0.05781 -0.01234 0.03037
O14 1 0.074189 -0.051225 -0.182038 11.00000 0.17322 0.05664 =
0.13215 0.01626 0.02017 -0.00898
O15 1 0.416539 0.126783 -0.394368 11.00000 0.11316 0.07087 =
0.15108 0.01405 -0.05811 -0.00727
O16 1 0.411069 -0.000613 -0.413582 11.00000 0.15358 0.07880 =
0.10308 -0.00805 -0.04551 0.00522
O17 1 0.401981 -0.131582 -0.429685 11.00000 0.10835 0.07100 =
0.09132 0.02064 -0.00187 0.01953
O18 1 0.188745 0.130646 -0.390034 11.00000 0.10458 0.08089 =
0.08447 0.00506 0.03409 -0.00050
O19 1 0.190880 -0.000774 -0.412163 11.00000 0.11359 0.06630 =
0.11127 -0.02834 0.00056 0.01568
O20 1 0.193821 -0.131068 -0.420450 11.00000 0.09892 0.08319 =
0.09134 0.01550 0.01757 -0.01580
O21 1 -0.002004 0.051351 -0.204795 11.00000 0.08996 0.11489 =
0.07887 0.00849 0.00389 0.01202
O22 1 -0.004804 -0.152188 -0.208600 11.00000 0.06683 0.12985 =
0.10183 0.01240 -0.00013 -0.02356
O23 1 0.417832 -0.250000 -0.359087 10.50000 0.20396 0.06352 =
0.12766 0.00000 -0.00158 0.00000
O24 1 0.190196 -0.250000 -0.354101 10.50000 0.19510 0.03633 =
0.14081 0.00000 0.04485 0.00000
O25 1 0.290643 -0.250000 0.053925 10.50000 0.10458 0.06197 =
0.06132 0.00000 -0.01238 0.00000
O26 1 0.105623 -0.250000 0.056298 10.50000 0.09613 0.06293 =
0.19174 0.00000 -0.01210 0.00000
HKLF 4
REM zsm-5_cluster_3_SAED
REM wR2 = 0.5465, GooF = S = 1.583, Restrained GooF = 1.584 for all data
REM R1 = 0.1992 for 2854 Fo > 4sig(Fo) and 0.2612 for all 5159 data
REM 332 parameters refined using 2 restraints
END
WGHT 0.2000 0.0000
REM Highest difference peak 0.304, deepest hole -0.200, 1-sigma level 0.061
Q1 1 0.1933 -0.2500 -0.6458 10.50000 0.05 0.30
Q2 1 0.2548 0.0585 -0.0214 11.00000 0.05 0.29
Q3 1 0.3241 -0.1793 -0.0282 11.00000 0.05 0.27
Q4 1 0.3227 0.0591 -0.0280 11.00000 0.05 0.27
Q5 1 0.2103 -0.1785 -0.0294 11.00000 0.05 0.26
Q6 1 0.4139 -0.2500 -0.6567 10.50000 0.05 0.24
Q7 1 0.2494 0.0654 0.0825 11.00000 0.05 0.24
Q8 1 0.1722 -0.1840 -0.0332 11.00000 0.05 0.24
Q9 1 0.4008 -0.1905 -0.0323 11.00000 0.05 0.22
Q10 1 0.1721 0.0595 -0.0240 11.00000 0.05 0.22
Q11 1 0.1915 -0.1743 0.1010 11.00000 0.05 0.21
Q12 1 0.3974 0.0566 -0.2886 11.00000 0.05 0.19
Q13 1 0.0887 -0.1322 -0.1451 11.00000 0.05 0.19
Q14 1 0.4182 0.0629 -0.0289 11.00000 0.05 0.19
Q15 1 0.3098 -0.1354 -0.1424 11.00000 0.05 0.19
Q16 1 0.2993 -0.1789 0.0750 11.00000 0.05 0.18
Q17 1 0.2108 -0.1828 -0.2845 11.00000 0.05 0.18
Q18 1 0.2064 0.0563 -0.2911 11.00000 0.05 0.18
Q19 1 0.0866 -0.1844 -0.0365 11.00000 0.05 0.17
Q20 1 0.1860 0.0608 0.1028 11.00000 0.05 0.17
Q21 1 0.2110 0.0568 -0.3884 11.00000 0.05 0.17
Q22 1 0.3070 -0.2500 0.3417 10.50000 0.05 0.16
Q23 1 0.3996 -0.1850 -0.2922 11.00000 0.05 0.16
Q24 1 0.0528 -0.1857 -0.5747 11.00000 0.05 0.16
Q25 1 0.1547 0.1808 -0.1794 11.00000 0.05 0.16
;
_shelx_res_checksum 28392
_shelx_hkl_file
;
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0 0 -4 106433. 45109. 1
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0 0 -10 5884.57 2501.42 1
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0 -1 -3 134910. 57181. 1
0 -1 -3 -461.21 743.235 1
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0 -1 -9 22025. 9337.74 1
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0 -2 0 154115. 57796. 1
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10 -16 1 309.93 809.271 1
10 -16 1 30.79 222.611 1
10 -16 1 106.24 88.723 1
10 16 2 424.03 428.382 1
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10 -17 1 -304.35 812.393 1
10 -17 1 -32.25 223.557 1
10 17 2 -256.29 407.852 1
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10 -17 2 972.56 990.538 1
10 -17 2 264.71 247.114 1
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10 17 3 -210.22 400.473 1
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10 -17 -9 315.99 468.306 1
10 -17 -9 -38.10 98.013 1
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10 -18 0 -166.51 644.086 1
10 -18 0 969.72 433.396 1
10 -18 0 605.39 268.212 1
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10 -18 -1 335.29 246.641 1
10 -18 -1 137.18 577.767 1
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-21 8 -6 -556.39 2390.73 1
-21 8 6 -128.29 899.715 1
-21 8 6 73.67 60.407 1
21 -8 6 557.33 445.600 1
21 8 7 184.67 413.623 1
21 -8 -7 199.72 132.072 1
-21 -8 -7 -81.30 319.394 1
21 -9 -1 1182.59 712.961 1
-21 9 -1 -217.98 568.968 1
-21 9 1 -406.62 608.609 1
21 -9 1 113.24 506.717 1
21 -9 -2 609.18 663.102 1
-21 9 -2 288.36 544.560 1
-21 9 2 -277.39 728.949 1
21 -9 -3 261.02 730.841 1
-21 9 3 -734.06 724.219 1
21 -9 3 252.13 404.446 1
21 -9 -4 -71.16 625.165 1
-21 9 -4 19.70 472.090 1
-21 9 4 801.70 777.483 1
21 -9 4 -206.62 386.755 1
21 -9 -5 -800.85 756.291 1
-21 9 -5 -12.89 453.358 1
-21 9 5 1376.54 916.461 1
-21 9 5 37.95 57.143 1
21 -9 5 -249.01 405.581 1
21 9 6 19.70 377.199 1
21 -9 -6 17.00 98.297 1
-21 9 -6 377.67 2891.20 1
-21 9 6 30.24 49.290 1
21 -10 -1 156.20 598.770 1
-21 10 -1 -433.21 534.247 1
-21 10 1 230.27 642.383 1
21 -10 1 69.66 447.776 1
21 -10 -2 815.23 710.501 1
-21 10 -2 -361.59 503.405 1
-21 10 2 61.19 608.136 1
21 -10 2 466.70 434.437 1
21 -10 -3 1779.56 901.134 1
-21 10 -3 -151.84 472.469 1
-21 10 3 349.01 686.376 1
21 -10 3 501.99 416.745 1
21 -10 -4 699.53 787.417 1
-21 10 -4 196.03 468.495 1
-21 10 4 -723.56 790.728 1
-21 10 4 429.99 193.377 1
21 -10 4 50.77 369.914 1
21 -10 -5 1342.48 1005.68 1
21 -10 -5 191.20 123.746 1
-21 10 -5 260.55 502.838 1
-21 10 5 25.50 53.491 1
-21 11 -1 -427.81 509.271 1
-21 11 1 23.03 600.472 1
21 -11 1 -315.61 431.504 1
21 -11 -2 274.64 641.343 1
-21 11 -2 88.56 455.818 1
-21 11 2 -384.11 663.008 1
21 -11 2 8.95 367.265 1
21 -11 -3 706.24 727.814 1
-21 11 -3 165.75 468.022 1
-21 11 3 19.31 667.076 1
-21 11 3 119.30 78.524 1
21 -11 3 -161.87 377.294 1
21 -11 -4 19.05 80.085 1
-21 11 4 127.34 78.779 1
21 -11 4 36.16 430.652 1
21 -12 -1 339.55 603.784 1
-21 12 -1 -226.40 538.789 1
-21 12 1 380.89 581.646 1
21 -12 1 27.19 433.396 1
21 -12 -2 -63.74 621.381 1
-21 12 -2 -253.26 518.921 1
-21 12 2 374.36 635.477 1
-21 12 2 -21.89 57.815 1
21 -12 2 74.59 397.067 1
21 -12 -3 145.22 103.217 1
21 -12 4 75.51 166.509 1
21 -13 1 84.72 226.584 1
21 -13 2 -76.43 225.638 1
22 -1 6 243.80 389.025 1
22 -1 7 300.66 416.272 1
22 -2 3 262.54 429.233 1
22 -2 4 -298.11 445.695 1
-22 2 -5 -288.93 502.554 1
22 -2 5 60.26 419.016 1
-22 2 -6 310.69 498.486 1
22 -2 6 64.81 427.625 1
-22 2 -7 -419.39 525.165 1
22 -2 7 177.29 395.080 1
22 -3 0 -255.44 565.657 1
22 -3 -1 -1107.9 700.567 1
-22 3 -1 -21.87 546.168 1
22 -3 1 -423.65 489.214 1
-22 3 -2 -439.73 586.754 1
22 -3 2 -171.43 473.320 1
-22 3 -3 190.16 565.562 1
22 -3 3 -391.01 501.797 1
-22 3 -4 633.11 580.889 1
22 -3 4 -118.07 471.807 1
-22 3 -5 597.82 554.209 1
22 -3 5 300.47 436.329 1
-22 3 -6 -812.39 565.184 1
22 -3 6 164.24 383.349 1
-22 4 0 169.16 593.471 1
22 -4 0 -1070.0 664.238 1
22 -4 -1 -838.88 653.453 1
-22 4 -1 387.13 612.582 1
-22 4 1 232.17 632.355 1
22 -4 1 9.34 496.215 1
22 -4 -2 138.22 677.672 1
-22 4 -2 208.23 571.617 1
-22 4 2 662.53 734.626 1
22 -4 2 212.87 470.671 1
22 -4 -3 769.06 749.195 1
-22 4 -3 384.01 581.740 1
22 -4 3 -230.94 469.631 1
22 -4 -4 -182.12 660.643 1
-22 4 -4 710.12 604.919 1
22 -4 4 -365.94 430.274 1
-22 4 -5 281.65 491.769 1
22 -4 5 137.37 414.475 1
-22 4 -6 700.57 524.976 1
22 -4 6 587.80 444.370 1
-22 5 0 -400.57 599.810 1
22 -5 0 -24.90 576.158 1
22 -5 -1 404.35 655.912 1
-22 5 -1 295.46 609.271 1
-22 5 1 695.08 712.393 1
22 -5 1 904.92 529.612 1
22 -5 -2 -39.03 744.181 1
-22 5 -2 550.24 565.941 1
-22 5 2 314.38 741.437 1
22 -5 2 -436.80 463.008 1
22 -5 -3 288.93 714.190 1
-22 5 -3 -154.59 503.405 1
-22 5 3 -741.06 787.984 1
22 -5 3 9.60 429.044 1
22 -5 -4 -1208.1 801.135 1
-22 5 -4 589.59 518.259 1
-22 5 4 688.36 808.798 1
22 -5 4 140.02 429.801 1
22 -5 -5 -766.32 812.014 1
-22 5 -5 182.40 506.717 1
-22 5 5 -1125.8 852.601 1
22 -5 5 -488.55 489.309 1
22 -5 -6 196.69 865.940 1
-22 5 -6 -118.26 561.210 1
-22 5 6 319.58 816.555 1
22 -5 6 427.15 494.985 1
-22 6 0 642.01 616.934 1
22 -6 0 -272.47 470.860 1
22 -6 -1 195.55 509.366 1
-22 6 -1 -672.56 570.860 1
-22 6 1 569.35 659.034 1
22 -6 1 -342.57 434.815 1
22 -6 -2 1263.95 781.456 1
-22 6 -2 942.67 602.459 1
-22 6 2 519.30 746.357 1
22 -6 2 264.52 455.723 1
22 -6 -3 267.36 713.528 1
-22 6 -3 -555.34 527.341 1
-22 6 3 622.99 788.079 1
22 -6 3 -225.07 477.388 1
22 -6 -4 -313.15 761.021 1
-22 6 -4 489.78 594.228 1
-22 6 4 -762.06 839.829 1
22 -6 4 167.27 502.838 1
22 -6 -5 -266.70 806.149 1
-22 6 -5 -457.62 538.978 1
-22 6 5 267.64 860.075 1
22 -6 5 299.62 514.758 1
22 -6 -6 -1286.7 978.239 1
-22 7 0 311.07 570.293 1
22 -7 0 763.01 571.901 1
22 -7 -1 5.90 581.646 1
-22 7 -1 683.73 573.036 1
-22 7 1 142.10 608.136 1
22 -7 1 -60.96 490.255 1
22 -7 -2 1056.76 702.081 1
-22 7 -2 -48.27 532.544 1
-22 7 2 399.81 633.396 1
22 -7 2 -54.82 492.809 1
22 -7 -3 -227.34 601.419 1
-22 7 -3 211.83 526.490 1
-22 7 3 -1014.2 777.388 1
22 -7 3 -36.08 459.224 1
22 -7 -4 -841.63 689.025 1
-22 7 -4 -449.29 556.196 1
-22 7 4 557.71 908.514 1
22 -7 4 -293.85 508.136 1
22 -7 -5 -359.03 847.303 1
-22 7 -5 215.23 536.518 1
-22 7 5 -157.80 863.575 1
22 -7 5 -479.94 509.460 1
-22 8 0 -240.49 558.467 1
22 -8 0 155.44 541.532 1
22 -8 -1 1391.67 787.133 1
-22 8 -1 1327.34 687.417 1
-22 8 1 428.85 650.520 1
22 -8 1 1218.54 599.905 1
22 -8 -2 729.04 686.944 1
-22 8 -2 -330.94 551.087 1
-22 8 2 -500.38 657.331 1
22 -8 2 83.26 499.905 1
22 -8 -3 -272.75 640.113 1
-22 8 -3 262.06 571.144 1
-22 8 3 1080.42 802.932 1
22 -8 3 550.14 517.880 1
22 -8 -4 15.43 630.558 1
-22 8 -4 -20.65 548.344 1
-22 8 4 -529.23 733.585 1
22 -8 4 -743.52 604.446 1
-22 9 0 45.58 609.933 1
22 -9 0 -218.83 571.050 1
22 -9 -1 -608.42 621.286 1
-22 9 -1 900.28 624.408 1
-22 9 1 -478.43 717.786 1
22 -9 1 -118.45 463.860 1
22 -9 -2 477.77 664.616 1
-22 9 -2 -160.45 545.789 1
-22 9 2 -397.73 694.701 1
22 -9 2 49.27 456.953 1
22 -9 -3 396.69 628.287 1
-22 9 -3 -550.71 583.632 1
-22 9 3 -191.77 728.665 1
22 -9 3 -199.81 469.063 1
-22 10 0 -472.94 655.723 1
22 -10 0 198.20 540.775 1
22 -10 -1 201.51 640.870 1
-22 10 -1 156.95 595.080 1
-22 10 1 -3.68 618.732 1
22 -10 1 446.64 592.431 1
22 -10 -2 120.91 707.284 1
-22 10 -2 -78.93 596.215 1
-22 10 2 -887.89 699.526 1
22 -10 2 -277.58 432.828 1
23 -2 3 83.12 388.836 1
23 -2 4 -38.60 435.856 1
-23 2 -5 379.85 567.076 1
23 -2 5 -284.11 463.576 1
23 -3 1 425.92 470.009 1
-23 3 -2 12.08 505.771 1
23 -3 2 -598.01 449.952 1
-23 3 -3 -396.88 571.712 1
23 -3 3 114.29 449.763 1
-23 3 -4 1153.26 654.209 1
23 -3 4 189.12 454.399 1
-23 3 -5 590.92 567.360 1
23 -3 5 -34.94 482.592 1
23 -4 -1 246.83 582.781 1
-23 4 -1 -153.36 538.410 1
-23 4 1 37.44 626.111 1
23 -4 1 472.00 527.436 1
23 -4 -2 -249.57 645.979 1
-23 4 -2 -108.61 567.265 1
-23 4 2 -782.97 739.072 1
23 -4 2 -213.34 462.724 1
23 -4 -3 -1599.8 825.354 1
-23 4 -3 83.89 555.439 1
23 -4 3 76.79 464.333 1
23 -4 -4 54.99 736.329 1
-23 4 -4 218.73 555.345 1
23 -4 4 -153.55 416.651 1
-23 4 -5 -189.40 574.455 1
23 -4 5 357.99 495.742 1
23 -5 -1 171.52 655.250 1
-23 5 -1 312.96 587.511 1
-23 5 1 71.86 619.867 1
23 -5 1 364.24 496.783 1
23 -5 -2 -117.03 657.331 1
-23 5 -2 -9.76 565.089 1
-23 5 2 942.29 786.470 1
23 -5 2 461.49 457.521 1
23 -5 -3 -515.42 717.312 1
-23 5 -3 -14.17 511.447 1
-23 5 3 441.82 775.212 1
23 -5 3 -260.55 434.910 1
23 -5 -4 505.96 764.711 1
-23 5 -4 197.16 512.866 1
-23 5 4 560.83 823.840 1
23 -5 4 284.67 452.790 1
23 -6 -1 149.95 536.896 1
-23 6 -1 -483.16 544.560 1
-23 6 1 -264.52 642.667 1
23 -6 1 -368.59 452.507 1
23 -6 -2 -471.81 736.991 1
-23 6 -2 120.25 530.936 1
-23 6 2 -621.66 763.954 1
23 -6 2 259.22 463.860 1
23 -6 -3 502.65 762.535 1
-23 6 -3 -139.83 528.949 1
-23 6 3 427.53 796.783 1
23 -6 3 -474.74 457.805 1
23 -6 -4 -431.03 835.382 1
23 -7 -1 884.48 620.718 1
-23 7 -1 -694.42 575.969 1
-23 7 1 -303.69 607.852 1
23 -7 1 -107.19 445.790 1
23 -7 -2 347.11 590.633 1
-23 7 -2 841.63 600.945 1
-23 7 2 -235.48 677.199 1
23 -7 2 -569.54 512.582 1
23 -7 -3 -21.44 666.792 1
-23 7 -3 331.79 597.161 1
-23 7 3 637.84 746.451 1
23 -7 3 -321.29 517.123 1
23 -8 -1 -613.91 631.125 1
-23 8 -1 472.28 622.800 1
-23 8 1 489.78 694.039 1
23 -8 1 -85.55 483.443 1
23 -8 -2 93.60 716.556 1
24 -3 0 192.24 483.159 1
24 -3 1 -110.97 448.155 1
-24 3 -2 398.39 559.791 1
24 -3 2 148.44 431.598 1
24 -3 3 32.95 514.947 1
-24 4 0 57.05 610.028 1
24 -4 0 -255.44 557.142 1
24 -4 -1 -139.45 575.875 1
-24 4 -1 -390.54 618.259 1
-24 4 1 -411.54 640.018 1
24 -4 1 337.94 492.904 1
24 -4 -2 -70.75 655.250 1
-24 4 -2 -949.86 672.847 1
24 -4 2 183.35 464.333 1
-24 5 0 21.88 611.258 1
24 -5 0 8.44 591.485 1
24 -5 -1 -575.97 711.163 1
-24 5 -1 161.21 619.962 1
-24 5 1 158.66 750.047 1
24 -5 1 -176.44 475.591 1
0 0 0 0. 0.00 0
;
_shelx_hkl_checksum 13873
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'
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 0.4229(3) 0.0585(2) -0.3393(3) 0.0654(13) Uani 1 1 d . . . . .
Si2 Si 0.3072(3) 0.0296(3) -0.1934(4) 0.0745(15) Uani 1 1 d . . . . .
Si3 Si 0.2804(3) 0.0629(2) 0.0304(3) 0.0640(13) Uani 1 1 d . . . . .
Si4 Si 0.1219(3) 0.0637(2) 0.0257(3) 0.0623(13) Uani 1 1 d . . . . .
Si5 Si 0.0714(2) 0.0284(2) -0.1857(3) 0.0560(12) Uani 1 1 d . . . . .
Si6 Si 0.1854(3) 0.0588(2) -0.3323(4) 0.0629(13) Uani 1 1 d D . . . .
Si7 Si 0.4219(3) -0.1719(2) -0.3300(3) 0.0695(14) Uani 1 1 d . . . . .
Si8 Si 0.3073(3) -0.1293(2) -0.1887(3) 0.0672(14) Uani 1 1 d . . . . .
Si9 Si 0.2758(3) -0.17362(19) 0.0274(3) 0.0627(13) Uani 1 1 d . . . . .
Si10 Si 0.1204(3) -0.1739(2) 0.0262(3) 0.0714(15) Uani 1 1 d . . . . .
Si11 Si 0.0683(2) -0.13006(19) -0.1847(3) 0.0606(12) Uani 1 1 d D . . . .
Si12 Si 0.1863(3) -0.1727(2) -0.3226(4) 0.0682(14) Uani 1 1 d . . . . .
O1 O 0.3729(6) 0.0565(4) -0.2456(7) 0.102(3) Uani 1 1 d . . . . .
O2 O 0.3057(5) 0.0588(4) -0.0855(6) 0.092(3) Uani 1 1 d . . . . .
O3 O 0.2000(6) 0.0588(6) 0.0300(10) 0.119(4) Uani 1 1 d . . . . .
O4 O 0.0998(6) 0.0609(4) -0.0871(6) 0.103(3) Uani 1 1 d . . . . .
O5 O 0.1137(5) 0.0540(4) -0.2778(7) 0.095(3) Uani 1 1 d . . . . .
O6 O 0.2432(7) 0.0561(4) -0.2501(8) 0.108(3) Uani 1 1 d . . . . .
O7 O 0.3750(5) -0.1525(5) -0.2351(6) 0.105(3) Uani 1 1 d . . . . .
O8 O 0.3081(5) -0.1551(6) -0.0772(6) 0.109(3) Uani 1 1 d . . . . .
O9 O 0.1986(5) -0.1570(5) 0.0259(10) 0.116(4) Uani 1 1 d . . . . .
O10 O 0.0886(7) -0.1594(6) -0.0827(7) 0.140(5) Uani 1 1 d D . . . .
O11 O 0.1165(6) -0.1570(5) -0.2706(7) 0.114(3) Uani 1 1 d . . . . .
O12 O 0.2425(6) -0.1539(6) -0.2438(7) 0.119(4) Uani 1 1 d . . . . .
O13 O 0.3084(10) -0.0510(6) -0.1880(13) 0.180(8) Uani 1 1 d . . . . .
O14 O 0.0742(7) -0.0512(4) -0.1820(8) 0.121(4) Uani 1 1 d . . . . .
O15 O 0.4165(6) 0.1268(4) -0.3944(8) 0.112(4) Uani 1 1 d . . . . .
O16 O 0.4111(6) -0.0006(4) -0.4136(7) 0.112(3) Uani 1 1 d . . . . .
O17 O 0.4020(5) -0.1316(3) -0.4297(6) 0.090(3) Uani 1 1 d . . . . .
O18 O 0.1887(5) 0.1306(4) -0.3900(7) 0.090(3) Uani 1 1 d D . . . .
O19 O 0.1909(5) -0.0008(4) -0.4122(7) 0.097(3) Uani 1 1 d . . . . .
O20 O 0.1938(5) -0.1311(4) -0.4205(7) 0.091(3) Uani 1 1 d . . . . .
O21 O -0.0020(6) 0.0514(4) -0.2048(7) 0.095(3) Uani 1 1 d . . . . .
O22 O -0.0048(5) -0.1522(5) -0.2086(7) 0.100(3) Uani 1 1 d . . . . .
O23 O 0.4178(10) -0.250000 -0.3591(11) 0.132(6) Uani 1 2 d S T P . .
O24 O 0.1902(8) -0.250000 -0.3541(12) 0.124(6) Uani 1 2 d S T P . .
O25 O 0.2906(6) -0.250000 0.0539(7) 0.076(3) Uani 1 2 d S T P . .
O26 O 0.1056(8) -0.250000 0.0563(13) 0.117(5) Uani 1 2 d S T P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Si1 0.053(4) 0.075(3) 0.068(2) 0.0014(18) 0.006(2) 0.012(2)
Si2 0.074(4) 0.077(3) 0.073(3) -0.001(2) 0.013(2) -0.002(2)
Si3 0.060(4) 0.068(3) 0.063(3) -0.0086(18) -0.008(2) 0.008(2)
Si4 0.057(4) 0.073(3) 0.057(2) -0.0072(17) 0.008(2) -0.002(2)
Si5 0.046(3) 0.062(2) 0.061(2) -0.0039(17) 0.0089(19) 0.0023(18)
Si6 0.057(4) 0.067(3) 0.065(3) 0.0087(18) 0.012(2) -0.0025(18)
Si7 0.061(4) 0.069(3) 0.078(3) -0.002(2) 0.002(2) -0.002(2)
Si8 0.075(4) 0.070(3) 0.056(2) -0.007(2) 0.004(2) -0.003(2)
Si9 0.066(4) 0.057(2) 0.065(2) 0.0010(17) -0.009(2) -0.0030(19)
Si10 0.071(4) 0.058(3) 0.085(3) 0.006(2) -0.001(2) 0.001(2)
Si11 0.055(3) 0.063(3) 0.064(2) 0.0033(17) 0.010(2) 0.0039(19)
Si12 0.061(4) 0.068(3) 0.076(3) 0.002(2) 0.010(2) -0.009(2)
O1 0.088(8) 0.123(7) 0.094(5) -0.009(4) 0.040(5) -0.019(5)
O2 0.111(9) 0.112(7) 0.053(4) -0.016(3) 0.008(4) -0.002(4)
O3 0.065(9) 0.169(12) 0.123(9) 0.000(6) -0.009(5) 0.000(5)
O4 0.134(10) 0.101(6) 0.075(4) -0.009(4) -0.033(5) -0.016(5)
O5 0.067(7) 0.119(6) 0.099(5) 0.014(4) 0.035(5) 0.003(4)
O6 0.123(11) 0.102(6) 0.099(6) 0.011(4) 0.004(6) 0.009(5)
O7 0.097(9) 0.129(7) 0.089(5) 0.005(5) 0.021(5) 0.017(6)
O8 0.110(10) 0.143(8) 0.075(5) 0.029(5) 0.009(4) 0.004(5)
O9 0.054(7) 0.095(6) 0.199(11) -0.012(7) 0.010(6) 0.000(4)
O10 0.182(14) 0.134(8) 0.102(6) 0.028(6) -0.044(7) -0.019(8)
O11 0.109(10) 0.106(6) 0.127(7) -0.040(5) 0.017(6) 0.016(5)
O12 0.105(10) 0.145(8) 0.106(6) 0.008(6) -0.010(6) -0.054(7)
O13 0.29(3) 0.098(8) 0.152(12) -0.058(7) -0.012(10) 0.030(8)
O14 0.173(13) 0.057(4) 0.132(8) 0.016(4) 0.020(7) -0.009(4)
O15 0.113(9) 0.071(5) 0.151(8) 0.014(5) -0.058(7) -0.007(4)
O16 0.154(10) 0.079(5) 0.103(5) -0.008(4) -0.046(6) 0.005(5)
O17 0.108(8) 0.071(4) 0.091(5) 0.021(3) -0.002(5) 0.020(4)
O18 0.105(8) 0.081(5) 0.084(5) 0.005(4) 0.034(4) 0.000(4)
O19 0.114(9) 0.066(5) 0.111(6) -0.028(4) 0.001(5) 0.016(4)
O20 0.099(8) 0.083(5) 0.091(5) 0.016(4) 0.018(4) -0.016(4)
O21 0.090(8) 0.115(7) 0.079(4) 0.008(4) 0.004(4) 0.012(4)
O22 0.067(8) 0.130(7) 0.102(5) 0.012(5) 0.000(4) -0.024(5)
O23 0.20(2) 0.064(7) 0.128(10) 0.000 -0.002(10) 0.000
O24 0.195(19) 0.036(5) 0.141(11) 0.000 0.045(9) 0.000
O25 0.105(10) 0.062(6) 0.061(5) 0.000 -0.012(5) 0.000
O26 0.096(12) 0.063(6) 0.192(13) 0.000 -0.012(9) 0.000
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'
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 O21 107.0(6) . 6_655 ?
O15 Si1 O1 109.9(6) . . ?
O15 Si1 O16 110.2(6) . . ?
O15 Si1 O21 109.0(6) . 6_655 ?
O16 Si1 O1 112.6(6) . . ?
O16 Si1 O21 107.9(6) . 6_655 ?
O1 Si2 O13 110.2(8) . . ?
O2 Si2 O1 107.4(6) . . ?
O2 Si2 O6 107.7(6) . . ?
O2 Si2 O13 109.3(7) . . ?
O6 Si2 O1 110.5(7) . . ?
O6 Si2 O13 111.5(8) . . ?
O3 Si3 O2 107.7(6) . . ?
O19 Si3 O2 108.2(6) 2 . ?
O19 Si3 O3 109.2(6) 2 . ?
O19 Si3 O20 110.6(6) 2 2 ?
O20 Si3 O2 109.5(5) 2 . ?
O20 Si3 O3 111.6(6) 2 . ?
O3 Si4 O4 108.3(7) . . ?
O3 Si4 O16 109.6(7) . 2 ?
O4 Si4 O16 109.7(6) . 2 ?
O17 Si4 O3 110.3(6) 2 . ?
O17 Si4 O4 108.3(5) 2 . ?
O17 Si4 O16 110.7(5) 2 2 ?
O4 Si5 O5 109.1(6) . . ?
O4 Si5 O14 111.8(6) . . ?
O5 Si5 O14 109.1(5) . . ?
O21 Si5 O4 110.9(6) . . ?
O21 Si5 O5 106.5(5) . . ?
O21 Si5 O14 109.3(7) . . ?
O5 Si6 O18 107.7(5) . . ?
O6 Si6 O5 109.3(6) . . ?
O6 Si6 O18 109.0(6) . . ?
O6 Si6 O19 112.7(5) . . ?
O19 Si6 O5 108.6(5) . . ?
O19 Si6 O18 109.4(5) . . ?
O17 Si7 O7 112.7(5) . . ?
O22 Si7 O7 102.7(6) 6_655 . ?
O22 Si7 O17 111.9(6) 6_655 . ?
O22 Si7 O23 111.2(8) 6_655 . ?
O23 Si7 O7 113.0(8) . . ?
O23 Si7 O17 105.6(6) . . ?
O7 Si8 O8 105.6(6) . . ?
O7 Si8 O12 116.0(7) . . ?
O12 Si8 O8 110.6(6) . . ?
O13 Si8 O7 106.6(9) . . ?
O13 Si8 O8 108.6(8) . . ?
O13 Si8 O12 109.1(9) . . ?
O8 Si9 O25 110.1(7) . . ?
O9 Si9 O8 109.8(6) . . ?
O9 Si9 O25 112.7(6) . . ?
O18 Si9 O8 108.1(6) 2 . ?
O18 Si9 O9 109.7(6) 2 . ?
O18 Si9 O25 106.3(5) 2 . ?
O9 Si10 O10 110.2(7) . . ?
O15 Si10 O9 109.3(6) 2 . ?
O15 Si10 O10 108.2(7) 2 . ?
O26 Si10 O9 112.5(7) . . ?
O26 Si10 O10 108.9(8) . . ?
O26 Si10 O15 107.7(7) . 2 ?
O10 Si11 O11 110.7(7) . . ?
O10 Si11 O14 109.8(7) . . ?
O10 Si11 O22 108.7(7) . . ?
O14 Si11 O11 107.9(6) . . ?
O22 Si11 O11 108.9(6) . . ?
O22 Si11 O14 110.8(7) . . ?
O11 Si12 O24 110.3(7) . . ?
O12 Si12 O11 106.6(7) . . ?
O12 Si12 O24 111.6(9) . . ?
O20 Si12 O11 110.4(6) . . ?
O20 Si12 O12 111.3(5) . . ?
O20 Si12 O24 106.6(7) . . ?
Si2 O1 Si1 150.7(7) . . ?
Si2 O2 Si3 154.9(7) . . ?
Si4 O3 Si3 173.2(9) . . ?
Si4 O4 Si5 156.8(6) . . ?
Si5 O5 Si6 148.1(7) . . ?
Si2 O6 Si6 158.3(7) . . ?
Si8 O7 Si7 152.0(7) . . ?
Si8 O8 Si9 155.0(8) . . ?
Si9 O9 Si10 155.7(7) . . ?
Si11 O10 Si10 166.2(9) . . ?
Si12 O11 Si11 155.8(8) . . ?
Si8 O12 Si12 166.2(7) . . ?
Si8 O13 Si2 176.6(13) . . ?
Si11 O14 Si5 173.0(10) . . ?
Si1 O15 Si10 150.2(7) . 2_554 ?
Si1 O16 Si4 163.4(9) . 2_554 ?
Si4 O17 Si7 146.2(6) 2_554 . ?
Si9 O18 Si6 146.5(6) 2_554 . ?
Si3 O19 Si6 159.8(7) 2_554 . ?
Si12 O20 Si3 146.3(7) . 2_554 ?
Si5 O21 Si1 147.1(6) . 6 ?
Si11 O22 Si7 149.4(7) . 6 ?
Si7 O23 Si7 151.3(11) 8 . ?
Si12 O24 Si12 148.8(11) . 8 ?
Si9 O25 Si9 146.2(8) . 8 ?
Si10 O26 Si10 143.5(13) 8 . ?
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 1.605(9) . ?
Si1 O15 1.551(9) . ?
Si1 O16 1.558(9) . ?
Si1 O21 1.621(12) 6_655 ?
Si2 O1 1.582(10) . ?
Si2 O2 1.557(9) . ?
Si2 O6 1.580(13) . ?
Si2 O13 1.607(13) . ?
Si3 O2 1.634(9) . ?
Si3 O3 1.612(12) . ?
Si3 O19 1.565(8) 2 ?
Si3 O20 1.593(8) 2 ?
Si4 O3 1.569(12) . ?
Si4 O4 1.574(9) . ?
Si4 O16 1.635(9) 2 ?
Si4 O17 1.552(8) 2 ?
Si5 O4 1.576(8) . ?
Si5 O5 1.579(9) . ?
Si5 O14 1.586(8) . ?
Si5 O21 1.561(11) . ?
Si6 O5 1.612(10) . ?
Si6 O6 1.598(13) . ?
Si6 O18 1.627(8) . ?
Si6 O19 1.600(9) . ?
Si7 O7 1.627(10) . ?
Si7 O17 1.608(8) . ?
Si7 O22 1.604(10) 6_655 ?
Si7 O23 1.604(6) . ?
Si8 O7 1.560(10) . ?
Si8 O8 1.579(9) . ?
Si8 O12 1.570(11) . ?
Si8 O13 1.557(13) . ?
Si9 O8 1.586(9) . ?
Si9 O9 1.581(11) . ?
Si9 O18 1.567(8) 2 ?
Si9 O25 1.589(5) . ?
Si10 O9 1.602(11) . ?
Si10 O10 1.617(10) . ?
Si10 O15 1.599(9) 2 ?
Si10 O26 1.594(7) . ?
Si11 O10 1.539(9) . ?
Si11 O11 1.593(10) . ?
Si11 O14 1.573(8) . ?
Si11 O22 1.562(10) . ?
Si12 O11 1.592(11) . ?
Si12 O12 1.587(11) . ?
Si12 O20 1.558(9) . ?
Si12 O24 1.597(6) . ?
_cod_database_fobs_code 2300668