#------------------------------------------------------------------------------
#$Date: 2021-05-06 10:08:50 +0300 (Thu, 06 May 2021) $
#$Revision: 264982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/23/2022344.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_2022344
loop_
_publ_author_name
'Shaw, Thomas E.'
'Sattelberger, Alfred P.'
'Jurca, Titel'
_publ_section_title
;
A 35-year-old mystery solved: a facile synthetic route and structural
confirmation of tetrachlorobis(diethyl ether)tungsten(IV)
;
_journal_coeditor_code YP3213
_journal_issue 4
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first 181
_journal_page_last 185
_journal_paper_doi 10.1107/S2053229621002412
_journal_volume 77
_journal_year 2021
_chemical_formula_iupac '[W Cl4 (C4 H10 O)2]'
_chemical_formula_moiety 'C8 H20 Cl4 O2 W'
_chemical_formula_sum 'C8 H20 Cl4 O2 W'
_chemical_formula_weight 473.89
_chemical_name_systematic
;
trans-Tetrachloridobis(diethyl ether-\kO)tungsten(IV)
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_cell_angle_alpha 90
_cell_angle_beta 106.339(4)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 7.5962(3)
_cell_length_b 11.4871(4)
_cell_length_c 9.0245(4)
_cell_measurement_reflns_used 2974
_cell_measurement_temperature 297.22(10)
_cell_measurement_theta_max 29.6070
_cell_measurement_theta_min 2.9320
_cell_volume 755.66(5)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2019)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2019)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2019)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 297.22(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device 'two-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Mini II'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0298
_diffrn_reflns_av_unetI/netI 0.0408
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 5730
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 30.667
_diffrn_reflns_theta_min 2.946
_diffrn_source 'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 8.332
_exptl_absorpt_correction_T_max 0.771
_exptl_absorpt_correction_T_min 0.514
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2019)
;
_exptl_crystal_colour 'clear dark yellow'
_exptl_crystal_density_diffrn 2.083
_exptl_crystal_description block
_exptl_crystal_F_000 452
_exptl_crystal_size_max 0.258
_exptl_crystal_size_mid 0.152
_exptl_crystal_size_min 0.084
_refine_diff_density_max 0.970
_refine_diff_density_min -0.837
_refine_ls_extinction_coef 0.0042(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref 1.013
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 73
_refine_ls_number_reflns 2198
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.013
_refine_ls_R_factor_all 0.0427
_refine_ls_R_factor_gt 0.0255
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0201P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0529
_refine_ls_wR_factor_ref 0.0577
_reflns_number_gt 1587
_reflns_number_total 2198
_reflns_threshold_expression 'I > 2\s(I)'
_iucr_refine_instructions_details
;
TITL exp_229_a.res in P2(1)/n
exp_229.res
created by SHELXL-2018/3 at 13:21:40 on 28-Feb-2021
REM Old TITL exp_229 in P2(1)/n
REM SHELXT solution in P2(1)/n: R1 0.092, Rweak 0.001, Alpha 0.018
REM 0.560 for 87 systematic absences, Orientation as input
REM Formula found by SHELXT: C16 C3 Cl1 W
CELL 0.71073 7.5962 11.4871 9.0245 90 106.339 90
ZERR 2 0.0003 0.0004 0.0004 0 0.004 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Cl O W
UNIT 16 40 8 4 2
L.S. 15
PLAN 5
CONF
MORE -1
BOND $H
fmap 2
acta
OMIT 2 2 0
OMIT 0 5 11
OMIT -10 0 4
REM
REM
REM
WGHT 0.020100
EXTI 0.004224
FVAR 0.77547
W1 5 0.500000 0.500000 0.500000 10.50000 0.02576 0.03029 =
0.02982 0.00141 0.01026 -0.00172
CL1 3 0.501317 0.626636 0.294588 11.00000 0.06378 0.04343 =
0.04164 0.01068 0.02364 0.00156
CL2 3 0.187546 0.462612 0.379500 11.00000 0.02967 0.06035 =
0.05692 -0.00779 0.00741 -0.00428
O1 4 0.571255 0.362736 0.379855 11.00000 0.03414 0.03095 =
0.04663 -0.00612 0.02177 -0.00521
C3 1 0.478177 0.248943 0.360301 11.00000 0.04464 0.03510 =
0.05158 -0.00762 0.01639 -0.01194
AFIX 23
H3A 2 0.431735 0.231808 0.250967 11.00000 -1.20000
H3B 2 0.374195 0.252988 0.402553 11.00000 -1.20000
AFIX 0
C1 1 0.719131 0.371883 0.302743 11.00000 0.03634 0.04382 =
0.05259 -0.00248 0.02568 0.00067
AFIX 23
H1A 2 0.809652 0.311634 0.342222 11.00000 -1.20000
H1B 2 0.779554 0.446707 0.327048 11.00000 -1.20000
AFIX 0
C2 1 0.646699 0.359704 0.131124 11.00000 0.06914 0.07250 =
0.05279 -0.00349 0.02868 0.00565
AFIX 137
H2A 2 0.741798 0.378525 0.084061 11.00000 -1.50000
H2B 2 0.545042 0.411744 0.093420 11.00000 -1.50000
H2C 2 0.606815 0.281033 0.105847 11.00000 -1.50000
AFIX 0
C4 1 0.602601 0.152136 0.438146 11.00000 0.08165 0.03480 =
0.07463 0.00435 0.02070 0.00102
AFIX 137
H4A 2 0.699018 0.142437 0.389573 11.00000 -1.50000
H4B 2 0.533600 0.081207 0.429453 11.00000 -1.50000
H4C 2 0.654820 0.170806 0.545233 11.00000 -1.50000
AFIX 0
HKLF 4
REM exp_229_a.res in P2(1)/n
REM wR2 = 0.0577, GooF = S = 1.013, Restrained GooF = 1.013 for all data
REM R1 = 0.0255 for 1587 Fo > 4sig(Fo) and 0.0427 for all 2198 data
REM 73 parameters refined using 0 restraints
END
WGHT 0.0201 0.0000
REM Highest difference peak 0.970, deepest hole -0.837, 1-sigma level 0.129
Q1 1 0.3777 0.5015 0.5189 11.00000 0.05 0.97
Q2 1 0.2540 0.5003 0.3367 11.00000 0.05 0.67
Q3 1 0.3834 0.4444 0.4197 11.00000 0.05 0.63
Q4 1 0.3797 0.5016 0.3451 11.00000 0.05 0.57
Q5 1 0.6081 0.6217 0.2948 11.00000 0.05 0.50
REM The information below was added by Olex2.
REM
REM R1 = 0.0255 for 1587 Fo > 4sig(Fo) and 0.0427 for all 5945 data
REM 73 parameters refined using n/a restraints
REM Highest difference peak 0.97, deepest hole -0.84
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0427
REM R1_gt = 0.0255
REM wR_ref = 0.0577
REM GOOF = 1.013
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 5945
REM Reflections_gt = 1587
REM Parameters = 73
REM Hole = -0.84
REM Peak = 0.97
REM Flack = n/a
;
_cod_data_source_file yp3213sup1.cif
_cod_data_source_block I
_cod_depositor_comments 'Adding full bibliography for 2022344.cif.'
_cod_database_code 2022344
_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'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W W1 0.500000 0.500000 0.500000 0.02813(8) Uani d 1 . .
Cl Cl1 0.50132(15) 0.62664(9) 0.29459(12) 0.0478(3) Uani d 1 . .
Cl Cl2 0.18755(13) 0.46261(10) 0.37950(14) 0.0499(3) Uani d 1 . .
O O1 0.5713(3) 0.36274(19) 0.3799(3) 0.0351(6) Uani d 1 . .
C C3 0.4782(5) 0.2489(3) 0.3603(4) 0.0432(9) Uani d 1 . .
H H3A 0.431735 0.231808 0.250967 0.052 Uiso calc 1 . .
H H3B 0.374195 0.252988 0.402553 0.052 Uiso calc 1 . .
C C1 0.7191(5) 0.3719(3) 0.3027(4) 0.0416(9) Uani d 1 . .
H H1A 0.809652 0.311634 0.342222 0.050 Uiso calc 1 . .
H H1B 0.779554 0.446707 0.327048 0.050 Uiso calc 1 . .
C C2 0.6467(5) 0.3597(4) 0.1311(5) 0.0625(13) Uani d 1 . .
H H2A 0.741798 0.378525 0.084061 0.094 Uiso calc 1 . .
H H2B 0.545042 0.411744 0.093420 0.094 Uiso calc 1 . .
H H2C 0.606815 0.281033 0.105847 0.094 Uiso calc 1 . .
C C4 0.6026(5) 0.1521(3) 0.4381(5) 0.0640(13) Uani d 1 . .
H H4A 0.699018 0.142437 0.389573 0.096 Uiso calc 1 . .
H H4B 0.533600 0.081207 0.429453 0.096 Uiso calc 1 . .
H H4C 0.654820 0.170806 0.545233 0.096 Uiso calc 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
W1 0.02576(11) 0.03029(12) 0.02982(12) -0.00172(8) 0.01026(8) 0.00141(10)
Cl1 0.0638(7) 0.0434(6) 0.0416(6) 0.0016(5) 0.0236(5) 0.0107(5)
Cl2 0.0297(4) 0.0603(6) 0.0569(7) -0.0043(4) 0.0074(5) -0.0078(6)
O1 0.0341(13) 0.0310(13) 0.0466(16) -0.0052(10) 0.0218(12) -0.0061(12)
C3 0.045(2) 0.035(2) 0.052(3) -0.0119(17) 0.016(2) -0.008(2)
C1 0.036(2) 0.044(2) 0.053(3) 0.0007(16) 0.0257(19) -0.002(2)
C2 0.069(3) 0.073(3) 0.053(3) 0.006(2) 0.029(3) -0.003(3)
C4 0.082(3) 0.035(2) 0.075(3) 0.001(2) 0.021(3) 0.004(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_diffrn_refln_index_h
_diffrn_refln_index_k
_diffrn_refln_index_l
0 0 1
0 0 -1
0 0 -1
0 0 2
0 0 -2
0 0 2
0 0 -2
0 0 -3
0 0 -3
0 0 3
0 0 3
0 0 4
0 0 -4
0 0 -4
0 0 -5
0 0 -5
0 0 5
0 0 6
0 0 -6
0 0 -7
0 0 -8
0 0 -9
0 0 -10
0 0 -11
0 0 -12
0 -1 0
0 1 -1
0 1 -1
0 1 1
0 -1 -1
0 -1 1
0 -1 1
0 1 -2
0 1 -2
0 1 -2
0 -1 2
0 -1 -2
0 -1 -2
0 1 2
0 -1 -3
0 1 -3
0 1 -3
0 -1 -3
0 -1 3
0 1 3
0 -1 -3
0 1 3
0 -1 -4
0 1 4
0 -1 -4
0 1 -4
0 -1 4
0 1 4
0 -1 4
0 1 -4
0 -1 -5
0 -1 -5
0 -1 5
0 1 -5
0 1 -5
0 -1 -5
0 1 -6
0 1 -6
0 -1 -6
0 -1 6
0 1 -7
0 -1 7
0 -1 -7
0 1 -8
0 -1 -8
0 -1 8
0 1 -9
0 -1 -9
0 -1 -10
0 1 -10
0 1 -11
0 -1 -11
0 1 -12
0 -1 -12
0 2 0
0 -2 0
0 2 1
0 2 1
0 -2 1
0 -2 1
0 -2 -1
0 2 -1
0 2 -1
0 2 -2
0 -2 -2
0 2 2
0 -2 -2
0 2 -2
0 2 -2
0 -2 2
0 2 2
0 2 2
0 -2 2
0 2 3
0 2 -3
0 -2 3
0 2 3
0 2 -3
0 2 -3
0 -2 -3
0 2 3
0 2 4
0 2 -4
0 -2 4
0 2 -4
0 -2 -4
0 2 -4
0 -2 -4
0 -2 -4
0 2 4
0 -2 -5
0 2 -5
0 2 -5
0 2 -5
0 2 -6
0 -2 6
0 -2 -6
0 2 -6
0 -2 -7
0 -2 7
0 2 -7
0 2 -8
0 -2 -8
0 2 -9
0 -2 -9
0 2 -10
0 -2 -10
0 -2 -11
0 2 -11
0 2 -12
0 -2 -12
0 3 0
0 3 0
0 -3 0
0 -3 1
0 3 -1
0 -3 -1
0 3 1
0 -3 1
0 3 1
0 3 1
0 -3 1
0 3 -2
0 3 -2
0 3 2
0 -3 2
0 3 -2
0 -3 2
0 -3 -2
0 -3 -2
0 3 2
0 -3 3
0 -3 3
0 3 3
0 3 3
0 3 -3
0 -3 -3
0 3 3
0 -3 -3
0 3 -3
0 3 -3
0 3 4
0 3 -4
0 3 -4
0 -3 -4
0 3 -4
0 -3 -5
0 3 -5
0 3 -5
0 3 -6
0 3 -6
0 -3 -6
0 -3 7
0 -3 -7
0 3 -7
0 3 -8
0 -3 -8
0 3 -9
0 -3 -9
0 3 -10
0 -3 -10
0 -3 -11
0 3 -11
0 -4 0
0 4 0
0 4 0
0 -4 1
0 -4 -1
0 4 -1
0 -4 1
0 -4 -1
0 -4 1
0 4 2
0 -4 2
0 4 -2
0 4 2
0 4 2
0 4 -2
0 -4 2
0 -4 -2
0 4 -2
0 4 2
0 -4 2
0 4 -3
0 -4 3
0 -4 3
0 4 3
0 4 -3
0 4 3
0 -4 -3
0 4 -3
0 -4 -3
0 -4 4
0 -4 -4
0 4 -4
0 4 -4
0 -4 -4
0 4 -4
0 4 4
0 4 -5
0 4 -5
0 -4 -5
0 -4 -6
0 4 -6
0 4 -6
0 4 -7
0 -4 -7
0 4 -7
0 4 -8
0 -4 -8
0 4 -9
0 -4 -9
0 4 -10
0 4 -11
0 -5 0
0 5 0
0 -5 0
0 -5 0
0 5 0
0 -5 1
0 -5 -1
0 -5 -1
0 -5 -1
0 5 -1
0 5 -1
0 -5 1
0 -5 2
0 -5 -2
0 -5 2
0 5 -2
0 5 -2
0 -5 2
0 5 2
0 5 -2
0 5 -3
0 5 -3
0 -5 3
0 -5 3
0 5 -3
0 -5 4
0 5 -4
0 5 -4
0 -5 -4
0 -5 -5
0 5 -5
0 5 -5
0 -5 -6
0 5 -6
0 5 -6
0 -5 -7
0 5 -7
0 5 -7
0 5 -8
0 5 -9
0 5 -10
0 5 -11
0 -6 0
0 6 0
0 -6 0
0 6 0
0 -6 0
0 6 -1
0 -6 1
0 -6 -1
0 -6 -1
0 6 -1
0 -6 2
0 6 -2
0 -6 -2
0 -6 -2
0 6 -2
0 -6 3
0 6 -3
0 6 -3
0 -6 3
0 6 -4
0 6 -4
0 -6 4
0 6 -5
0 -6 5
0 6 -5
0 6 -6
0 6 -6
0 6 -7
0 6 -7
0 6 -8
0 6 -9
0 6 -10
0 6 -11
0 7 0
0 -7 0
0 -7 -1
0 7 -1
0 -7 1
0 7 -2
0 7 -2
0 -7 2
0 7 -3
0 7 -3
0 -7 3
0 7 -4
0 -7 4
0 7 -4
0 7 -5
0 7 -5
0 -7 5
0 7 -6
0 7 -6
0 7 -7
0 7 -7
0 7 -8
0 7 -8
0 7 -9
0 7 -10
0 7 -11
0 8 0
0 -8 0
0 -8 1
0 8 -1
0 -8 2
0 8 -2
0 8 2
0 8 -3
0 -8 3
0 8 -4
0 -8 4
0 8 -5
0 -8 5
0 8 -6
0 8 -6
0 8 -7
0 8 -7
0 8 -8
0 8 -8
0 8 -9
0 8 -10
0 -9 0
0 9 0
0 9 1
0 -9 1
0 -9 -1
0 9 -1
0 9 -2
0 -9 2
0 -9 3
0 9 -3
0 9 -4
0 -9 4
0 -9 5
0 9 -5
0 -9 6
0 9 -6
0 9 -7
0 9 -8
0 -10 0
0 10 0
0 10 -1
0 10 1
0 -10 1
0 -10 -1
0 10 -2
0 -10 2
0 10 -3
0 -10 3
0 10 -4
0 -10 4
0 10 -5
0 -10 5
0 10 -6
0 10 -7
0 10 -8
0 -11 0
0 11 0
0 -11 -1
0 11 -1
0 -11 1
0 11 -2
0 -11 -2
0 -11 3
0 11 -3
0 -11 4
0 11 -4
0 -11 5
0 11 -5
0 11 -6
0 11 -7
0 11 -8
0 11 -9
0 12 0
0 -12 0
0 -12 -1
0 -12 1
0 12 -1
0 -12 -2
0 12 -2
0 -12 2
0 -12 -3
0 12 -3
0 -12 3
0 12 -4
0 -12 4
0 -12 5
0 12 -5
0 12 -6
0 12 -7
0 12 -8
0 -13 0
0 13 -1
0 -13 1
0 -13 -1
0 13 -2
0 -13 -2
0 -13 2
0 -13 3
0 13 -3
0 -13 4
0 13 -4
0 -13 -4
0 13 -5
0 13 -6
0 13 -7
0 -14 0
0 -14 1
0 -14 -1
0 -14 -2
0 -14 2
0 14 -2
0 -14 3
0 -14 -3
0 14 -3
0 -14 4
0 14 -4
0 -14 -4
0 -14 -5
0 14 -5
0 14 -6
0 -15 0
0 -15 -1
0 15 -2
0 -15 -2
0 -15 2
0 -15 3
0 -15 -3
0 15 -3
0 -15 -4
0 15 -4
0 -16 0
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-8 -6 8
8 6 -8
8 6 -7
8 6 -7
8 6 -6
8 6 -6
8 6 -6
8 6 -5
8 6 -5
8 6 -5
8 6 -4
8 6 -4
8 6 -4
8 6 -3
8 6 -3
8 6 -2
-8 6 2
8 6 -2
8 6 -1
-8 6 1
8 6 -1
-8 -6 0
8 6 0
-8 6 0
-8 -6 -1
8 6 1
-8 6 -1
-8 -6 -2
8 6 2
-8 6 -2
-8 -6 -3
-8 6 -3
-8 -6 -4
-8 6 -4
-8 6 -4
-8 -7 9
8 7 -8
8 7 -7
8 7 -7
8 7 -6
8 7 -6
8 7 -5
8 7 -5
8 7 -5
8 7 -4
8 7 -4
8 7 -4
8 7 -3
8 7 -3
8 7 -2
-8 7 2
8 7 -2
8 7 -1
-8 7 1
8 7 -1
-8 -7 0
8 7 0
-8 7 0
8 7 0
-8 -7 -1
8 7 1
-8 7 -1
8 7 1
-8 -7 -2
-8 7 -2
-8 -7 -3
-8 7 -3
-8 7 -3
8 8 -8
8 8 -8
8 8 -7
8 8 -7
8 8 -6
8 8 -6
8 8 -5
8 8 -5
8 8 -5
8 8 -4
8 8 -4
8 8 -4
8 8 -3
8 8 -3
8 8 -2
8 8 -2
8 8 -1
-8 8 1
8 8 -1
8 8 0
-8 8 0
8 8 0
-8 -8 -1
8 8 1
-8 8 -1
-8 -8 -2
-8 8 -2
-8 -8 -3
8 9 -7
8 9 -7
8 9 -6
8 9 -6
8 9 -5
8 9 -5
8 9 -4
8 9 -4
8 9 -4
8 9 -3
8 9 -3
8 9 -3
8 9 -2
8 9 -2
8 9 -1
8 9 -1
8 9 0
-8 9 0
-8 -9 -1
-8 9 -1
-8 -9 -2
8 10 -6
8 10 -5
8 10 -5
8 10 -4
8 10 -4
8 10 -3
8 10 -3
8 10 -3
8 10 -2
8 10 -2
8 10 -1
8 10 0
-8 10 0
9 0 -5
9 0 -5
9 0 -5
9 0 -4
9 0 -4
9 0 -3
9 0 -2
-9 0 1
9 0 -1
-9 0 0
9 0 0
-9 0 -1
9 0 1
-9 0 -2
9 0 2
-9 0 -3
9 1 -7
9 1 -6
9 1 -6
9 1 -5
9 1 -5
9 1 -5
9 1 -4
9 -1 -4
9 1 -4
9 -1 -4
9 1 -3
9 -1 -3
9 1 -2
9 -1 -2
-9 -1 1
9 1 -1
9 -1 -1
-9 -1 0
-9 1 0
9 1 0
-9 1 0
-9 1 -1
-9 -1 -1
-9 1 -1
9 1 1
-9 1 -2
-9 -1 -2
-9 1 -2
9 1 2
-9 1 -3
-9 -1 -3
9 1 3
9 2 -9
9 2 -8
9 2 -7
9 2 -7
9 2 -6
9 2 -6
9 2 -6
9 2 -5
9 2 -5
9 2 -5
9 2 -4
9 -2 -4
9 2 -4
9 2 -3
9 -2 -3
9 2 -3
9 2 -2
9 -2 -2
-9 2 1
-9 -2 1
-9 2 0
-9 -2 0
9 2 0
-9 -2 -1
9 2 1
-9 2 -1
-9 2 -2
-9 -2 -2
9 2 2
-9 2 -3
-9 -2 -3
9 2 3
9 3 -9
9 3 -8
9 3 -7
9 3 -7
9 3 -6
9 3 -6
9 3 -6
9 3 -5
9 3 -5
9 3 -5
9 3 -4
9 3 -4
9 3 -3
9 -3 -3
9 3 -3
-9 3 2
9 3 -2
-9 3 1
-9 -3 1
9 3 -1
-9 -3 0
-9 3 0
9 3 0
-9 3 -1
-9 -3 -1
-9 -3 -2
-9 3 -2
9 3 2
-9 3 -3
-9 -3 -3
9 3 3
9 4 -9
9 4 -8
9 4 -7
9 4 -7
9 4 -6
9 4 -6
9 4 -6
9 4 -5
9 4 -5
9 4 -5
9 4 -4
9 4 -4
-9 4 3
9 4 -3
9 4 -3
-9 4 2
9 4 -2
9 4 -2
-9 -4 1
-9 4 1
9 4 -1
-9 -4 0
-9 4 0
9 4 0
-9 -4 -1
-9 4 -1
9 4 1
-9 -4 -2
-9 4 -2
9 4 2
9 5 -8
9 5 -7
9 5 -7
9 5 -6
9 5 -6
9 5 -6
9 5 -5
9 5 -5
9 5 -5
9 5 -4
9 5 -4
9 5 -3
9 5 -3
-9 5 2
9 5 -2
9 5 -2
-9 5 1
9 5 -1
9 5 -1
-9 -5 0
-9 5 0
9 5 0
-9 -5 -1
-9 5 -1
9 5 1
-9 -5 -2
-9 5 -2
9 6 -7
9 6 -7
9 6 -6
9 6 -6
9 6 -6
9 6 -5
9 6 -5
9 6 -5
9 6 -4
9 6 -4
9 6 -4
9 6 -3
9 6 -3
-9 6 2
9 6 -2
9 6 -2
-9 6 1
9 6 -1
9 6 -1
-9 -6 0
-9 6 0
9 6 0
9 6 0
-9 -6 -1
-9 6 -1
9 6 1
9 7 -7
9 7 -6
9 7 -6
9 7 -6
9 7 -5
9 7 -5
9 7 -5
9 7 -4
9 7 -4
9 7 -4
9 7 -3
9 7 -3
9 7 -2
9 7 -2
-9 7 1
9 7 -1
9 7 -1
-9 7 0
9 7 0
9 7 0
-9 -7 -1
9 7 1
-9 7 -1
9 7 1
9 8 -5
9 8 -5
9 8 -5
9 8 -4
9 8 -4
9 8 -4
9 8 -3
9 8 -3
9 8 -2
9 8 -2
9 8 -1
-9 8 1
9 8 -1
9 8 0
-9 8 0
9 8 0
9 9 -2
10 0 -5
10 0 -4
10 0 -4
10 0 -2
10 0 -1
-10 0 0
10 0 0
-10 0 -1
10 1 -5
10 1 -5
10 1 -5
10 1 -4
10 1 -4
10 1 -3
10 -1 -3
10 1 -3
10 1 -2
10 -1 -2
-10 -1 1
10 1 -1
10 -1 -1
-10 -1 0
10 1 0
10 -1 0
-10 -1 -1
10 2 -7
10 2 -6
10 2 -6
10 2 -5
10 2 -5
10 2 -5
10 2 -4
10 -2 -4
10 2 -4
10 2 -3
10 -2 -3
10 2 -3
10 2 -2
10 -2 -2
-10 -2 1
10 2 -1
10 -2 -1
-10 -2 0
10 3 -7
10 3 -7
10 3 -6
10 3 -6
10 3 -6
10 3 -5
10 3 -5
10 3 -5
10 3 -4
10 3 -4
10 3 -3
10 -3 -3
10 3 -3
10 -3 -2
10 3 -2
-10 3 1
10 3 -1
-10 3 0
-10 -3 0
10 3 0
10 4 -6
10 4 -6
10 4 -6
10 4 -5
10 4 -5
10 4 -5
10 4 -4
10 4 -4
10 4 -3
10 -4 -3
10 4 -3
-10 4 2
10 4 -2
10 4 -2
-10 4 1
10 4 -1
10 5 -6
10 5 -5
10 5 -5
10 5 -5
10 5 -4
10 5 -4
10 5 -3
10 5 -3
-10 5 2
10 5 -2
10 5 -2
-10 5 1
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-6 12 -1 0.0909
-10 5 6 0.0912
6 8 -10 0.0953
10 -3 -7 0.1184
-1 -12 8 0.0348
-10 -3 2 0.0967
2 -10 -10 0.0433
0 10 9 0.0307
-7 2 -7 0.0851
3 -1 -13 0.0760
-2 -6 -10 0.0605
6 13 -3 0.0961
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 W1 Cl1 . 3_666 180.0 y
Cl2 W1 Cl1 . 3_666 91.37(4) y
Cl2 W1 Cl1 3_666 . 91.37(4) ?
Cl2 W1 Cl1 3_666 3_666 88.63(4) ?
Cl2 W1 Cl1 . . 88.63(4) y
Cl2 W1 Cl2 3_666 . 180.0 y
O1 W1 Cl1 3_666 3_666 89.92(7) ?
O1 W1 Cl1 . . 89.92(7) y
O1 W1 Cl1 3_666 . 90.08(7) ?
O1 W1 Cl1 . 3_666 90.08(7) y
O1 W1 Cl2 . 3_666 90.16(7) y
O1 W1 Cl2 3_666 . 90.16(7) ?
O1 W1 Cl2 . . 89.84(7) y
O1 W1 Cl2 3_666 3_666 89.84(7) ?
O1 W1 O1 . 3_666 180.0 y
C3 O1 W1 . . 123.46(18) ?
C3 O1 C1 . . 114.1(2) ?
C1 O1 W1 . . 122.43(19) ?
O1 C3 H3A . . 109.1 ?
O1 C3 H3B . . 109.1 ?
O1 C3 C4 . . 112.6(3) ?
H3A C3 H3B . . 107.8 ?
C4 C3 H3A . . 109.1 ?
C4 C3 H3B . . 109.1 ?
O1 C1 H1A . . 109.2 ?
O1 C1 H1B . . 109.2 ?
O1 C1 C2 . . 111.9(3) ?
H1A C1 H1B . . 107.9 ?
C2 C1 H1A . . 109.2 ?
C2 C1 H1B . . 109.2 ?
C1 C2 H2A . . 109.5 ?
C1 C2 H2B . . 109.5 ?
C1 C2 H2C . . 109.5 ?
H2A C2 H2B . . 109.5 ?
H2A C2 H2C . . 109.5 ?
H2B C2 H2C . . 109.5 ?
C3 C4 H4A . . 109.5 ?
C3 C4 H4B . . 109.5 ?
C3 C4 H4C . . 109.5 ?
H4A C4 H4B . . 109.5 ?
H4A C4 H4C . . 109.5 ?
H4B C4 H4C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
W1 Cl1 3_666 2.3586(10) ?
W1 Cl1 . 2.3586(10) y
W1 Cl2 3_666 2.3554(10) ?
W1 Cl2 . 2.3554(10) y
W1 O1 3_666 2.070(2) ?
W1 O1 . 2.070(2) y
O1 C1 . 1.482(3) y
O1 C3 . 1.473(4) y
C3 H3A . 0.9700 ?
C3 H3B . 0.9700 ?
C3 C4 . 1.500(5) ?
C1 H1A . 0.9700 ?
C1 H1B . 0.9700 ?
C1 C2 . 1.497(4) ?
C2 H2A . 0.9600 ?
C2 H2B . 0.9600 ?
C2 H2C . 0.9600 ?
C4 H4A . 0.9600 ?
C4 H4B . 0.9600 ?
C4 H4C . 0.9600 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
W1 O1 C3 C4 . . . . -115.4(3) ?
W1 O1 C1 C2 . . . . -115.7(3) ?
C3 O1 C1 C2 . . . . 63.1(4) ?
C1 O1 C3 C4 . . . . 65.8(4) ?