#------------------------------------------------------------------------------
#$Date: 2021-06-05 20:42:22 +0200 (Sat 05 de Jun de 2021) $
#$Revision: 266044 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/73/7707330.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7707330
loop_
_publ_author_name
'Löber, Manuel'
'Ströbele, Markus'
'Romao, Carl P.'
'Meyer, Hans-Jürgen'
_publ_section_title
;
 W₂O₃I₄ and WO₂I₂:
 metallic phases in the chemical transport reaction of tungsten.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6789
_journal_page_last               6792
_journal_paper_doi               10.1039/d1dt01212f
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'I2 O2 W'
_chemical_formula_sum            'I2 O2 W'
_chemical_formula_weight         469.65
_space_group_crystal_system      orthorhombic
_space_group_IT_number           71
_space_group_name_Hall           '-I 2 2'
_space_group_name_H-M_alt        'I m m m'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-05-18
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_audit_update_record
;
2020-05-18 deposited with the CCDC.	2021-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   3.7484(3)
_cell_length_b                   3.9049(3)
_cell_length_c                   16.6283(13)
_cell_measurement_reflns_used    746
_cell_measurement_temperature    99.98(13)
_cell_measurement_theta_max      33.3150
_cell_measurement_theta_min      4.8930
_cell_volume                     243.39(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.65a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.65a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.65a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -60.00  -3.00   0.50    5.06    --  -15.51 -57.00  60.00  114
  2  ω    -25.00   4.00   0.50    5.06    --  -15.51 -73.00  72.05   58
  3  ω    -60.00  -8.00   0.50    5.06    --   17.55 -19.00 120.00  104
  4  ω    -60.00  -3.00   0.50    5.06    --  -15.51 -57.00 120.00  114
  5  ω     12.00  63.00   0.50    5.06    --   17.55-123.00 -78.00  102
  6  ω    -38.00   1.00   0.50    5.06    --  -15.51 -67.00-166.75   78
  7  ω    -60.00  -3.00   0.50    5.06    --  -15.51 -57.00-180.00  114
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0272907000
_diffrn_orient_matrix_UB_12      -0.1082707000
_diffrn_orient_matrix_UB_13      -0.0336861000
_diffrn_orient_matrix_UB_21      -0.0077291000
_diffrn_orient_matrix_UB_22      -0.1442495000
_diffrn_orient_matrix_UB_23      0.0258736000
_diffrn_orient_matrix_UB_31      -0.1870718000
_diffrn_orient_matrix_UB_32      0.0217917000
_diffrn_orient_matrix_UB_33      0.0038558000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            873
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.930
_diffrn_reflns_theta_min         4.904
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    36.259
_exptl_absorpt_correction_T_max  0.620
_exptl_absorpt_correction_T_min  0.246
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.65a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    6.408
_exptl_crystal_description       plate
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.061
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.016
_exptl_crystal_size_rad          0.016
_refine_diff_density_max         0.816
_refine_diff_density_min         -1.243
_refine_diff_density_rms         0.243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     14
_refine_ls_number_reflns         166
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0203
_refine_ls_R_factor_gt           0.0181
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+2.0270P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0403
_refine_ls_wR_factor_ref         0.0411
_reflns_Friedel_coverage         0.000
_reflns_number_gt                157
_reflns_number_total             166
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt01212f2.cif
_cod_data_source_block           wo2i2_2
_cod_depositor_comments
'Adding full bibliography for 7707330--7707331.cif.'
_cod_original_cell_volume        243.39(4)
_cod_database_code               7707330
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         WO2I2
_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.
;
_reflns_odcompleteness_completeness 99.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
;
_shelx_res_file
;
TITL wo2i2_2_a.res in Immm
    wo2i2_2.res
    created by SHELXL-2018/3 at 11:55:19 on 18-May-2020
REM Old TITL WO2I2_2 in Immm
REM SHELXT solution in Immm: R1 0.188, Rweak 0.012, Alpha 0.036
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: O4 I2 W
CELL 0.71073 3.748392 3.904919 16.628256 90 90 90
ZERR 2 0.00031 0.000347 0.001349 0 0 0
LATT 2
SYMM -X,-Y,+Z
SYMM -X,+Y,-Z
SYMM +X,-Y,-Z
SFAC I O W
UNIT 4 4 2
ISOR 0.01 0.002 O1

L.S. 4
PLAN  5
TEMP -173
CONF
MORE -1
fmap 2
acta
SHEL 0.81 99
REM <olex2.extras>
REM <HklSrc "%.\\WO2I2_2.hkl">
REM </olex2.extras>

WGHT    0.000000    2.027000
FVAR       0.48016
W1    3    0.500000    0.500000    0.500000    10.12500    0.00469    0.10554 =
         0.00694    0.00000    0.00000    0.00000
I1    1    0.500000    0.500000    0.660719    10.25000    0.00965    0.01639 =
         0.01157    0.00000    0.00000    0.00000
O1    2    0.500000    0.000000    0.500000    10.12500    0.01593    0.00192 =
         0.00094    0.00000    0.00000    0.00000
O2    2    0.000000    0.500000    0.500000    10.12500    0.00493    0.04222 =
         0.00619    0.00000    0.00000    0.00000
HKLF 4




REM  wo2i2_2_a.res in Immm
REM wR2 = 0.0411, GooF = S = 1.071, Restrained GooF = 1.055 for all data
REM R1 = 0.0181 for 157 Fo > 4sig(Fo) and 0.0203 for all 166 data
REM 14 parameters refined using 6 restraints

END

WGHT      0.0000      2.0269

REM Highest difference peak  0.816,  deepest hole -1.243,  1-sigma level  0.243
Q1    1   0.5000  0.0000  0.6317  10.25000  0.05    0.82
Q2    1   0.5941 -0.0672  0.5000  10.50000  0.05    0.75
Q3    1   0.5000  0.6101  0.5259  10.50000  0.05    0.72
Q4    1   0.1220  0.0000  0.4833  10.50000  0.05    0.70
Q5    1   0.5000  0.7586  0.6784  10.50000  0.05    0.59
;
_shelx_res_checksum              56492
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.904
_oxdiff_exptl_absorpt_empirical_full_min 0.462
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
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
W1 W 0.500000 0.500000 0.500000 0.0391(3) Uani 1 8 d S T P . .
I1 I 0.500000 0.500000 0.66072(4) 0.0125(2) Uani 1 4 d S T P . .
O1 O 0.500000 0.000000 0.500000 0.0063(19) Uani 1 8 d S TU P . .
O2 O 0.000000 0.500000 0.500000 0.018(2) Uani 1 8 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
W1 0.0047(3) 0.1055(9) 0.0069(4) 0.000 0.000 0.000
I1 0.0096(3) 0.0164(4) 0.0116(4) 0.000 0.000 0.000
O1 0.016(4) 0.002(4) 0.001(4) 0.000 0.000 0.000
O2 0.005(5) 0.042(7) 0.006(5) 0.000 0.000 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
I I -0.4742 1.8119 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 0 1 0.0273
2 0 -1 0.0321
0 -5 11 0.0207
0 5 -11 0.0141
0 4 17 0.0141
0 -4 -17 0.0151
0 -1 23 0.0103
0 1 -23 0.0056
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
I1 W1 I1 180.0 . 9_666 ?
O1 W1 I1 90.0 . 9_666 ?
O1 W1 I1 90.0 . . ?
O1 W1 I1 90.0 1_565 9_666 ?
O1 W1 I1 90.0 1_565 . ?
O1 W1 O1 180.0 1_565 . ?
O2 W1 I1 90.0 . . ?
O2 W1 I1 90.0 . 9_666 ?
O2 W1 I1 90.0 1_655 . ?
O2 W1 I1 90.0 1_655 9_666 ?
O2 W1 O1 90.0 . . ?
O2 W1 O1 90.0 1_655 . ?
O2 W1 O1 90.0 1_655 1_565 ?
O2 W1 O1 90.0 . 1_565 ?
O2 W1 O2 180.0 1_655 . ?
W1 O1 W1 180.0 1_545 . ?
W1 O2 W1 180.0 1_455 . ?
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
W1 I1 2.6725(7) 9_666 ?
W1 I1 2.6725(7) . ?
W1 O1 1.95246(17) . ?
W1 O1 1.95246(17) 1_565 ?
W1 O2 1.87420(15) 1_655 ?
W1 O2 1.87420(15) . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.9990 -0.0007 1.0159 0.0204 0.0418 0.3779
1.9990 0.0007 -1.0159 -0.0204 -0.0418 -0.3779
0.2073 -4.8036 11.4085 0.1301 0.9865 -0.0995
-0.0812 4.7980 -11.4827 -0.1305 -0.9886 0.0755
0.3816 3.6521 17.4632 -0.9941 -0.0779 0.0755
-0.0767 -3.6688 -17.4779 0.9881 0.0776 -0.1330
0.3581 -0.6247 23.2407 -0.7250 0.6887 0.0090
-0.3581 0.6247 -23.2407 0.7250 -0.6887 -0.0090
