W<sub>2</sub>O<sub>3</sub>I<sub>4</sub> and WO<sub>2</sub>I<sub>2</sub>: metallic phases in the chemical transport reaction of tungsten.
Löber, Manuel; Ströbele, Markus; Romao, Carl P.; Meyer, Hans-Jürgen; Dalton transactions (Cambridge, England : 2003) 50 (2021) 6789–6792; doi:10.1039/d1dt01212f

data_7707331
_publ_section_title
;
 W<sub>2</sub>O<sub>3</sub>I<sub>4</sub> and WO<sub>2</sub>I<sub>2</sub>:
 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         'I4 O3 W2'
_chemical_formula_sum            'I4 O3 W2'
_chemical_formula_weight         923.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-I 2y'
_space_group_name_H-M_alt        'I 1 2/m 1'
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-17
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2021-01-17 deposited with the CCDC.	2021-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.810(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2484(6)
_cell_length_b                   7.4882(4)
_cell_length_c                   13.3648(8)
_cell_measurement_reflns_used    4075
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      33.0350
_cell_measurement_theta_min      4.4650
_cell_volume                     914.64(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.80a (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)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     15.00  42.00   0.50   10.57    --   17.39-128.00 -83.00   54
  2  \w    -32.00  -4.00   0.50   10.57    --  -15.36 -63.00 -30.59   56
  3  \w      6.00  60.00   0.50   10.57    --  -15.36  19.00 120.00  108
  4  \w    -52.00  -6.00   0.50   10.57    --  -15.36 -57.00  90.00   92
  5  \w    -60.00  -5.00   0.50   10.57    --  -15.36 -57.00-180.00  110
  6  \w    -45.00  -1.00   0.50   10.57    --  -15.36 -63.00 -83.34   88
  7  \w    -92.00  -6.00   0.50   10.57    --  -15.36 -37.00-180.00  172
  8  \w    -43.00  -6.00   0.50   10.57    --  -15.36 -65.00  17.98   74
  9  \w     20.00  52.00   0.50   10.57    --   17.39-104.00-114.21   64
 10  \w     14.00  49.00   0.50   10.57    --   17.39 -99.00  30.00   70
 11  \w      9.00  93.00   0.50   10.57    --   17.39  37.00  90.00  168
 12  \w    -59.00   0.00   0.50   10.57    --   17.39 -19.00 -90.00  118
 13  \w     -2.00  49.00   0.50   10.57    --   17.39 -99.00  90.00  102
 14  \w     10.00  93.00   0.50   10.57    --   17.39  37.00   0.00  166
 15  \w      4.00  53.00   0.50   10.57    --   17.39-106.00 -76.21   98
 16  \w      2.00  38.00   0.50   10.57    --   17.39 -77.00 120.00   72
 17  \w     21.00  49.00   0.50   10.57    --   17.39 -99.00 -30.00   56
 18  \w     -3.00  48.00   0.50   10.57    --   17.39 -99.00-180.00  102
 19  \w    -58.00   5.00   0.50   10.57    --   17.39 -19.00 -30.00  126
 20  \w     16.00  41.00   0.50   10.57    --   17.39-128.00 -83.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0765642000
_diffrn_orient_matrix_UB_12      0.0082105000
_diffrn_orient_matrix_UB_13      0.0154637000
_diffrn_orient_matrix_UB_21      -0.0118003000
_diffrn_orient_matrix_UB_22      0.0164995000
_diffrn_orient_matrix_UB_23      0.0503796000
_diffrn_orient_matrix_UB_31      0.0046870000
_diffrn_orient_matrix_UB_32      -0.0929197000
_diffrn_orient_matrix_UB_33      0.0103188000
_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  0.0440
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9630
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.018
_diffrn_reflns_theta_min         3.517
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    38.580
_exptl_absorpt_correction_T_max  0.683
_exptl_absorpt_correction_T_min  0.485
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.80a (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_colour_primary    black
_exptl_crystal_density_diffrn    6.705
_exptl_crystal_description       plate
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.035
_exptl_crystal_size_mid          0.021
_exptl_crystal_size_min          0.017
_refine_diff_density_max         2.687
_refine_diff_density_min         -2.113
_refine_diff_density_rms         0.489
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     48
_refine_ls_number_reflns         978
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0460P)^2^+13.4427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0672
_refine_ls_wR_factor_ref         0.0684
_reflns_Friedel_coverage         0.000
_reflns_number_gt                932
_reflns_number_total             978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01212f2.cif
_cod_data_source_block           wo2i-2
_cod_depositor_comments
'Adding full bibliography for 7707330--7707331.cif.'
_cod_database_code               7707331
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         W2O3I4
_shelx_estimated_absorpt_t_max   0.560
_shelx_estimated_absorpt_t_min   0.345
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
;
_shelx_res_checksum              22380
_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 1.141
_oxdiff_exptl_absorpt_empirical_full_min 0.893