#------------------------------------------------------------------------------
#$Date: 2023-10-07 03:00:39 +0300 (Sat, 07 Oct 2023) $
#$Revision: 286841 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/30/07/2300717.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_2300717
loop_
_publ_author_name
'Ruth, Paul Niklas'
'Graw, Nico'
'Ernemann, Tobias'
'Herbst-Irmer, Regine'
'Stalke, Dietmar'
_publ_section_title
;
 Indium Kα radiation from a MetalJet X-ray source: comparison
 of the Eiger2 CdTe and Photon III detectors.
;
_journal_issue                   'Pt 5'
_journal_name_full               'Journal of applied crystallography'
_journal_page_first              1322
_journal_page_last               1329
_journal_paper_doi               10.1107/S1600576723007215
_journal_volume                  56
_journal_year                    2023
_chemical_formula_moiety         'O4 W, 2(H2 O), 2(Na)'
_chemical_formula_sum            'H4 Na2 O6 W'
_chemical_formula_weight         329.86
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2019/2
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.434(2)
_cell_length_b                   10.553(2)
_cell_length_c                   13.792(3)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      45.2905
_cell_measurement_theta_min      2.4745
_cell_volume                     1227.5(5)
_computing_cell_refinement       'Bruker SAINT V8.40B'
_computing_data_collection       'Bruker APEX2 v2012.2'
_computing_data_reduction        'Bruker SAINT V8.40B'
_computing_molecular_graphics    'VESTA 3.5.7'
_computing_publication_material  'VESTA 3.5.7'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT(Sheldrick,Acta Cryst.(2015)A71,3-8)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_type            'Bruker Photon III C14 CMOS'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           InK\a
_diffrn_radiation_wavelength     0.5134
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            341446
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        17.941
_diffrn_reflns_theta_max         45.340
_diffrn_reflns_theta_min         2.475
_diffrn_source                   'Excillum In Metaljet D2 70 kV'
_exptl_absorpt_coefficient_mu    8.052
_exptl_absorpt_correction_T_max  0.6141
_exptl_absorpt_correction_T_min  0.3374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.570
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.208
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.086
_refine_diff_density_max         4.227
_refine_diff_density_min         -4.374
_refine_diff_density_rms         0.330
_refine_ls_extinction_coef       0.00849(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.273
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_refine_ls_number_reflns         13654
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.273
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0200
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0133P)²+1.2796P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0449
_refine_ls_wR_factor_ref         0.0456
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12323
_reflns_number_total             13654
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            nb5354sup1.cif
_cod_data_source_block           NaWO4_photon
_cod_depositor_comments
'Adding full bibliography for 2300712--2300725.cif.'
_cod_database_code               2300717
_cod_database_fobs_code          2300717
_shelx_shelxl_version_number     2019/2
_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.
;
_shelx_estimated_absorpt_t_min   0.285
_shelx_estimated_absorpt_t_max   0.544
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, 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
O1 O 0.55238(8) 0.67723(6) 0.40076(4) 0.00796(7) Uani 1 1 d . . . . .
O2 O 0.63144(8) 0.64889(6) 0.60971(5) 0.00839(7) Uani 1 1 d . . . . .
O3 O 0.31256(8) 0.60730(6) 0.53761(5) 0.00886(7) Uani 1 1 d . . . . .
O4 O 0.44297(8) 0.86159(5) 0.54162(5) 0.00746(6) Uani 1 1 d . . . . .
O5 O 0.77222(9) 0.64038(7) 0.20093(5) 0.00976(8) Uani 1 1 d D . . . .
H5A H 0.863(2) 0.645(3) 0.175(2) 0.031(7) Uiso 1 1 d D . . . .
H5B H 0.731(4) 0.709(2) 0.181(2) 0.038(9) Uiso 1 1 d D . . . .
O6 O 0.96254(10) 0.40791(7) 0.30024(5) 0.01046(8) Uani 1 1 d D . . . .
H6A H 0.936(3) 0.399(2) 0.2423(14) 0.024(6) Uiso 1 1 d D . . . .
H6B H 0.939(4) 0.339(2) 0.327(2) 0.027(7) Uiso 1 1 d D . . . .
Na1 Na 0.75924(5) 0.54888(4) 0.35232(3) 0.00809(5) Uani 1 1 d . . . . .
Na2 Na 0.65560(5) 0.49556(4) 0.08568(3) 0.00810(5) Uani 1 1 d . . . . .
W1 W 0.48650(2) 0.69837(2) 0.52275(2) 0.00451(1) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0044 0.0030 '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'
Na Na 0.0182 0.0125 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.3261 4.0239 '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
W1 O1 Na1 125.54(3) . . ?
W1 O2 Na2 127.52(4) . 2_665 ?
W1 O3 Na1 132.78(4) . 5_666 ?
W1 O3 Na2 128.95(4) . 6_556 ?
Na1 O3 Na2 88.35(3) 5_666 6_556 ?
W1 O4 Na1 128.39(3) . 4_466 ?
W1 O4 Na2 122.27(3) . 3_655 ?
Na1 O4 Na2 89.43(3) 4_466 3_655 ?
W1 O4 Na2 119.11(3) . 7_576 ?
Na1 O4 Na2 94.73(3) 4_466 7_576 ?
Na2 O4 Na2 94.21(3) 3_655 7_576 ?
Na1 O5 Na2 108.18(3) . . ?
Na1 O6 Na2 92.82(3) . 6_656 ?
O5 Na1 O1 93.00(3) . . ?
O5 Na1 O3 154.57(3) . 5_666 ?
O1 Na1 O3 91.73(3) . 5_666 ?
O5 Na1 O4 111.55(3) . 4_566 ?
O1 Na1 O4 94.76(3) . 4_566 ?
O3 Na1 O4 92.91(3) 5_666 4_566 ?
O5 Na1 O6 87.38(3) . . ?
O1 Na1 O6 176.93(3) . . ?
O3 Na1 O6 86.65(3) 5_666 . ?
O4 Na1 O6 87.93(3) 4_566 . ?
O5 Na1 Na2 157.64(3) . 2_665 ?
O1 Na1 Na2 88.05(2) . 2_665 ?
O3 Na1 Na2 47.49(2) 5_666 2_665 ?
O4 Na1 Na2 46.16(2) 4_566 2_665 ?
O6 Na1 Na2 92.76(2) . 2_665 ?
O5 Na1 Na2 104.11(2) . 6_656 ?
O1 Na1 Na2 138.29(3) . 6_656 ?
O3 Na1 Na2 88.58(2) 5_666 6_656 ?
O4 Na1 Na2 43.62(2) 4_566 6_656 ?
O6 Na1 Na2 44.33(2) . 6_656 ?
Na2 Na1 Na2 62.279(14) 2_665 6_656 ?
O5 Na1 W1 115.65(3) . . ?
O1 Na1 W1 23.476(16) . . ?
O3 Na1 W1 73.81(2) 5_666 . ?
O4 Na1 W1 80.76(3) 4_566 . ?
O6 Na1 W1 156.74(2) . . ?
Na2 Na1 W1 64.797(16) 2_665 . ?
Na2 Na1 W1 120.995(18) 6_656 . ?
O5 Na1 W1 95.46(3) . 4_566 ?
O1 Na1 W1 80.45(2) . 4_566 ?
O3 Na1 W1 109.97(3) 5_666 4_566 ?
O4 Na1 W1 22.099(16) 4_566 4_566 ?
O6 Na1 W1 102.55(3) . 4_566 ?
Na2 Na1 W1 62.672(13) 2_665 4_566 ?
Na2 Na1 W1 60.527(13) 6_656 4_566 ?
W1 Na1 W1 73.470(16) . 4_566 ?
O5 Na1 Na2 36.89(2) . . ?
O1 Na1 Na2 101.08(2) . . ?
O3 Na1 Na2 117.72(3) 5_666 . ?
O4 Na1 Na2 144.65(2) 4_566 . ?
O6 Na1 Na2 77.44(2) . . ?
Na2 Na1 Na2 163.422(14) 2_665 . ?
Na2 Na1 Na2 115.491(15) 6_656 . ?
W1 Na1 Na2 122.654(17) . . ?
W1 Na1 Na2 132.153(14) 4_566 . ?
O2 Na2 O4 89.20(3) 2_664 3_645 ?
O2 Na2 O5 90.36(3) 2_664 . ?
O4 Na2 O5 173.99(3) 3_645 . ?
O2 Na2 O4 173.46(3) 2_664 7_575 ?
O4 Na2 O4 85.79(3) 3_645 7_575 ?
O5 Na2 O4 94.18(3) . 7_575 ?
O2 Na2 O6 99.83(3) 2_664 6_556 ?
O4 Na2 O6 90.99(3) 3_645 6_556 ?
O5 Na2 O6 95.00(3) . 6_556 ?
O4 Na2 O6 84.48(3) 7_575 6_556 ?
O2 Na2 O3 89.84(3) 2_664 6_656 ?
O4 Na2 O3 87.88(3) 3_645 6_656 ?
O5 Na2 O3 86.12(3) . 6_656 ?
O4 Na2 O3 85.78(3) 7_575 6_656 ?
O6 Na2 O3 170.26(3) 6_556 6_656 ?
O2 Na2 Na1 83.20(2) 2_664 2_664 ?
O4 Na2 Na1 44.41(2) 3_645 2_664 ?
O5 Na2 Na1 129.60(3) . 2_664 ?
O4 Na2 Na1 90.28(2) 7_575 2_664 ?
O6 Na2 Na1 135.39(3) 6_556 2_664 ?
O3 Na2 Na1 44.152(19) 6_656 2_664 ?
O2 Na2 Na1 142.27(2) 2_664 6_556 ?
O4 Na2 Na1 86.71(2) 3_645 6_556 ?
O5 Na2 Na1 97.28(2) . 6_556 ?
O4 Na2 Na1 41.644(19) 7_575 6_556 ?
O6 Na2 Na1 42.86(2) 6_556 6_556 ?
O3 Na2 Na1 127.40(2) 6_656 6_556 ?
Na1 Na2 Na1 117.722(14) 2_664 6_556 ?
O2 Na2 Na2 132.15(3) 2_664 5_665 ?
O4 Na2 Na2 43.092(19) 3_645 5_665 ?
O5 Na2 Na2 136.57(3) . 5_665 ?
O4 Na2 Na2 42.702(19) 7_575 5_665 ?
O6 Na2 Na2 86.89(3) 6_556 5_665 ?
O3 Na2 Na2 85.67(3) 6_656 5_665 ?
Na1 Na2 Na2 61.154(19) 2_664 5_665 ?
Na1 Na2 Na2 56.568(19) 6_556 5_665 ?
O2 Na2 W1 153.98(2) 2_664 7_575 ?
O4 Na2 W1 102.27(2) 3_645 7_575 ?
O5 Na2 W1 75.80(2) . 7_575 ?
O4 Na2 W1 25.326(15) 7_575 7_575 ?
O6 Na2 W1 103.20(2) 6_556 7_575 ?
O3 Na2 W1 67.65(2) 6_656 7_575 ?
Na1 Na2 W1 88.796(14) 2_664 7_575 ?
Na1 Na2 W1 62.636(11) 6_556 7_575 ?
Na2 Na2 W1 61.665(13) 5_665 7_575 ?
O2 Na2 W1 75.88(2) 2_664 3_645 ?
O4 Na2 W1 24.177(15) 3_645 3_645 ?
O5 Na2 W1 160.19(2) . 3_645 ?
O4 Na2 W1 100.82(2) 7_575 3_645 ?
O6 Na2 W1 73.86(2) 6_556 3_645 ?
O3 Na2 W1 107.68(2) 6_656 3_645 ?
Na1 Na2 W1 63.705(12) 2_664 3_645 ?
Na1 Na2 W1 85.702(14) 6_556 3_645 ?
Na2 Na2 W1 60.543(13) 5_665 3_645 ?
W1 Na2 W1 122.207(17) 7_575 3_645 ?
O2 Na2 Na1 77.74(2) 2_664 . ?
O4 Na2 Na1 150.34(2) 3_645 . ?
O5 Na2 Na1 34.928(19) . . ?
O4 Na2 Na1 108.63(2) 7_575 . ?
O6 Na2 Na1 65.73(2) 6_556 . ?
O3 Na2 Na1 118.18(2) 6_656 . ?
Na1 Na2 Na1 154.322(16) 2_664 . ?
Na1 Na2 Na1 87.688(14) 6_556 . ?
Na2 Na2 Na1 144.07(2) 5_665 . ?
W1 Na2 Na1 100.874(13) 7_575 . ?
W1 Na2 Na1 126.282(14) 3_645 . ?
O3 W1 O4 109.77(3) . . ?
O3 W1 O1 107.45(3) . . ?
O4 W1 O1 108.83(3) . . ?
O3 W1 O2 109.32(3) . . ?
O4 W1 O2 108.97(3) . . ?
O1 W1 O2 112.47(3) . . ?
O3 W1 Na2 141.42(2) . 7_576 ?
O4 W1 Na2 35.56(2) . 7_576 ?
O1 W1 Na2 102.35(2) . 7_576 ?
O2 W1 Na2 80.29(2) . 7_576 ?
O3 W1 Na1 111.30(3) . . ?
O4 W1 Na1 129.99(2) . . ?
O1 W1 Na1 30.98(2) . . ?
O2 W1 Na1 82.82(3) . . ?
Na2 W1 Na1 106.899(14) 7_576 . ?
O3 W1 Na2 103.93(3) . 3_655 ?
O4 W1 Na2 33.55(2) . 3_655 ?
O1 W1 Na2 79.90(2) . 3_655 ?
O2 W1 Na2 138.08(2) . 3_655 ?
Na2 W1 Na2 57.794(17) 7_576 3_655 ?
Na1 W1 Na2 108.207(15) . 3_655 ?
O3 W1 Na1 84.73(3) . 4_466 ?
O4 W1 Na1 29.51(2) . 4_466 ?
O1 W1 Na1 133.49(2) . 4_466 ?
O2 W1 Na1 104.56(3) . 4_466 ?
Na2 W1 Na1 56.836(16) 7_576 4_466 ?
Na1 W1 Na1 159.433(5) . 4_466 ?
Na2 W1 Na1 53.622(15) 3_655 4_466 ?
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
O1 W1 1.7859(7) . ?
O1 Na1 2.3075(8) . ?
O2 W1 1.7903(7) . ?
O2 Na2 2.3790(8) 2_665 ?
O3 W1 1.7657(7) . ?
O3 Na1 2.3212(8) 5_666 ?
O3 Na2 2.4566(9) 6_556 ?
O4 W1 1.7803(7) . ?
O4 Na1 2.3311(8) 4_466 ?
O4 Na2 2.4026(8) 3_655 ?
O4 Na2 2.4203(8) 7_576 ?
O5 Na1 2.3030(9) . ?
O5 Na2 2.4144(9) . ?
O6 Na1 2.3810(9) . ?
O6 Na2 2.4458(9) 6_656 ?
Na1 Na2 3.3310(9) 2_665 ?
Na1 Na2 3.4961(10) 6_656 ?
Na1 W1 3.6477(7) . ?
Na1 W1 3.7091(6) 4_566 ?
Na1 Na2 3.8215(10) . ?
Na2 Na2 3.5333(10) 5_665 ?
Na2 W1 3.6359(7) 7_575 ?
Na2 W1 3.6755(7) 3_645 ?
