#------------------------------------------------------------------------------
#$Date: 2024-02-04 14:00:49 +0200 (Sun, 04 Feb 2024) $
#$Revision: 289518 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/46/7714600.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_7714600
loop_
_publ_author_name
'Raabe, Jan-Christian'
'Jameel, Froze'
'Stein, Matthias'
'Albert, Jakob'
'Poller, Maximilian J.'
_publ_section_title
;
 Heteroelements in polyoxometalates: a study on the influence of different
 group 15 elements on polyoxometalate formation.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              454
_journal_page_last               466
_journal_paper_doi               10.1039/d3dt03883a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'Na6 O76 P4 W14, 2.5(O)'
_chemical_formula_sum            'H6 Na6 O58 P4 W14'
_chemical_formula_weight         4091.72
_chemical_properties_physical    Hygroscopic
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_primary     heavy
_audit_creation_date             2023-04-05
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-09-08 deposited with the CCDC.	2023-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                99.1067(16)
_cell_angle_beta                 91.2955(16)
_cell_angle_gamma                104.3378(18)
_cell_formula_units_Z            1
_cell_length_a                   10.8321(2)
_cell_length_b                   12.6641(3)
_cell_length_c                   15.4456(3)
_cell_measurement_reflns_used    56046
_cell_measurement_temperature    99.92(18)
_cell_measurement_theta_max      29.3570
_cell_measurement_theta_min      2.8500
_cell_volume                     2022.70(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.92(18)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4127
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -86.00 -43.00   1.00   20.00    --   -9.92 154.00  82.20   43
  2  ω    -15.00  31.00   1.00   20.00    --   -9.92 -99.00   0.00   46
  3  ω    -86.00 -43.00   1.00   20.00    --   -9.92 154.00 163.41   43
  4  ω    -85.00 -42.00   1.00   20.00    --   -9.92 153.00 -28.92   43
  5  ω    -69.00  27.00   1.00   20.00    --   10.55 -19.00-180.00   96
  6  ω    -69.00  27.00   1.00   20.00    --   10.55 -19.00   0.00   96
  7  ω      2.00  63.00   1.00   20.00    --   10.55-120.00 -25.80   61
  8  ω    -14.00  85.00   1.00   20.00    --   10.55  38.00-180.00   99
  9  ω    -27.00  91.00   1.00   20.00    --   10.55  19.00   0.00  118
 10  ω    -84.00 -41.00   1.00   20.00    --   -9.92 152.00-104.93   43
 11  ω    -15.00  31.00   1.00   20.00    --   -9.92 -99.00 150.00   46
 12  ω    -85.00 -42.00   1.00   20.00    --   -9.92 153.00  17.67   43
 13  ω    -69.00 -30.00   1.00   20.00    --   -9.92 129.00 -46.76   39
 14  ω    -42.00  23.00   1.00   20.00    --   -9.92 -77.00-120.00   65
 15  ω    -43.00  21.00   1.00   20.00    --   -9.92  77.00 -90.00   64
 16  ω    -15.00  31.00   1.00   20.00    --   -9.92 -99.00 -60.00   46
 17  ω    -81.00 -38.00   1.00   20.00    --   -9.92 148.00  -8.82   43
 18  ω    -69.00 -30.00   1.00   20.00    --   -9.92 129.00-118.80   39
 19  ω    -43.00  21.00   1.00   20.00    --   -9.92  77.00   0.00   64
 20  ω    -42.00  23.00   1.00   20.00    --   -9.92 -77.00-150.00   65
 21  ω    -43.00  21.00   1.00   20.00    --   -9.92  77.00 -60.00   64
 22  ω    -78.00  30.00   1.00   20.00    --   10.55   0.00-150.00  108
 23  ω    -78.00  99.00   1.00   20.00    --   10.55   0.00-180.00  177
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0379700000
_diffrn_orient_matrix_UB_12      -0.0370519000
_diffrn_orient_matrix_UB_13      -0.0138964000
_diffrn_orient_matrix_UB_21      -0.0340321000
_diffrn_orient_matrix_UB_22      -0.0146716000
_diffrn_orient_matrix_UB_23      -0.0417207000
_diffrn_orient_matrix_UB_31      0.0445774000
_diffrn_orient_matrix_UB_32      0.0430380000
_diffrn_orient_matrix_UB_33      -0.0154399000
_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  0.0753
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            88070
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.455
_diffrn_reflns_theta_min         2.288
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    20.037
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15221
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.359
_exptl_crystal_description       block
_exptl_crystal_F_000             1790
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Water'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.567
_refine_diff_density_min         -4.396
_refine_diff_density_rms         0.305
_refine_ls_extinction_coef       0.00039(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         10454
_refine_ls_number_restraints     641
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0283
_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/[σ²(Fo²)+(0.0313P)²+19.9366P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0719
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10049
_reflns_number_total             10454
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt03883a2.cif
_cod_data_source_block           jcr253-2_auto
_cod_depositor_comments
'Adding full bibliography for 7714599--7714602.cif.'
_cod_original_cell_volume        2022.72(7)
_cod_original_formula_sum        'Na6 H6 P4 W14 O58'
_cod_database_code               7714600
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Na7PW6O24
_chemical_oxdiff_usercomment     'Raabe/Albert, 15.02.2023, Mo, 100K'
_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_max   0.123
_shelx_estimated_absorpt_t_min   0.060
_olex2_refinement_description
;
1. Restrained distances
 Na3-O9X \\sim Na3-O9W
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O16) \\sim Ueq: with sigma of
0.002 and sigma for terminal atoms of 0.004
Uanis(O4) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(P1) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O17) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O9X) = Uanis(O9W)
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O9X)=1-FVAR(1)
 Sof(O9W)=FVAR(1)
 Fixed Sof: O28(0.25)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 3.400
_oxdiff_exptl_absorpt_empirical_full_min 0.560
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
W1 W 0.37237(2) 1.08332(2) 0.73505(2) 0.00588(5) Uani 1 1 d . . . . .
W2 W 0.10971(2) 0.84046(2) 0.63875(2) 0.01493(6) Uani 1 1 d . . . . .
W3 W -0.00999(2) 0.65882(2) 0.77093(2) 0.01364(6) Uani 1 1 d . . . . .
W4 W 0.12640(2) 0.72348(2) 1.00190(2) 0.00944(6) Uani 1 1 d . . . . .
W5 W 0.43961(2) 0.70264(2) 0.91176(2) 0.00398(5) Uani 1 1 d . . . . .
W6 W 0.31779(2) 0.66471(2) 0.70007(2) 0.00517(5) Uani 1 1 d . . . . .
W7 W 0.56767(2) 0.88616(2) 0.77745(2) 0.00352(5) Uani 1 1 d . . . . .
P1 P 0.25235(13) 0.87822(11) 0.84988(9) 0.0052(2) Uani 1 1 d . U . . .
P2 P 0.59047(13) 1.13275(11) 0.90237(9) 0.0046(2) Uani 1 1 d . . . . .
Na1 Na 0.1363(2) 1.2634(2) 0.71297(16) 0.0169(5) Uani 1 1 d . . . . .
Na2 Na 0.6662(2) 0.5849(2) 1.05591(17) 0.0157(5) Uani 1 1 d . . . . .
Na3 Na 0.7020(2) 0.92698(18) 0.99505(14) 0.0082(4) Uani 1 1 d D . . . .
O1 O 0.3074(4) 0.9995(3) 0.8454(2) 0.0070(7) Uani 1 1 d . U . . .
O1W O 0.3366(6) 1.3547(5) 0.6680(4) 0.0406(16) Uani 1 1 d . . . . .
O2 O 0.1328(4) 0.8291(4) 0.7850(3) 0.0117(8) Uani 1 1 d . . . . .
O2W O 0.0407(7) 1.3779(6) 0.6362(3) 0.0442(17) Uani 1 1 d . . . . .
O3 O 0.2186(3) 0.8678(3) 0.9433(3) 0.0076(7) Uani 1 1 d . . . . .
O3W O 0.0637(5) 1.1216(4) 0.5857(3) 0.0262(11) Uani 1 1 d . . . . .
O4 O 0.3529(3) 0.8115(3) 0.8220(2) 0.0064(7) Uani 1 1 d . U . . .
O4W O -0.0401(6) 1.1491(8) 0.7720(4) 0.073(3) Uani 1 1 d . . . . .
O5 O 0.2484(4) 0.9674(3) 0.6669(3) 0.0110(8) Uani 1 1 d . . . . .
O5W O 0.5169(5) 0.6110(4) 1.1636(4) 0.0226(10) Uani 1 1 d . . . . .
O6 O 0.0138(4) 0.6964(4) 0.6550(3) 0.0172(9) Uani 1 1 d . . . . .
O6W O 0.8450(4) 0.5808(4) 1.1533(3) 0.0139(8) Uani 1 1 d . . . . .
O7 O 0.0447(4) 0.6646(4) 0.8914(3) 0.0177(9) Uani 1 1 d . . . . .
O7W O 0.7481(5) 0.5204(5) 0.9262(3) 0.0289(12) Uani 1 1 d . . . . .
O8 O 0.2791(4) 0.6701(3) 0.9466(3) 0.0116(8) Uani 1 1 d . . . . .
O8W O 0.7640(4) 0.7800(3) 1.0545(3) 0.0114(8) Uani 1 1 d . . . . .
O9 O 0.5832(3) 0.8033(3) 0.8693(2) 0.0043(7) Uani 1 1 d . . . . .
O9W O 0.8809(8) 0.9234(8) 0.9078(6) 0.0117(12) Uani 0.478(9) 1 d D . P A 1
O10 O 0.4041(3) 0.6177(3) 0.8001(2) 0.0054(7) Uani 1 1 d . . . . .
O11 O 0.5000(4) 0.7578(3) 0.6986(2) 0.0062(7) Uani 1 1 d . . . . .
O12 O 0.4892(4) 0.9724(3) 0.7250(2) 0.0071(7) Uani 1 1 d . U . . .
O13 O 0.2625(4) 0.7569(3) 0.6390(3) 0.0097(7) Uani 1 1 d . . . . .
O14 O 0.1665(4) 0.6120(3) 0.7460(3) 0.0100(8) Uani 1 1 d . . . . .
O15 O 0.5877(3) 1.0096(3) 0.8869(2) 0.0057(7) Uani 1 1 d . . . . .
O16 O 0.5169(4) 1.1635(3) 0.8276(2) 0.0064(7) Uani 1 1 d . U . . .
O17 O 0.7291(4) 1.2023(3) 0.9039(2) 0.0076(7) Uani 1 1 d . U . . .
O18 O 0.5290(3) 1.1610(3) 0.9889(2) 0.0062(7) Uani 1 1 d . . . . .
O19 O 0.4487(4) 1.1429(4) 0.6506(3) 0.0143(8) Uani 1 1 d . . . . .
O20 O 0.2779(4) 1.1733(3) 0.7720(3) 0.0083(7) Uani 1 1 d . . . . .
O21 O 0.1049(5) 0.8202(4) 0.5247(3) 0.0250(11) Uani 1 1 d . . . . .
O22 O -0.0116(5) 0.9066(4) 0.6614(4) 0.0243(11) Uani 1 1 d . . . . .
O23 O -0.0934(4) 0.5221(4) 0.7435(3) 0.0207(10) Uani 1 1 d . . . . .
O24 O -0.1325(5) 0.7259(5) 0.7941(4) 0.0378(15) Uani 1 1 d . . . . .
O25 O 0.0785(4) 0.6102(4) 1.0546(3) 0.0170(9) Uani 1 1 d . . . . .
O26 O 0.0270(4) 0.8073(4) 1.0460(3) 0.0135(8) Uani 1 1 d . . . . .
O27 O 0.5094(4) 0.6187(3) 0.9621(3) 0.0102(8) Uani 1 1 d . . . . .
O29 O 0.3321(4) 0.5569(3) 0.6192(2) 0.0084(7) Uani 1 1 d . . . . .
O35 O 0.9270(4) 0.9350(4) 0.7944(3) 0.0181(9) Uani 1 1 d . . . . .
O36 O 0.7204(4) 0.9219(3) 0.7453(3) 0.0093(7) Uani 1 1 d . . . . .
O9X O 0.9201(7) 0.9676(7) 0.9466(5) 0.0117(12) Uani 0.522(9) 1 d D . P A 2
O28 O -0.1150(15) 1.0240(13) 0.6647(11) 0.012(3) Uiso 0.25 1 d . . P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Na Na 0.0362 0.0249 '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'
P P 0.1023 0.0942 '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_
_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
O5 W1 O1 85.05(16) . . ?
O5 W1 O12 86.01(16) . . ?
O5 W1 O16 159.85(16) . . ?
O12 W1 O1 80.93(14) . . ?
O16 W1 O1 80.02(14) . . ?
O16 W1 O12 78.37(15) . . ?
O19 W1 O1 169.87(17) . . ?
O19 W1 O5 98.7(2) . . ?
O19 W1 O12 89.88(17) . . ?
O19 W1 O16 94.00(18) . . ?
O19 W1 O20 102.28(19) . . ?
O20 W1 O1 86.24(16) . . ?
O20 W1 O5 100.08(18) . . ?
O20 W1 O12 165.30(16) . . ?
O20 W1 O16 92.41(17) . . ?
O5 W2 O2 84.22(16) . . ?
O5 W2 O6 152.63(17) . . ?
O5 W2 O13 81.94(16) . . ?
O6 W2 O2 72.12(17) . . ?
O6 W2 O13 80.07(16) . . ?
O13 W2 O2 78.53(14) . . ?
O21 W2 O2 166.20(19) . . ?
O21 W2 O5 100.8(2) . . ?
O21 W2 O6 99.5(2) . . ?
O21 W2 O13 89.36(19) . . ?
O21 W2 O22 102.2(2) . . ?
O22 W2 O2 89.8(2) . . ?
O22 W2 O5 97.1(2) . . ?
O22 W2 O6 96.3(2) . . ?
O22 W2 O13 168.3(2) . . ?
O6 W3 O2 71.98(16) . . ?
O6 W3 O14 81.00(16) . . ?
O7 W3 O2 84.41(17) . . ?
O7 W3 O6 153.45(18) . . ?
O7 W3 O14 82.72(17) . . ?
O14 W3 O2 78.89(15) . . ?
O23 W3 O2 166.88(18) . . ?
O23 W3 O6 99.9(2) . . ?
O23 W3 O7 100.8(2) . . ?
O23 W3 O14 89.77(19) . . ?
O23 W3 O24 102.4(3) . . ?
O24 W3 O2 88.8(2) . . ?
O24 W3 O6 95.3(3) . . ?
O24 W3 O7 96.2(2) . . ?
O24 W3 O14 167.7(2) . . ?
O7 W4 O3 85.91(17) . . ?
O7 W4 O8 83.82(18) . . ?
O7 W4 O17 159.37(16) . 2_677 ?
O8 W4 O3 79.81(15) . . ?
O17 W4 O3 80.54(15) 2_677 . ?
O17 W4 O8 78.55(16) 2_677 . ?
O25 W4 O3 170.63(19) . . ?
O25 W4 O7 100.1(2) . . ?
O25 W4 O8 93.62(19) . . ?
O25 W4 O17 91.66(19) . 2_677 ?
O25 W4 O26 101.5(2) . . ?
O26 W4 O3 84.20(17) . . ?
O26 W4 O7 101.0(2) . . ?
O26 W4 O8 162.93(18) . . ?
O26 W4 O17 93.04(17) . 2_677 ?
O8 W5 O4 82.58(16) . . ?
O8 W5 O9 151.04(17) . . ?
O8 W5 O10 96.92(18) . . ?
O8 W5 O18 85.22(17) . 2_677 ?
O9 W5 O4 72.43(14) . . ?
O9 W5 O18 78.98(15) . 2_677 ?
O10 W5 O4 74.05(14) . . ?
O10 W5 O9 90.20(15) . . ?
O10 W5 O18 159.92(15) . 2_677 ?
O18 W5 O4 86.50(14) 2_677 . ?
O27 W5 O4 172.07(16) . . ?
O27 W5 O8 102.63(19) . . ?
O27 W5 O9 103.87(17) . . ?
O27 W5 O10 99.20(18) . . ?
O27 W5 O18 99.80(17) . 2_677 ?
O10 W6 O4 72.44(14) . . ?
O10 W6 O11 79.28(15) . . ?
O11 W6 O4 72.55(14) . . ?
O13 W6 O4 86.10(16) . . ?
O13 W6 O10 157.87(17) . . ?
O13 W6 O11 89.37(17) . . ?
O13 W6 O14 96.06(18) . . ?
O14 W6 O4 85.45(15) . . ?
O14 W6 O10 87.74(16) . . ?
O14 W6 O11 156.95(16) . . ?
O29 W6 O4 165.09(16) . . ?
O29 W6 O10 96.45(16) . . ?
O29 W6 O11 95.99(17) . . ?
O29 W6 O13 103.64(18) . . ?
O29 W6 O14 104.40(18) . . ?
O9 W7 O4 72.49(14) . . ?
O9 W7 O15 79.85(15) . . ?
O11 W7 O4 74.05(14) . . ?
O11 W7 O9 91.23(16) . . ?
O11 W7 O15 160.42(15) . . ?
O12 W7 O4 82.90(15) . . ?
O12 W7 O9 151.38(16) . . ?
O12 W7 O11 95.92(17) . . ?
O12 W7 O15 84.42(16) . . ?
O15 W7 O4 86.61(13) . . ?
O36 W7 O4 172.78(16) . . ?
O36 W7 O9 102.77(17) . . ?
O36 W7 O11 100.95(18) . . ?
O36 W7 O12 103.00(18) . . ?
O36 W7 O15 98.02(17) . . ?
O1 P1 O2 110.5(2) . . ?
O1 P1 O4 109.8(2) . . ?
O2 P1 O4 107.3(2) . . ?
O3 P1 O1 108.6(2) . . ?
O3 P1 O2 110.8(2) . . ?
O3 P1 O4 109.8(2) . . ?
O15 P2 O16 112.1(2) . . ?
O15 P2 O17 109.6(2) . . ?
O15 P2 O18 109.1(2) . . ?
O17 P2 O16 106.0(2) . . ?
O18 P2 O16 108.4(2) . . ?
O18 P2 O17 111.7(2) . . ?
O1W Na1 Na2 77.04(19) . 2_677 ?
O1W Na1 O2W 88.1(2) . . ?
O1W Na1 O3W 99.9(2) . . ?
O1W Na1 O4W 167.8(3) . . ?
O1W Na1 O6W 90.9(2) . 2_677 ?
O1W Na1 O20 77.27(18) . . ?
O2W Na1 Na2 115.81(18) . 2_677 ?
O2W Na1 O3W 86.0(2) . . ?
O2W Na1 O6W 84.65(18) . 2_677 ?
O3W Na1 Na2 157.62(16) . 2_677 ?
O3W Na1 O6W 165.5(2) . 2_677 ?
O4W Na1 Na2 97.64(16) . 2_677 ?
O4W Na1 O2W 104.1(3) . . ?
O4W Na1 O3W 80.8(2) . . ?
O4W Na1 O6W 90.7(2) . 2_677 ?
O6W Na1 Na2 35.01(10) 2_677 2_677 ?
O20 Na1 Na2 62.64(11) . 2_677 ?
O20 Na1 O2W 165.3(2) . . ?
O20 Na1 O3W 95.00(19) . . ?
O20 Na1 O4W 90.6(3) . . ?
O20 Na1 O6W 96.89(16) . 2_677 ?
O5W Na2 W5 82.69(13) . 2_667 ?
O5W Na2 O6W 98.99(18) . . ?
O5W Na2 O8W 97.11(17) . . ?
O5W Na2 O27 75.65(16) . 2_667 ?
O6W Na2 W5 81.36(12) . 2_667 ?
O6W Na2 O27 107.83(16) . 2_667 ?
O7W Na2 W5 87.47(15) . 2_667 ?
O7W Na2 O5W 160.4(2) . . ?
O7W Na2 O6W 96.19(19) . . ?
O7W Na2 O8W 95.43(18) . . ?
O7W Na2 O27 87.99(18) . 2_667 ?
O7W Na2 O27 84.70(19) . . ?
O8W Na2 W5 170.24(13) . 2_667 ?
O8W Na2 O6W 89.05(16) . . ?
O8W Na2 O27 162.35(17) . 2_667 ?
O27 Na2 W5 107.70(12) . 2_667 ?
O27 Na2 W5 26.68(9) 2_667 2_667 ?
O27 Na2 O5W 82.25(18) . . ?
O27 Na2 O6W 170.93(18) . . ?
O27 Na2 O8W 81.88(15) . . ?
O27 Na2 O27 81.21(15) . 2_667 ?
O1 Na3 P1 29.17(9) 2_677 2_677 ?
O1 Na3 O3 58.36(13) 2_677 2_677 ?
O1 Na3 O15 115.97(15) 2_677 . ?
O1 Na3 O18 81.64(14) 2_677 2_677 ?
O3 Na3 P1 29.20(9) 2_677 2_677 ?
O3 Na3 O15 79.12(14) 2_677 . ?
O8W Na3 P1 105.01(13) . 2_677 ?
O8W Na3 O1 82.29(14) . 2_677 ?
O8W Na3 O3 125.09(16) . 2_677 ?
O8W Na3 O15 155.77(16) . . ?
O8W Na3 O18 90.61(15) . 2_677 ?
O8W Na3 O9X 84.1(2) . . ?
O9 Na3 P1 154.75(13) . 2_677 ?
O9 Na3 O1 144.10(15) . 2_677 ?
O9 Na3 O3 140.99(16) . 2_677 ?
O9 Na3 O8W 93.47(15) . . ?
O9 Na3 O15 62.34(13) . . ?
O9 Na3 O18 62.70(13) . 2_677 ?
O9 Na3 O9X 102.3(2) . . ?
O9W Na3 P1 114.9(2) . 2_677 ?
O9W Na3 O1 130.6(3) . 2_677 ?
O9W Na3 O3 94.0(3) . 2_677 ?
O9W Na3 O8W 83.7(2) . . ?
O9W Na3 O9 83.7(3) . . ?
O9W Na3 O15 94.4(2) . . ?
O9W Na3 O18 145.6(3) . 2_677 ?
O15 Na3 P1 97.75(11) . 2_677 ?
O18 Na3 P1 99.43(11) 2_677 2_677 ?
O18 Na3 O3 116.51(15) 2_677 2_677 ?
O18 Na3 O15 77.37(13) 2_677 . ?
O9X Na3 O15 101.6(2) . . ?
W1 O1 Na3 131.41(18) . 2_677 ?
P1 O1 W1 131.4(2) . . ?
P1 O1 Na3 97.21(19) . 2_677 ?
W3 O2 W2 93.86(14) . . ?
P1 O2 W2 128.8(2) . . ?
P1 O2 W3 128.6(2) . . ?
W4 O3 Na3 133.01(18) . 2_677 ?
P1 O3 W4 131.2(2) . . ?
P1 O3 Na3 95.77(19) . 2_677 ?
W5 O4 W7 89.19(12) . . ?
W6 O4 W5 90.55(13) . . ?
W6 O4 W7 90.13(12) . . ?
P1 O4 W5 125.9(2) . . ?
P1 O4 W6 123.5(2) . . ?
P1 O4 W7 126.5(2) . . ?
W1 O5 W2 159.6(2) . . ?
W2 O6 W3 121.3(2) . . ?
Na2 O6W Na1 107.54(18) . 2_677 ?
W4 O7 W3 158.6(3) . . ?
W5 O8 W4 149.3(2) . . ?
Na3 O8W Na2 135.4(2) . . ?
W5 O9 Na3 107.80(16) . . ?
W7 O9 W5 124.05(19) . . ?
W7 O9 Na3 109.17(16) . . ?
W5 O10 W6 122.74(19) . . ?
W7 O11 W6 123.11(19) . . ?
W7 O12 W1 148.7(2) . . ?
W6 O13 W2 139.4(2) . . ?
W6 O14 W3 138.8(2) . . ?
W7 O15 Na3 99.18(15) . . ?
P2 O15 W7 135.5(2) . . ?
P2 O15 Na3 121.6(2) . . ?
P2 O16 W1 136.6(2) . . ?
P2 O17 W4 136.0(2) . 2_677 ?
W5 O18 Na3 100.45(15) 2_677 2_677 ?
P2 O18 W5 135.1(2) . 2_677 ?
P2 O18 Na3 120.2(2) . 2_677 ?
W1 O20 Na1 138.9(2) . . ?
W5 O27 Na2 106.86(19) . 2_667 ?
W5 O27 Na2 153.5(2) . . ?
Na2 O27 Na2 98.79(15) . 2_667 ?
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 O1 2.187(4) . ?
W1 O5 1.880(4) . ?
W1 O12 2.102(4) . ?
W1 O16 2.044(4) . ?
W1 O19 1.734(4) . ?
W1 O20 1.752(4) . ?
W2 O2 2.298(4) . ?
W2 O5 1.893(4) . ?
W2 O6 1.920(5) . ?
W2 O13 2.174(4) . ?
W2 O21 1.738(5) . ?
W2 O22 1.739(5) . ?
W3 O2 2.297(4) . ?
W3 O6 1.931(5) . ?
W3 O7 1.924(5) . ?
W3 O14 2.162(4) . ?
W3 O23 1.723(4) . ?
W3 O24 1.759(5) . ?
W4 O3 2.195(4) . ?
W4 O7 1.859(4) . ?
W4 O8 2.088(4) . ?
W4 O17 2.046(4) 2_677 ?
W4 O25 1.735(4) . ?
W4 O26 1.766(4) . ?
W5 O4 2.426(4) . ?
W5 O8 1.800(4) . ?
W5 O9 1.950(3) . ?
W5 O10 1.859(4) . ?
W5 O18 2.073(4) 2_677 ?
W5 O27 1.715(4) . ?
W6 O4 2.379(4) . ?
W6 O10 2.030(4) . ?
W6 O11 2.035(4) . ?
W6 O13 1.811(4) . ?
W6 O14 1.815(4) . ?
W6 O29 1.738(4) . ?
W7 O4 2.443(4) . ?
W7 O9 1.921(4) . ?
W7 O11 1.846(4) . ?
W7 O12 1.812(4) . ?
W7 O15 2.080(4) . ?
W7 O36 1.710(4) . ?
P1 O1 1.517(4) . ?
P1 O2 1.553(4) . ?
P1 O3 1.515(4) . ?
P1 O4 1.565(4) . ?
P2 O15 1.533(4) . ?
P2 O16 1.541(4) . ?
P2 O17 1.539(4) . ?
P2 O18 1.538(4) . ?
Na1 Na2 4.057(3) 2_677 ?
Na1 O1W 2.368(6) . ?
Na1 O2W 2.411(6) . ?
Na1 O3W 2.412(6) . ?
Na1 O4W 2.389(7) . ?
Na1 O6W 2.587(5) 2_677 ?
Na1 O20 2.372(5) . ?
Na2 O5W 2.388(6) . ?
Na2 O6W 2.441(5) . ?
Na2 O7W 2.322(6) . ?
Na2 O8W 2.439(5) . ?
Na2 O27 2.769(5) 2_667 ?
Na2 O27 2.368(5) . ?
Na3 O1 2.506(4) 2_677 ?
Na3 O3 2.544(4) 2_677 ?
Na3 O8W 2.428(5) . ?
Na3 O9 2.409(4) . ?
Na3 O9W 2.391(8) . ?
Na3 O15 2.552(4) . ?
Na3 O18 2.509(4) 2_677 ?
Na3 O9X 2.451(8) . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 W1 O5 W2 8.0(7) . . . . ?
O1 W1 O20 Na1 -139.0(3) . . . . ?
O1 P1 O2 W2 49.7(3) . . . . ?
O1 P1 O2 W3 -171.5(2) . . . . ?
O1 P1 O3 W4 176.3(3) . . . . ?
O1 P1 O3 Na3 -1.9(2) . . . 2_677 ?
O1 P1 O4 W5 121.0(2) . . . . ?
O1 P1 O4 W6 -119.5(2) . . . . ?
O1 P1 O4 W7 0.0(3) . . . . ?
O2 W2 O5 W1 -9.9(7) . . . . ?
O2 P1 O1 W1 -55.9(3) . . . . ?
O2 P1 O1 Na3 123.6(2) . . . 2_677 ?
O2 P1 O3 W4 54.8(4) . . . . ?
O2 P1 O3 Na3 -123.4(2) . . . 2_677 ?
O2 P1 O4 W5 -118.9(3) . . . . ?
O2 P1 O4 W6 0.6(3) . . . . ?
O2 P1 O4 W7 120.2(3) . . . . ?
O3 W4 O7 W3 -8.5(7) . . . . ?
O3 P1 O1 W1 -177.6(3) . . . . ?
O3 P1 O1 Na3 1.9(2) . . . 2_677 ?
O3 P1 O2 W2 170.1(3) . . . . ?
O3 P1 O2 W3 -51.1(3) . . . . ?
O3 P1 O4 W5 1.6(3) . . . . ?
O3 P1 O4 W6 121.1(2) . . . . ?
O3 P1 O4 W7 -119.4(3) . . . . ?
O4 W5 O8 W4 -57.2(5) . . . . ?
O4 W5 O10 W6 -4.35(18) . . . . ?
O4 W6 O13 W2 -63.8(3) . . . . ?
O4 W6 O14 W3 65.4(3) . . . . ?
O4 W7 O11 W6 3.58(19) . . . . ?
O4 W7 O12 W1 53.0(4) . . . . ?
O4 P1 O1 W1 62.3(3) . . . . ?
O4 P1 O1 Na3 -118.22(19) . . . 2_677 ?
O4 P1 O2 W2 -70.0(3) . . . . ?
O4 P1 O2 W3 68.8(3) . . . . ?
O4 P1 O3 W4 -63.5(3) . . . . ?
O4 P1 O3 Na3 118.27(19) . . . 2_677 ?
O5 W1 O20 Na1 -54.7(3) . . . . ?
O6 W2 O5 W1 -39.9(9) . . . . ?
O8 W4 O7 W3 -88.6(7) . . . . ?
O8 W5 O10 W6 75.9(2) . . . . ?
O8 W5 O27 Na2 42.2(2) . . . 2_667 ?
O8 W5 O27 Na2 -122.8(5) . . . . ?
O9 W5 O8 W4 -26.9(7) . . . . ?
O9 W5 O10 W6 -76.0(2) . . . . ?
O9 W5 O27 Na2 45.4(5) . . . . ?
O9 W5 O27 Na2 -149.54(16) . . . 2_667 ?
O9 W7 O11 W6 75.0(2) . . . . ?
O9 W7 O12 W1 22.5(6) . . . . ?
O10 W5 O8 W4 -130.0(5) . . . . ?
O10 W5 O27 Na2 137.9(5) . . . . ?
O10 W5 O27 Na2 -57.04(19) . . . 2_667 ?
O10 W6 O13 W2 -77.8(6) . . . . ?
O10 W6 O14 W3 138.0(3) . . . . ?
O11 W6 O13 W2 -136.4(3) . . . . ?
O11 W6 O14 W3 82.6(5) . . . . ?
O11 W7 O12 W1 126.1(4) . . . . ?
O12 W1 O5 W2 89.3(7) . . . . ?
O12 W1 O20 Na1 -168.2(5) . . . . ?
O12 W7 O11 W6 -77.3(2) . . . . ?
O13 W2 O5 W1 -89.1(7) . . . . ?
O13 W6 O14 W3 -20.2(3) . . . . ?
O14 W6 O13 W2 21.1(3) . . . . ?
O15 W7 O11 W6 12.7(6) . . . . ?
O15 W7 O12 W1 -34.2(4) . . . . ?
O15 P2 O16 W1 24.4(4) . . . . ?
O15 P2 O17 W4 -92.5(4) . . . 2_677 ?
O15 P2 O18 W5 145.3(3) . . . 2_677 ?
O15 P2 O18 Na3 -63.2(3) . . . 2_677 ?
O16 W1 O5 W2 50.3(10) . . . . ?
O16 W1 O20 Na1 141.2(3) . . . . ?
O16 P2 O15 W7 26.0(4) . . . . ?
O16 P2 O15 Na3 179.0(2) . . . . ?
O16 P2 O17 W4 146.4(3) . . . 2_677 ?
O16 P2 O18 W5 -92.4(3) . . . 2_677 ?
O16 P2 O18 Na3 59.1(3) . . . 2_677 ?
O17 W4 O7 W3 -57.3(11) 2_677 . . . ?
O17 P2 O15 W7 -91.4(3) . . . . ?
O17 P2 O15 Na3 61.6(3) . . . . ?
O17 P2 O16 W1 143.9(3) . . . . ?
O17 P2 O18 W5 24.0(4) . . . 2_677 ?
O17 P2 O18 Na3 175.5(2) . . . 2_677 ?
O18 W5 O8 W4 29.9(5) 2_677 . . . ?
O18 W5 O10 W6 -19.2(6) 2_677 . . . ?
O18 W5 O27 Na2 -35.5(5) 2_677 . . . ?
O18 W5 O27 Na2 129.50(16) 2_677 . . 2_667 ?
O18 P2 O15 W7 146.1(3) . . . . ?
O18 P2 O15 Na3 -60.9(3) . . . . ?
O18 P2 O16 W1 -96.0(3) . . . . ?
O18 P2 O17 W4 28.5(4) . . . 2_677 ?
O19 W1 O5 W2 178.5(7) . . . . ?
O19 W1 O20 Na1 46.6(3) . . . . ?
O20 W1 O5 W2 -77.2(7) . . . . ?
O21 W2 O5 W1 -176.9(7) . . . . ?
O22 W2 O5 W1 79.1(7) . . . . ?
O25 W4 O7 W3 178.8(7) . . . . ?
O26 W4 O7 W3 74.8(7) . . . . ?
O27 W5 O8 W4 128.9(5) . . . . ?
O27 W5 O10 W6 179.9(2) . . . . ?
O29 W6 O13 W2 127.6(3) . . . . ?
O29 W6 O14 W3 -126.0(3) . . . . ?
O36 W7 O11 W6 178.2(2) . . . . ?
O36 W7 O12 W1 -131.2(4) . . . . ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.509 -0.510 0.500 493.8 215.4 '21.6 H2O'
