Incorporating highly basic polyoxometalate anions comprising Nb or Ta into nanoscale reaction fields of porous ionic crystals.
Weng, Zhewei; Ogiwara, Naoki; Kitao, Takashi; Kikukawa, Yuji; Gao, Yu; Yan, Likai; Uchida, Sayaka; Nanoscale 13 (2021) 18451–18457; doi:10.1039/d1nr04762k

data_1564795
_publ_section_title
;
 Incorporating highly basic polyoxometalate anions comprising Nb or Ta
 into nanoscale reaction fields of porous ionic crystals.
;
_journal_issue                   44
_journal_name_full               Nanoscale
_journal_page_first              18451
_journal_page_last               18457
_journal_paper_doi               10.1039/d1nr04762k
_journal_volume                  13
_journal_year                    2021
_chemical_formula_moiety         'C12 H12 Cr6 K4 N Nb1 O105.5 P2 W17'
_chemical_formula_sum            'C12 H12 Cr6 K4 N Nb O105.5 P2 W17'
_chemical_formula_weight         5606.93
_chemical_name_systematic        'PIC 1'
_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_date             2021-06-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-06-22 deposited with the CCDC.	2021-10-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.5576(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8007(2)
_cell_length_b                   26.9370(4)
_cell_length_c                   29.2946(6)
_cell_measurement_reflns_used    35238
_cell_measurement_temperature    153.15
_cell_measurement_theta_max      30.5420
_cell_measurement_theta_min      2.6020
_cell_volume                     12386.9(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      153.15
_diffrn_detector                 'HPC area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'Rigaku HyPix-6000 area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.885
_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    -61.00 -35.00   0.50    7.30    --    5.00  45.00 150.00   52
  2  \w   -104.00  74.00   0.50    7.30    --  -14.80  45.00 150.00  356
  3  \w    -69.00 -43.00   0.50    7.30    --  -14.80  45.00 120.00   52
  4  \w     42.00  68.00   0.50    7.30    --  -14.80  45.00 120.00   52
  5  \w    -37.00 -11.00   0.50    7.30    --  -14.80  45.00   0.00   52
  6  \w     23.00  49.00   0.50    7.30    --  -14.80  45.00   0.00   52
  7  \w    -50.00  68.00   0.50    7.30    --  -14.80  45.00  30.00  236
  8  \w    -84.00 -59.00   0.50    7.30    --  -14.80  45.00  30.00   50
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC HyPix-6000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0305708000
_diffrn_orient_matrix_UB_12      0.0026283000
_diffrn_orient_matrix_UB_13      -0.0158060000
_diffrn_orient_matrix_UB_21      0.0332772000
_diffrn_orient_matrix_UB_22      -0.0029151000
_diffrn_orient_matrix_UB_23      0.0181696000
_diffrn_orient_matrix_UB_31      -0.0006323000
_diffrn_orient_matrix_UB_32      -0.0260496000
_diffrn_orient_matrix_UB_33      -0.0036182000
_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  0.0584
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            140475
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.584
_diffrn_reflns_theta_min         2.348
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              'Ultrax 18'
_exptl_absorpt_coefficient_mu    16.567
_exptl_absorpt_correction_T_max  0.01640
_exptl_absorpt_correction_T_min  0.00296
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    3.007
_exptl_crystal_description       sphere
_exptl_crystal_F_000             9936
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         4.200
_refine_diff_density_min         -1.751
_refine_diff_density_rms         0.417
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1342
_refine_ls_number_reflns         33684
_refine_ls_number_restraints     4034
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0589
_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/[\s^2^(Fo^2^)+(0.0835P)^2^+161.7350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1522
_refine_ls_wR_factor_ref         0.1608
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26481
_reflns_number_total             33684
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nr04762k2.cif
_cod_data_source_block           exp_15_sq
_cod_depositor_comments
'Adding full bibliography for 1564793--1564795.cif.'
_cod_original_formula_sum        'C12 H12 Cr6 K4 N Nb O105.50 P2 W17'
_cod_database_code               1564795
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         P2W17NbCr4O80
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{W6, Nb6}
{W5, Nb5}
{W4, Nb4}
{W3, Nb3}
{W2, Nb2}
{W1, Nb1}
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(W6) = Uanis(Nb6)
Uanis(W5) = Uanis(Nb5)
Uanis(W4) = Uanis(Nb4)
Uanis(W3) = Uanis(Nb3)
Uanis(W2) = Uanis(Nb2)
Uanis(W1) = Uanis(Nb1)
5. 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
6. Others
 Fixed Sof: W1(0.83333) W2(0.83333) W3(0.83333) W4(0.83333) W5(0.83333)
 W6(0.83333) Nb1(0.16667) Nb2(0.16667) Nb3(0.16667) Nb4(0.16667) Nb5(0.16667)
 Nb6(0.16667) O104(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10), C11(H11), C12(H12)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              35511
_shelx_fab_checksum              89248
_platon_squeeze_void_probe_radius 1.20
_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 2.094
_oxdiff_exptl_absorpt_empirical_full_min 0.566